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25 January 2011, Volume 32 Issue 2
Processing Technology
Optimization of the Extraction Process of Polyphenols from the Flower of Pomegranate (Punica granatum L.) in Xinjiang
Rahima ABDULLA1,2,LIU Li1,Haji Akber AISA1,*
2011, 32(2 ):  1-4.  doi:10.7506/spkx1002-6630-201102001
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To optimize the process conditions for the solvent extraction of polyphenols from the flower of pomegranate (Punica granatum L.) grown in Xinjiang, the effects of solvent type, extraction duration and temperature, and material/liquid ratio on polyphenol yield were studied by single factor and orthogonal array design experiments. The optimal extraction process for polyphenols from pomegranate flower was found to be based on the extraction with 20-fold volume of 60% aqueous ethanol solution at 50 ℃ for 1 h, which gave 44.20% crude polyphenol yield and 46.19% product purity, 20.42% pure polyphenol yield as calculated by multiplying them. The method is easy to operate, low-cost and highly efficient, thereby being suitable for the massive industrial production of polyphenols.

Process Optimization for Extraction of Total Flavones from Sabina pingii var. wilsonii
FU Jin-song,WANG Bo,CAI Guang-hua,YANG Mei,WANG Xiao-ling*
2011, 32(2 ):  5-8.  doi:10.7506/spkx1002-6630-201102002
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The key conditions for extracting total flavones from the branches and leaves of Sabina pingii var. wilsonii with aqueous ethanol solution under the assistance of ultrasound, including ultrasound treatment time, ethanol concentration, liquid/solid ratio, and extraction times, were optimized by combined single factor and orthogonal array design methods. The optimal conditions for improved extraction of total flavones were determined as follows: 70 min ultrasound treatment repeated twice for extracting the raw material with 10-fold volume (mL/g) of 75% aqueous ethanol solution. The maximum yield of total flavones was 5.29% under the optimized conditions.

Application of Response Surface Methodology for Optimizing Decolorization of Enzymatically Prepared Fructooligosaccharides
WAN Cheng,NIE Shao-ping,ZHANG Yuan-yuan,XIE Ming-yong*
2011, 32(2 ):  9-12.  doi:10.7506/spkx1002-6630-201102003
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Activated carbon powder was used for the adsorptive decolorization of the enzymatically prepared fructooligosaccharide solution in our laboratory, and the effects of the dosage of activated carbon as well as decolorization temperature and time on decolorization rate and fructooligosaccharide loss rate were studied. On the basis of single factor experiments, response surface methodology was employed to optimize the above three conditions. Their optimal levels were found to be: 22 g/L activated carbon dosage used for 30 min decolorization at 60 ℃. Under these conditions, the rate of decolorization of fructooligosaccharides solution was 79.16%.

Effects of Processing Factors on the Quality of Dongpo Pork
CHEN Lin,SUN Zhi-da*
2011, 32(2 ):  13-17.  doi:10.7506/spkx1002-6630-201102004
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The effects of seasoning formula and processing parameters on the sensory and textural quality of Huangzhou Dongpo pork, a famous traditional dish in Hubei province, were investigated by using sensory panel evaluation and texture profile analysis (TPA) based on the use of a TA-XT2 type texture analyzer. Soy sauce amount and stewing time had a significant effect (P< 0.05) on the sensory characteristics of Dongpo pork. Stewing time and the amounts of added rice wine, sugar and salt were significantly (or even exceedingly significantly) negatively correlated with multiple texture parameters. The texture profile of the fat meat was substantially affected by stewing time, but little affected by the amounts of soy sauce and rice wine. The amounts of water and salt were the factors having little effect on the texture profile of the pork skin, but soy sauce amount and stewing time had a substantial effect, and soy sauce amount had a significant effect on its springiness (P <0.05). The texture profile of the lean meat was substantially affected by stewing time and salt amount.

Equilibrium and Kinetic Studies and Process Optimization of Fluorid Adsorption from Traditional Tibetan Bian Tea Infusion
HE Chun-lei1,LUO Xue-ping1,2,WEI Xiao-hui2,DU Xiao1,*,QIN Wen3
2011, 32(2 ):  18-23.  doi:10.7506/spkx1002-6630-201102005
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In the present study, food-grade tertiary calcium phosphate (TCP) and 731 type anion exchange resin were selected out of 11 kinds of adsorbents as better ones towards fluoride in the infusion of traditional Tibetan Bian tea. To prepare lowfluoride Bian tea cream, equilibrium and kinetic studies of fluoride from Bian tea infusion with a fluoride of 7.18 mg/L were made, and the technological conditions of TCP adsorption for reducing fluoride were optimized by orthogonal array design method. Meanwhile, the Bian tea cream prepared based on optimized fluoride reduction process was evaluated for its sensory quality. TCP was found to have stronger ability to adsorb fluoride at high temperature, with a saturated adsorption quantity of over 10.63 mg/g. The best process parameters for TCP adsorption towards fluoride were as follows: tea infusion temperature 100 ℃; TCP loading 0.7 g/100 mL; and adsorption time 20 min, and the resulting removal rate of fluoride from Bian tea infusion was up to 95.80%. After the reduction of fluoride, concentration was done to obtain a low-fluoride tea cream. The product exhibited a fluoride content of 66.52 mg/kg, 94.80% lower than that of the control (directly concentrated without fluoride reduction), and its redilution had the characteristics of brilliant red color, strong stale flavor, and pure and mild taste.

Polysaccharides from Yacon: Optimization of Ultrasound-assisted Extraction and Hydroxyl Free Radical Scavenging Evaluation
LU Ming-sheng1,WANG Shu-jun1,FANG Yao-wei1,LIU Shu1,XU Xing-quan2,LI Qiu-min1
2011, 32(2 ):  24-27.  doi:10.7506/spkx1002-6630-201102006
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In this study, the process conditions for extracting polysaccharides from yacon fruits with the assistance of ultrasound were optimized by single factor and orthogonal array design methods. The optimal extraction process conditions were determined as follows: ultrasound power, 80 W; extraction temperature, 50 ℃; and material/liquid ratio, 1:30 (g/mL) for an extraction duration of 15 min. Under these conditions, the extraction yield of polysaccharides from yacon fruits was 53.3%. The decreasing order of importance of the four process conditions affecting polysaccharide extraction was extraction duration, extraction temperature, ultrasound power and material/liquid ratio. The crude polysaccharides obtained had strong hydroxyl free radical scavenging effect, with an IC50 of 1.82 mg/mL, which was more than 20-fold increased after protein removal, revealing an IC50 of 0.085 mg/mL.

Microbial Fermentation for Cell Disruption in Combination with Ultrasonic Treatment for the Extraction of Total Flavonoids from Pueraria lobata Tubers
WANG Xing-min1,2,YIN Zhong-yi1,ZHENG Xu-xu1,ZHANG Yu-wen1,ZENG Le1
2011, 32(2 ):  28-31.  doi:10.7506/spkx1002-6630-201102007
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Some enzymes produced during mold fermentation degrade the tissue structures of the residue left after the extraction of starch from Pueraria lobata tubers to facilitate total flavonoids extraction. On the basis of the fact, the development of a method for the extraction of total flavonoids from the residue left after starch extraction using mold fermentation and subsequent ultrasonic treatment was presented in this work. Aspergillus niger and Trichoderma koningii were separately cultured in Pueraria lobata tuber residue to degrade its tissue structures, and Aspergillus niger was the selected strain according to the release of total flavonoids. The parameters affecting Aspergillus niger fermentation, including oxygen condition, soybean meal amount in the fermentation medium, initial fermentation pH and fermentation temperature were investigated by single factor experiments. Additionally, the combined method was compared with sole Aspergillus niger fermentation and sole ultrasonic treatment. The best Aspergillus niger fermentation process was that Pueraria lobata tuber residue suspended in 20-fold volume of water with the addition of 1.0 g of soybean meal, which was adjusted to pH 5, was inoculated with 5% Aspergillus niger seed culture for 60h fermentation at 30 ℃, and the resulting concentration of total flavonoids in the fermentation broth was determined by HPLC to be 3.769μg/mL, which was increased to 5.204 μ g/mL after 5 min ultrasonic treatment. Subsequently, separation and distillation were sequentially done to obtain a crude product with a total flavonoids content of 2.974 mg/g.

Separation and Purification of Aucubin from Eucommia ulmoides Seed Meal
LI Hui1,2,WEN Chi-fu1,2,LI Ya-nan1,PENG Yu-dan1,WANG Lan1,ZHANG Yong-kang1,2
2011, 32(2 ):  32-35.  doi:10.7506/spkx1002-6630-201102008
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The objective of this study was to develop a macroporous resin adsorption method for separating and purifying aucubin in Eucommia ulmoides seed meal extracted into 80% aqueous ethanol solution. Twelve kinds of macroporous resins were compared for differences in their adsorption and desorption performances towards aucubin, and the results indicated that macroporous resins SIPI-7, HZ-820 and S-8 had better abilities to adsorb and desorb aucubin, among which, HZ-820 was considered to be the best resin due to the highest desorption rate. The optimal conditions for the adsorption and desorption of HZ-820 were found to be: sample loading, 0.5 g/g (weight ratio of Eucommia ulmoides seed meal extracted to HZ-820 resin); desorpion solvent, 50% aqueous ethanol solution containing 3% acetic acid at a flow rate of 1.0 mL/min. The high aucubin eluate fractions obtained under such conditions were pooled, condensed and recrystallized into a considerable amount of product containing 96.82% of aucubin.

Ultrasonic-assisted Preparation and Stability Evaluation of Lycopene/β-Cyclodextrin Inclusion Complexes
JIN Xue-yuan,LIU Hong,QIN Xia
2011, 32(2 ):  36-38.  doi:10.7506/spkx1002-6630-201102009
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Recently, β-cyclodextrin inclusion has become a popular strategy to improve the stability of lycopene. In this study, lycopene was prepared into lycopene/β-cyclodextrin inclusion complexes by means of ultrasonic treatment. The preparation process was optimized by single factor and orthogonal array design experiments, in which the effects of ultrasonic power, ultrasonic treatment time and the molar ratio of lycopene to β-cyclodextrin on inclusion rate were explored, and the lycopene/ β-cyclodextrin inclusion complexes prepared were subjected to stability evaluation. The optimal inclusion conditions determined were as follows: ultrasonic power, 250 W; ultrasonic treatment time, 25 min; and the molar ratio of lycopene to β-cyclodextrin, 1:150. A maximum inclusion rate of 73.6% was achieved under these conditions. The included lycopene exhibited a retention rate of 92.2% in 60 d. This study suggests that the preparation of lycopene/β-cyclodextrin inclusion complexes under the assistance of ultrasonic seems to be a promising method for improving the stability of lycopene.

Optimization of the Extraction Process for Gastric Mucin from Porcine Gastric Mucosa
DONG Na,DONG Wen-bin,TIAN Ying
2011, 32(2 ):  39-42.  doi:10.7506/spkx1002-6630-201102010
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This paper presents an optimized extraction process for gastric mucin from porcine gastric mucosa with aqueous hydrochloric acid solution. A series of single factor experiments were carried out to evaluate the effects of material/liquid ratio, hydrochloric acid concentration, extraction temperature and length of extraction time on gastric mucin yield, and the four process conditions were optimized by quadratic orthogonal rotary combination design based on this. The optimal process conditions for the extraction of gastric mucin were determined as follows: liquid/material ratio, 0.61:1 (mL/g); hydrochloric acid concentration, 5.4%; extraction temperature, 44.9 ℃; and extraction duration 2.0 h. Under these conditions, the yield of gastric mucin was 3.74%, and the product obtained contained 8.7% of total nitrogen and 26.3% of reducing substances and met the quality requirements stipulated by the Ministerial Standards of Chemical Medicine. Thus, the optimized extraction process is feasible for the preparation of gastric mucin.

Study on microencapsulation of lutein
WANG Chuang1,SONG Jiang-feng2,3,LI Da-jing1,2,3,*,LIU Chun-quan2,3
2011, 32(2 ):  43-47.  doi:10.7506/spkx1002-6630-201102011
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Lutein microcapsules were prepared sequentially by emulsification, homogenization and spray-drying using lutein crystal as the core material and octenylsuccinate starch in combination with sucrose as the wall material in this study. The processing technology was optimized by single factor and orthogonal array design experiments. The weight percentage of sucrose occupying the compound wall material of 10%, compound wall material concentration of 0.15g/mL, core material/wall material weight ratio of 1:15, the weight ratio of emulsifier to wall material of 0.6%, homogenization number with colloid miller of 2, feeding speed of 400 mL/h, air inlet temperature of 160 ℃ and air outlet temperature of 80 ℃ were found optimal, and the product obtained under these conditions presented 92.35% microencapsulation efficiency, 90.27% yield and good quality.

Effect of β-Glucosidase Treatment Conditions on Vanillin Content in Vanilla Extract
JIANG Xin1,2,HAN Bing-jun2,PENG Li-xu3,*
2011, 32(2 ):  48-52.  doi:10.7506/spkx1002-6630-201102012
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The extract rich in vanilla, which was prepared by Soxhelt extraction, was treated with β-glucosidase to increase vanillin content, and the treatment conditions were investigated. On the basis of single factor experiments, the process optimization for the enzymolysis process of the extract was performed using uniform design coupled with partial least square regression analysis. The analytical method used for the determination of vanilla was HPLC, and data processing was carried out using DPS software. The optimal enzymolysis conditions were determined to be: reaction temperature of 45 ℃, reaction time of 24 h, stirring speed of 150 r/min, and material/liquid ratio of 1:6. After β-glucosidase treatment under the optimized conditions, the theoretical amount of vanilla in 20 g of the extract was 1.531 g, with a relative error of smaller than 10% when compared to the experimental amount.

Extraction and Purification of Polysaccharides from Sphacelotheca sorghi (Link) Clint
YU Miao,SHI Tai-yuan,MA Tao,LI Li-feng,CHI Ji-jie,WANG Chen,HAN Yan-qiu,GAO Ya
2011, 32(2 ):  53-56.  doi:10.7506/spkx1002-6630-201102013
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The process of polysaccharide extraction from Sphacelotheca sorghi (Link) Clint was investigated in this study. The effects of extraction number and temperature, length of extraction time, and material/liquid ratio on polysaccharide yield were explored, and the optimization of the four process conciliations was achieved by orthogonal array design method based on single factor experiments. Extraction temperature was found to have the most important effect on polysaccharide yield, sequentially followed by material/liquid ratio, extraction number and length of extraction time. The optimal extraction process for polysaccharides was Sphacelotheca sorghi (Link) Clint was extracted three times for 2 h each time with a 20-fold volume of water in 80 ℃ water bath, and the resulting yield of crude water-soluble polysaccharides was approximately 7%. The purification of the crude product obtained was performed by using tannic acid and activated carbon together, and as a result, its purity was increased to 75.63%.

Separation, Purification and Structural Analysis of Flavonoids from Diospyros kaki Leaves
SUN Hua-peng1,ZHONG Xiao-hong1,*,LU Ying1,2,ZHOU Zhou1
2011, 32(2 ):  57-61.  doi:10.7506/spkx1002-6630-201102014
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In this study, high-speed countercurrent chromatography (HSCCC) followed by preparative high performance liquid chromatography (HPLC) was used to separate and purify flavonoid monomers from the crude ethyl acetate extract from Diospyros kaki leaves. Meanwhile, the flavonoid monomers obtained were preliminarily identified by color development reaction and further structurally characterized by UV spectroscopy and mass spectroscopy. The HSCCC separation of flavonoids was achieved by using a solvent system composed of ethylacetate, methanol and water (5:1:5, V/V) at a flow rate of 1.5 mL/min and setting the rotational speed at 850 r/min with a detection wavelength set at 254 nm. For further separation, the separated fractions were then applied to preparative HPLC, and 4 flavonoid compounds, named A-Ⅱ, A-Ⅲ, B-Ⅱ and B-Ⅲ, were obtained. A-II and A-III might be quercetin flavonoids, and B-Ⅱ and B-Ⅲ might be kaemoferol.

Effect of Edible Film Coating on Reducing Oil Uptake in Deep-fried Fish Blocks
LING Jun-jie1,WANG Zhi-geng1,*,CHENG Hua-ping2,YU Long-mei3,LIU Tong-ge3
2011, 32(2 ):  62-65.  doi:10.7506/spkx1002-6630-201102015
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The objective of this study was the optimization of edible film coating treatment for reducing oil uptake in deepfried grass carp fish blocks. The effects of different film coating agents (CMC-Na, Arabic gum and sodium alginate), the time point of film coating agent addition, the concentrations of CMC-Na and sodium alginate (added separately) and the ratio of CMC-Na to sodium alginate when added together at 1% in total on oil uptake were probed. In comparison with the control (without the addition of any film coating agent), CMC-Na, Arabic gum and sodium alginate were all able to significantly (P <0.05) inhibit oil uptake in deep-fried fish blocks, showing inhibition rates of 21.33%, 16.97% and 9.99% when added at 2% level, respectively. Optimum reduction of oil uptake was obtained when the above films were separately used in the coating processing. Oil uptake was best inhibited by combined use of CMC-Na and sodium alginate at a mixing ratio of 1:2, which showed an inhibition rate of 34.54% at a total addition concentration of 1%.

Optimization of Ultrasound-assisted Extraction of Phenolic Compounds from Robinia pseudoacacia L. Flowers by Response Surface Methodology
WANG Xiao-yang,TANG Lin*,ZHAO Lei
2011, 32(2 ):  66-70.  doi:10.7506/spkx1002-6630-201102016
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Objective: The optimization of the extraction process of phenolic compounds from Robinia pseudoacacia L.flowers under ultrasound assistance was achieved by response surface methodology to maximize phenolic extraction yield. Methods: On the basis of single-factor experiments, Box-Behnken central composite design (CCD) involving four variables at three levels was utilized to set up a quadratic polynomial regression equation for phenolic extraction yield as function of extraction temperature, ultrasound power, length of ultrasound treatment time and material/liquid ratio, and the pairwise interactive effects of the above four variables on their function were investigated by response surface analysis. Results: The optimum conditions for extracting phenolic compounds from Robinia pseudoacacia L.flowers were found to be: 36 min ultrasound treatment at 110 W power for extracting the raw material with a 20-fold volume of 60% aqueous ethanol solution at 35 ℃. Under these optimum conditions, the yield of polyphenols was 7.891%.

Preparation and Properties of Acetylated Acid Modified Waxy Corn Starch
TANG Hong-bo1,SUN Min2,LI Yan-ping1,MA Bing-jie1
2011, 32(2 ):  71-75.  doi:10.7506/spkx1002-6630-201102017
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In this study, the process for preparing acetylated acid modified waxy corn starch from waxy corn starch by acetic anhydride acetylation under the catalysis of sodium hydroxide and subsequent hydrochloric acid hydrolysis, in which anhydrous sodium sulfate was first added to starch milk as a swelling inhibitor, was studied. Meanwhile, the modified starch prepared was functionally characterized. Waxy corn starch had been modified by hydrochloric acid was acetylated by acetic anhydride to explore the effects of the acetylation reaction conditions, including temperature, time, pH, acetic anhydride loading, and anhydrous sodium sulfate loading, on starch substitute degree. Additionally, the effect of the sequential order of acetylation and acidic hydrolysis on starch substitute degree and fluidity was evaluated when the reaction conditions of acidic hydrolysis and acetylation were both kept unchanged, and the results showed no effect. The above reaction conditions were all found to affect the preparation of acetylated acid modified waxy corn starch. The optimum conditions for the acetylation of hydrochloric acidmodified waxy corn starch with acetic anhydride were determined as follows: reaction at 25 ℃, pH 8.5 for 50 min under the catalysis of 1.5% anhydrous sodium sulfate. After the optimized acetylation, hydrochloric acid-modified waxy corn starch showed an increase in both transparency and freeze-thaw stability, which was positively correlated with substitute degree. Starch retrogradation, however, was not affected by acetylation.

Extraction, Purification and Characterization of Morin from Xinjiang Black Mulberry (Morus nigra L.) Tree Branch
ZHOU Lin,XU Li*,YU Mao-de,LIU Jun-chi,HUANG Xian-zhi
2011, 32(2 ):  76-78.  doi:10.7506/spkx1002-6630-201102018
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A process for the preparation of morin from Xinjiang black mulberry (Morus nigra L.) tree branch using organic solvent extraction and polyamide resin column chromatographic purification is presented in this paper. Thin layer chromatography and HPLC were integratively used for the qualitative analysis of morin. The 95% ethanol extract from black mulberry tree branch was reextracted separately with ethyl acetate and chloroform, and the thin layer chromatographic results showed that morin was present in the ethyl acetate phase rather than the chloroform phase. High-purity morin was obtained after twice purification on polyamide resin column, which displayed excellent characteristic adsorption at 370 nm wavelength. Thus, polyamide resin is a promising material for the purification of flavonoid, like morin.

Optimization of Enzymatic Extraction of Polysaccharide from Longan (Dimocarpus longan Lour.) Pulp Using Response Surface Methodology
HE Yin,WANG Qiang*,ZHONG Kui
2011, 32(2 ):  79-83.  doi:10.7506/spkx1002-6630-201102019
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Polysaccharide in fresh longan pulp was extracted with the assistance of enzymatic hydrolysis. Cellulase gave relatively higher polysaccharide yield than pectinase and neutral protease, and was chosen for further study. The effects of cellulase concentration, the ratio of water to material, and extraction temperature and time on the yield of polysaccharide was investigated by single factor experiments. Subsequently, a quadratic regression rotational combinational design involving the above four factors at five levels was employed, and data obtained were analyzed with response surface methodology. Polysaccharide yield was most significantly affected by cellulase concentration, followed by extraction time, temperature and water-tomaterial ratio. An optimum polysaccharide yield of (12.23 ± 0.15) mg/g (on the basis of dried longan biomass weight) was obtained when longan pulp was treated with 1.2% cellulase at 45.0 ℃ for 187.0 min in a water-to-material ratio of 6:1, which was much higher than that obtained by conventional hot extraction.

Optimization of Microwave-assisted Extraction of Saponins from the Whole Plant of Alternant heraphiloxeroides (Mart.) Griseb
CAI Ling-yun1,2,LI Yun-xiang2,HE Shun-mei2,PAN Qi-bing2,SU Yuan-rong1
2011, 32(2 ):  84-87.  doi:10.7506/spkx1002-6630-201102020
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Objective: The development of an optimal process for the microwave-assisted extraction of saponins from the whole plant of Alteman theraphiloxeroides (Mart.) Griseb (APG) in presented in this paper. Methods: Microwave was used for the extraction of saponins with aqueous methanol solution as an assistant approach, and process optimization was achieved by single factor and orthogonal array design experiments. The quantitative analysis of saponins was performed using oleanolic acid as a reference substance, which showed maximum adsorption at 570 nm wavelength, with a calibration equation of Y = 1.904C +0.0054 (r = 0.9990). Results: The optimum process conditions for the extraction of saponins were 20 s microwave treatment at 640 W power for intermittently extracting with a 20-fold volume of 20% aqueous solution for 4 times. Conclusion: The developed extraction process is easy to operate and reliable.

Optimization of Extraction Processes of Pigment and Pectin from Pyracantha fortuneana Fruits
LIANG Xian-chang1,LI Jia-xing1,*,HUANG Shou-en2,HUANG Cheng3,WANG Xiao-yong4
2011, 32(2 ):  88-92.  doi:10.7506/spkx1002-6630-201102021
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The fruit pigment of Pyracantha fortuneana was extracted into aqueous ethanol solution, and the residue was then hydrolyzed with hydrochloric acid to obtain pectin existing in the supernatant. Orthogonal array designs L9(33) and L9(34) were used to optimize the extraction processes for pigment and pectin. The optimum conditions for pigment extraction were as follows: extraction temperature 90 ℃; extraction time 2 h; and solid-to-liquid ratio 1:20 (m/V), which gave a crude pigment yield of 25.31%, and those for pectin extraction were as follows: extraction temperature 90 ℃; extraction time 2.5 h; initial pH 1.5; and solid-to-liquid ratio 1:25 (m/V), under which a pectin yield of 4.72% was achieved. The two processes are of low-cost equipment investment and simplicity, thereby being suitable for massive production.

Response Surface Optimization of Alkaline Protease Hydrolysis for Collagen Extraction from Rana amurensis Boulenger Residue after Oil Extraction
ZHANG Gen-sheng,FAN Ai-yue,HAN Bing,HUANG Qiao-li,YUE Xiao-xia
2011, 32(2 ):  93-97.  doi:10.7506/spkx1002-6630-201102022
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The residue of Rana amurensis Boulenger after oil extraction was hydrolyzed by alkaline protease to extract collagen into the supernatant. The effects of initial hydrolysis pH, enzyme loading, and hydrolysis temperature and time on collagen yield were investigated by single factor experiments and response surface methodology. The optimum values of the four conditions for improved collagen extraction were determined as follows: initial hydrolysis pH 10; enzyme loading 1.5%; hydrolysis temperature 50 ℃; and hydrolysis time 2.5 h. Under the optimized conditions, a collagen yield of 55.38% was attained, with a product purity of 64.15%.

Process Optimization for the Ultrasonic-assisted Extraction of Allium mongolicum Regel Seed Polysaccharides Using Response Surface Methodology
ZHANG Jun-ping1,2,HOU Xi-lin1,2,*,DONG Hai-yan1,2,YU Tian1,MA Zhi-hu1,2
2011, 32(2 ):  98-103.  doi:10.7506/spkx1002-6630-201102023
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Objective: The ultrasonic-assisted extraction process for polysaccharides from the residue of Allium mongolicum Regel seeds after the oil of extraction with supercritical carbon dioxide was optimized using response surface methodology. Methods: On the basis of single factor experiments, a three-factor, three-level Box-Behnken central composite design (CCD) was utilized for mathematical modeling for polysaccharide yield as a response to extraction temperature and time as well as material/water ratio, followed by response surface analysis of the relationship between the function and the three variables. Results: The optimum conditions for the extraction of Allium mongolicum Regel seed polysaccharides were as follows: water/ material ratio, 48.0:1; ultrasonic power, 300 W; extraction temperature, 73.1 ℃; extraction time, 1.6 h; and extraction number, 2. Under such conditions, the model-predicted and experimental values of polysaccharide yield were 7.59% and 7.47%, respectively, revealing 1.58% relative error between them. Conclusion: Ultrasonic treatment can substantially shorten the time required for polysaccharide extraction, and the developed extraction process is simple, reliable and highly efficient.

Process Optimization for Total Polyphenol Extraction from the Tree Branch Bark of Xinjiang Black Mulberry (Morus nigra L.) by Response Surface Methodology
WU Chun1,XU Li1,*,LIU Jun-chi1,HUANG Xian-zhi1,MAIMAITI Yi-ming2
2011, 32(2 ):  104-107.  doi:10.7506/spkx1002-6630-201102024
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The objective of this study was the optimization of the extraction process for total polyphenols from the tree branch bark of Xinjiang black mulberry (Morus nigra L.) by response surface methodology. Based on single factor experiments, a threefactor, three-level Box-Behnken central composite design (CCD) coupled with response surface analysis (RSM) was employed to probe the effects of ethanol concentration, extraction temperature and length of extraction time on the yield of total polyphenols. It was found that the best extraction conditions were as follows: ethanol concentration, 78%; and liquid/material ratio, 30:1 (mL/g) for an extraction duration of 240 min at 70 ℃, and that a maximum total polyphenol yield of 0.793% under such conditions. The extraction process proves stable and reliable and is applicable for the production of polyphenols.

Process Optimization for the Ultrasonic Extraction of Total Saponins from Hetian-jade Jujube
ZHANG Na,CHEN Jin-ping*,YAN Jing,LI Ren-jie
2011, 32(2 ):  108-110.  doi:10.7506/spkx1002-6630-201102025
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Total saponins from Hetian-jade jujube were extracted by an orthogonal array design and determined by color development reaction with vanillin and perchloric acid. The results showed that the optimal extraction conditions were as follows: 70% of ethanol concentration, 1:12 of ratio of raw material to liquid, and 30 min of extraction time. The content of total saponins in the crude extract obtained under the above conditions was 9.358 mg/g. A convenient and quick process has been presented for the extraction of total saponins from Hetian-jade jujube.

Extraction and Nitrosation Inhibition Activity of Total Flavonoids from Punica granatum L. Peel
WU Jia,XIE Cheng-xi*
2011, 32(2 ):  111-114.  doi:10.7506/spkx1002-6630-201102026
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The optimal conditions for total flavonoids extraction from Punica granatum L. peel were studied by orthogonal array design and their abilities to scavenge nitrite and inhibit nitrosamines were tested spectrophotometrically. A maximum extraction yield of 84.8 mg flavonoids/g peel was obtained when a 60-fold volume of 60% aqueous ethanol solution was utilized to extract Punica granatum L. peel for 40 min with the assistance of sonication at 150 mA electric current intensity, and the crude extract exhibited a maximum sodium nitrite scavenging rate of 81.2% and a maximum block rate of 67.0% against the synthesis of nitrosamines, suggesting a strong ability to inhibit nitrosation.

Macroporous Resin Adsorption for the Separation of Sea Asparagus Flavonoids
XU Qing,LU Ying-ying,XIN Jian-mei,LUO Hong-yu*
2011, 32(2 ):  115-119.  doi:10.7506/spkx1002-6630-201102027
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Two types of macroporous resins, D101 and AB-8, were comparatively studied for their static adsorption and desorption performances towards sea asparagus flavonoids, and AB-8 was the selected resin for the separation and purification of the crude ethanol extract (rich in flavonoids) from sea asparagus prepared with microwave assistance. The optimum process for the adsorption of sea asparagus flavonoids onto AB-8 was that the crude extract was adjusted to a concentration of 0.5 mg/mL at pH 6 before loading at a flow rate of 1 mL/min. The flowing of 75% ethanol aqueous solution through AB-8 column at a rate of 2 mL/min was found optimum for the desorption of sea asparagus flavonoids, resulting in a desorption rate of 85.25%. The adsorption/desorption process is ease to operate and displays a good separation effect, thereby being suitable for the industrial separation and purification of sea asparagus flavonoids.

Optimization of Process Conditions for Pilot-scale Supercritical Carbon Dioxide Extraction of Essential Oil from Xuefeng Tangerine Peel
CHEN Ling-juan1,2,ZHAO Liang-zhong2,*,LIN Qin-lu1,XIA Xiang2,HUANG Da-chuan2
2011, 32(2 ):  120-123.  doi:10.7506/spkx1002-6630-201102028
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Supercritical carbon dioxide fluid extraction (SFE) technique was utilized to simultaneously extract the essential oil compounds and pigments in Xuefeng tangerine peel. To maximize the yield of crude extract from tangerine peel, the process conditions for the pilot-scale extraction of Xuefeng tangerine peel were optimized by orthogonal array design method. The optimum pilot-scale extraction conditions were determined as follows: CO2 flow rate of 21.27 L/min for an extraction duration of 1 h at 30 MPa, 40 ℃, which yielded 4.56% of crude extract (pigments plus essential oil). The crude extract obtained under these conditions was separated with a separalory funnel, and the oil phase was then centrifugated at 12000 r/min for 10 min to harvest the upper phase, which was analyzed by GC-MS for its volatile composition. A total of 21 volatile compounds were detected in the analyte, and the prominent compounds were D-limonene, α-farnesene, calarene, β-elemene, β-pinene, and so on and the total content of D-limonene and α-farnesene exceeded 90%.

Comparative Study of DPPH Free Radical Scavenging Activity of Germ Protein of Wheat Grown in Heilongjiang Enzymolyzed in Different Ways
YANG Ming-duo1,2,WU Ying-ying1,2,ZHANG Hong-wei1,2,3
2011, 32(2 ):  124-126.  doi:10.7506/spkx1002-6630-201102029
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In the present study, four different types of proteases were utilized to hydrolyze germ protein of wheat grown in Heilongjiang (prepared by alkaline extraction and subsequent acid precipitation) in different ways, i.e., single-enzyme hydrolysis as well as one-step and stepwise double-enzyme hydrolysis. After the completion of hydrolysis, degree of hydrolysis and DPPH radical scavenging activity were measured to comparatively study the relationship between hydrolysis way and free radical scavenging effect of wheat germ protein hydrolysate. Among four proteases, alkaline protease hydrolysis resulted in a hydrolysate with the highest DPPH radical scavenging activity (the scavenging rate was 39.74%) when used separately. As for double-enzyme way, stepwise hydrolysis was superior to one-step hydrolysis, and sequential hydrolysis with alkaline protease followed by papain was the best way for improved DPPH radical scavenging activity of wheat germ protein hydrolysate, reaching 45.36%.

Optimization of Flavonoids Extraction from Fructus Cannabis by Response Surface Methodology
ZHAO Xuan1,LI Hong-liang2,ZHANG Hui-mei1
2011, 32(2 ):  127-131.  doi:10.7506/spkx1002-6630-201102030
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To optimize the process for flavnonoids extraction from Fructus Cannabis, a series of single-factor experiments were made to investigate the effects of extraction solvent type, ethanol concentration, extraction duration and temperature, liquid-tosolid ratio ratio and the degree of pulverization of the raw material on flavnonoids yield, and based on this, a 19-run response surface design involving 5 of the above 6 factors at 3 levels was generated by the Design-Expert software according to the central composite design principle and experimental data obtained were subjected to quadratic regression analysis to create a mathematical model describing flavnonoids extraction. The optimal extraction conditions were found to be: ethanol concentration of 70% and liquid-to-solid ratio of 35:1 for an extraction duration of 2.5 h at 75 ℃. Under these conditions, the yield of flavonoids was 17.80 mg/g.

Optimization of Extraction Process for Total Flavonoids from Xinjiang Propolis and Its Flavonoid Composition as Analyzed by GC-MS
Munuerding TOHENIYAZI,Aierken AIMIER,Yimit RAHMAN1
2011, 32(2 ):  132-135.  doi:10.7506/spkx1002-6630-201102031
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Objective: The optimal process for total flavonoids extraction from Xinjiang propolis was determined, and the flavonoid composition of Xinjiang propolis was analyzed. Methods: Combined single factor and orthogonal array design methods were used to optimize the process conditions for total flavonoids extraction. The quantitative analysis of flavonoids was performed spectrometrically at 502 nm using rutin as a reference substance. Flavonoid composition analysis was achieved by using GC-MS. Results: The optimal extraction conditions were using a 9-fold volume of 95% ethanol as an extraction solvent for the 48 h extraction of the raw material at 50 ℃. Under these conditions, the extraction efficiency of total flavonoids was 10.82%. Conclusion: The extraction process and the analytical method are both reliable and simple, which can provide useful approaches for the extraction and exploitation of total flavonoids from Xinjiang propolis.

Analysis & Detection
Molecular Identification and Phylogenetic Analysis of Functional Food Dendrobium officinale and Its Adulterants
DING Ge1,2,ZHANG Dai-zhen3,ZHANG Wei-chao4,DING Xiao-yu2,*
2011, 32(2 ):  141-145.  doi:10.7506/spkx1002-6630-201102033
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To develop a simple and reproducible molecular method to discriminate between functional food Dendrobium officinale and its adulterants, PCR products of the matK gene were sequenced to find single nucleotide polymorphism (SNP) sites. Then allele-specific PCR primers were designed according to the identified SNP sites. The phylogeny of D. officinale and its adulterants were analyzed by Mega 3.0. It was found that D. officinale and its adulterants can be discriminated by SNP sites and allele-specific PCR primers. There was apparent genetic difference between all the samples tested. It is concluded that this method can be used to discriminate between D. officinale and its adulterants rapidly and accurately.
Determination of Molecular Weight Distribution of Garlic Oligosaccharide and Polysaccharide by Matrix-assisted Laser Desorption/Ionization Mass Spectrometry
HUANG Xue-song,YAN Feng-chao,WU Jian-zhong
2011, 32(2 ):  146-149.  doi:10.7506/spkx1002-6630-201102034
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A series of garlic oligosaccharide and polysaccharide samples were prepared by precipitation with varying volumes of acetone or ethanol, and their molecular weight distributions were determined by matrix assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS). Three-fold volume of acetone could precipitate more oligosaccharide and polysaccharide than 4-fold volume of ethanol. The molecular weight distribution of oligosaccharide and polysaccharide was from 362 to 2811 u, and can be adjusted by applying different proportions of precipitators.
Enzymatic Preparation and Electrospray Ionization Mass Spectrometry (ESI-MS) Analysis of Alginate Oligosaccharides
LI Xiao,WANG Hong-min,HUANG Lin-juan,WANG Zhong-fu
2011, 32(2 ):  150-153.  doi:10.7506/spkx1002-6630-201102035
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The enzymatic preparation of alginate oligosaccharides with different degrees of plormerization (DPs) from algin was achieved by using 1805 enzyme, an enzyme obtained from the 1805 group of Dalian Institute of Chemical Physics, Chinese Academy of Sciences. Hydrolyzed algin was analyzed for its contents of total sugar and uronic acid and monosaccharide composition, and meanwhile UV spectrometrical analysis at 280 nm was performed to see whether protein is present in it. In addition, the mixture of oligosaccharides was separated by silica column chromatography, and the separated fractions were analyzed by thin layer chromatography (TLC) and electrospray ionization mass spectrometry (ESI-MS). The hydrolysis products of algin were a mixture of oligosaccharides mainly with a DP of 2-10. Monomers consisting of 2-5 glucose units were substantially separated by silica column chromatography. These investigations will provide some useful references for the preparation, separation and identification of alginate oligosaccharides.
Determination of Shikimic Acid in Chinese Star Anise Fruit by Ion Chromatography with Suppressed Conductivity Detection
HU Chao-juan,ZHOU Guang-ming,YU Na
2011, 32(2 ):  154-156.  doi:10.7506/spkx1002-6630-201102036
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A method for the determination of shikimic acid in Chinese star anise (Illicium verum Hook.f.) fruit by ion chromatography with suppressed conductivity detection was developed. The chromatographic separation was conducted on Metrohm A supp 4 (4 mm× 250 mm) anion exchange column, using 1.8 mmol/L Na2CO3 + 1.7 mmol/L NaHCO3 as a mobile phase at a flow rate of 0.8 mL/min. The total analysis time was 15 min. The linear range was between 1 mg/L and 100 mg/L and the correlation coefficient was 0.9993. A detection limit of 0.02~0.8 mg/L was achieved under optimized separation conditions. The RSD of peak area was 1.04% (n = 6), and the RSD of retention time was 0.47%. The average spike recoveries were between 97.3% and 98.9%. This method is fast, simple and reliable.
Rapid Determination of Total Bacterial Number in Liquid Foods by A Flow Cytometry Method
IU Dao-liang,ZHAO Zhan-min,HU Lian-xia,ZHANG Jun-feng,SUN Xiao-xia
2011, 32(2 ):  157-163.  doi:10.7506/spkx1002-6630-201102037
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The total numbers of bacteria in liquid foods such as milk and fruit juice were determined by a flow cytometry (FCM) method. A detection limit of 10 CFU/mL was achieved by removing the non-microorganism particles in fruit juice through membrane filtration and centrifugation. The reproducibility was tested to verify the reliability of the method in determining milks by comparing with the standard plate count (SPC) method. The FCM result was linearly correlated with that of SPC within a certain concentration range. FCM is faster and more accurate than SPC methods in determining the total number of bacteria in liquid samples.
Evaluation of Aroma-producing Characteristics of Saccharomyces cerevisiae Strains by Electronic Nose
LIU Ning,MA Jie,LIU Yan-lin
2011, 32(2 ):  164-167.  doi:10.7506/spkx1002-6630-201102038
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An electronic nose (PEN3) was used to characterize and classify wines fermented by different strains of Saccharomyces cerevisiae. The aroma components emanating from the wines were dynamically sampled by a PEN3 system and analysis of the acquired data was made comparatively using principal component analysis (PCA) and linear discrimination analysis (LDA). The results showed that electronic nose was able to differentiate the wine samples following either analysis of PCA or LDA. The aroma-producing characteristics of Saccharomyces cerevisiae was of strain-specific diversity. Meanwhile loadings analysis showed most of the tested sensors played an important role in analyzing aroma difference, with exception of the seventh, ninth and tenth sensors.
Volatile Profile and Terpene Index of Wild Tea Leaves in Sichuan-Chongqing Region
WANG Heng-hong,TONG Hua-rong,LI Lan-ying,ZHU Ling
2011, 32(2 ):  168-172.  doi:10.7506/spkx1002-6630-201102039
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To analyze the volatile profiles and phylogenetic relationship of different varieties of wild tea tree leaves in the climatic region of Sichuan and Chongqing, baked green tea samples processed from wild (including parental and first filial generations) and domesticated (Fuding Dabai Cha tea) varieties of fresh tea tree leaves were extracted by steam distillation extraction (SDE) for their volatile oils, and the oils were analyzed by GC-MS. A total of 71 compound were detected including alcohols, such as linalool and its oxides, geraniol, nerol and α-terpinol; terpenoides, such as β-phellandrene,β-myrcene, limonene,α-cedrene, caryophyllenev,α-farnesene; aldehydes, such as β-Cyclocitral, benzaldehyde, (E)-2-hexenal; organic ester compounds, such as hexadecanoic acid methyl ester and dibutyl phthalate; five typical green tea aroma compounds, such as cis-Jasmone, α-Inone, and so on; and several amine, hydrocarbon, nap, anthracene, and acid compounds as well. Terpene analysis showed that the parental generation of wild tea trees had a higher terpene index (TI) than their first filial generation and Fuding Dabai Cha tea. Thus, TI is one of the important evidence for the differentiation of tea tree resources.
Multi-residue Analysis of Organophosphorus Pesticides in Hotpot Condiment by Gas Chromatography
CAO Shu-rui,WANG Guo-min,ZHANG Lei,WANG Bo,ZHENG Guo-can,LI Ying-guo,ZHANG Jin-zhong
2011, 32(2 ):  173-176.  doi:10.7506/spkx1002-6630-201102040
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A multi-residue analytical method for the determination of 17 organophosphorus pesticides in hotpot condiment using gas chromatography equipped with a DB 1701 capillary column and a flame phosphorous detector (FPD) was developed. Gel permeation chromatography (GPC) and solid phase extraction were used to remove fats and pigments in hotpot condiment. The spiked recoveries ranged from 81.83% to 105.4% with a relative standard derivation (RSD) varying from 0.9% to 5.2%, and the detection limits varied from 1.0μg/kg to 5.3μg/kg. In conclusion, the developed method is rapid, accurate and sensitive can meet the requirements for the multi-residue analysis of organophosphorus in hotpot condiment.
Comparative Analysis of Fatty Acid Profile in Black and White Peanuts
HOU Dong-yan,HUI Rui-hua,LI Tie-chun,LIU Xiao-yuan
2011, 32(2 ):  177-179.  doi:10.7506/spkx1002-6630-201102041
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The fatty acid profiles of black and white peanuts were analyzed and compared. The lipid fractions in black and white peanuts were extracted by Soxhlet extraction, followed by esterification with a potassium hydroxide/methanol solution. The fatty acid methyl esters (FAME) were analyzed by gas chromatography-mass spectrometry (GC-MS). A total of 19 and 17 fatty acids were identified in black and white peanuts, respectively. Unsaturated fatty acids represented 61.07% and 67.59% of the total fatty acids in black and white peanuts, respectively.
Determination of 14 Mono-phenols in Dry Red Wines by HPLC
2011, 32(2 ):  180-183. 
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The contents of 14 mono-phenols in six Cabernet Sauvignon dry red wines with different aging times or different geographical origins of grape were determined using a HPLC method. The chromatographic separation was performed on a ZORBAX SB-C18 column at 30 ℃ with an acetonitrile/acetic acid/water mixture as a mobile phase at a flow rate of 1.0 mL/min and the detection wavelength was set at 280 nm. The contents of 14 mono-phenols in Cabernet Sauvignon wine varied with geographical origin of grape, and higher contents of gallic acid, catechin, and epicatechin were found in all the six wine samples. Cabernet Sauvignon wines with different aging times from the same region differed in their mono-phenols content as well. The contents of several major mono-phenols decreased with increasing aging time, while a few others exhibited an opposite change.
Microwave Airtight Digestion and Atomic Absorption Spectrophotometric Analysis of Cadmium in Goose Liver
SI Wen-hui,LI Ke-jian,ZHENG Li-qing,FANG Zhi-cheng
2011, 32(2 ):  184-186.  doi:10.7506/spkx1002-6630-201102043
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Goose liver was digested with mixed acids by a microwave system under a gradient pressure program at a power output of 600 W to determine the content of cadmium by an atomic absorption spectrometry method. The limit of detection was 0.36μg/mL, the precision RSD of 5 replicate determinations was 3.03%, and the spike recoveries in 5 samples were between 97.09% and 100.86%. This method may reduce the sample contamination problem effectively due to thorough exposure of samples to mixed acid for rapid digestion in an airtight environment, and is simple, convenient, quick and accurate.
Simultaneous Determination of Six Carbamate Pesticide Residues in Milk by HPLC-ESI-MS/MS
TIAN Hong-zhe,ZHAO Ying-bo,ZHOU Yan-ming
2011, 32(2 ):  187-190.  doi:10.7506/spkx1002-6630-201102044
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A high performance liquid chromatography-ion trap mass spectrometric (HPLC-ESI-MS/MS) method was developed to determine six carbamate pesticide residues in milk samples simultaneously. Samples were extracted with acetonitrile, cleaned up on an Oasis HLB-SPE column, separated on a C18 column using mixed methanol and 0.02 mol/L ammonium acetate as a mobile phase (60:40, V/V) by gradient elution, followed by multiple reaction monitoring (MRM) mode detection. The limits of quantification ranged from 1.0 to 10.0μg/kg. The average recoveries in spiked samples were between 79.21% and 91.38% with relative standard deviations from 3.44% to 5.71%. The proposed method can meet the current requirements for the analysis residual pesticides.
HPLC Determination of Chlorogenic Acids in Flowers, Branches and Leaves of Prunus mume
SHI Jia-yi,ZHANG Ying
2011, 32(2 ):  191-194.  doi:10.7506/spkx1002-6630-201102045
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Three chlorogenic acid isomers, namely, neochlorogenic acid, chlorogenic acid, and cryptochlorogenic acid in the flowers, branches, and leaves of Prunus mume were simultaneously determine by a HPLC method. The samples were separated by a Luna C18 column using 2% acetic acid and acetonitrile as a mixed mobile phase. The detection wavelength was 328 nm. The analytical method displayed a wide linear range of 5 to 200μg/mL for the three chlorogenic acid isomers. The detection limits were 0.21, 0.16μg/mL and 0.29μg/mL for neochlorogenic acid, chlorogenic acid, and cryptochlorogenic acid, respectively. The contents of total chlorogenic acid isomers were (48.26 ± 0.11), (10.82 ± 0.04) mg/g, and (21.33 ± 0.08) mg/g in the flowers, branches and leaves of Prunus mume, respectively. In conclusion, this method is simple, rapid, accurate and sensitive, and Prunus mume is a good source of chlorogenic acids.
Determination of Lead, Arsenic, Cadmium, Chromium, Copper, Manganese, Zinc and Nickel in Spices by Inductively Coupled Plasma Mass Spectrometry with Microwave Digestion
XIE Nan,GE Yu,XU Hong-bin,CAO Cheng-ming
2011, 32(2 ):  195-197.  doi:10.7506/spkx1002-6630-201102046
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Inductively coupled plasma mass spectrometry (ICP-MS) with microwave digestion was applied to determine lead, arsenic, cadmium, chromium, copper, manganese, zinc and nickel in spices. The linear range of the developed ICP-MS method was from 0 to 500 ng/mL (r > 0.9995). The detection limits were between 0.009 ng/mL and 0.42 ng/mL. The precision of the method was evaluated with a relative standard derivation (RSD) of lower than 5%, and the average recoveries in a sample spiked at three levels were in the range of 88% to 109% (n = 11). The results of determining various elements in three standard reference materials of GBW08521, GBW(E)080684 and GBW07605 (GSV-4) were all within the ranges of standard values. This method proves good simplicity, sensitivity and accuracy in the determination of heavy metal elements in spices.
HPLC Determination of Fructose, Glucose and Sucrose in Sugarcane Internode
LU Ping-jie,DAI Rong-chun,YE Bing-ying,LIN Rong-hua,HE Wen-jin,CHEN You-qiang,CHEN Ru-kai
2011, 32(2 ):  198-200.  doi:10.7506/spkx1002-6630-201102047
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Fructose, glucose and sucrose contents in sugarcane internodes were determined using high performance liquid chromatography with refractive index detector (RID). The chromatographic separation was achieved on an Agilent Zorbax carbohydrate column (4.6 mm× 250 mm, 5 μm), which was held at a constant temperature of 30 ℃, using a mobile phase composed of acetonitrile and water (75:25, V/V) at a flow rate of 1.0 mL/min. RID temperature was set as 35 ℃. Average spike recoveries for 5 replicate determinations of three saccharides were found in a range of 97.84% to 99.12%, with a relative standard deviation (RSD) between 0.82% and 0.87%. The developed calibration curves displayed good linearity over a concentration range of 0.625 to 20 mg/mL, with a correlation coefficient exceeding 0.9982 (n = 6). This method has been applied to determine two different varieties sugarcane internodes with satisfying results.
Comparison of Four Methods for Determining Protein Content in Crude Acaudina molpadioides Polysaccharides
U Wei,CHANG Yao-guang,XUE Chang-hu,WU Xiao-lin
2011, 32(2 ):  201-204.  doi:10.7506/spkx1002-6630-201102048
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Protein content in crude polysaccharide extract isolated from Acaudina molpadioides was determined comparatively by four commonly used protein quantification methods, i.e., Lowry, bicinchoninic acid, Bradford and fluorescence spectrometric methods in order to find out an accurate and simply method for quantifying protein in the matrix. It was calculated on the basis of amino acid composition that the crude extract contained (5.06 ± 0.31)% of protein, which served as a benchmark for the comparison among protein quantification methods. Lowry, bicinchoninic acid fluorescence spectrometric methods gave protein contents of (4.92 ± 0.20)%, (6.29 ± 0.51)% and (3.88 ± 0.25)%, respectively, while no protein was detected by Bradford method. The comparative results show that Lowry method is the most accurate method among the four quantification methods. Moreover, the method has the other characteristics of good reproducibility, short time consumption, simplicity and low requirements for analytical instruments and equipments.
Simultaneous Distillation Extraction and GC-MS Analysis of Volatile Components in Dictyophora indusiata Fisch
HUANG Ming-quan,TIAN Hong-yu,SUN Bao-guo,CHEN Hai-tao,JIANG Yuan-ning
2011, 32(2 ):  205-212.  doi:10.7506/spkx1002-6630-201102049
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The volatile components in Dictyophora indusiata Fisch from Fujian were extracted with a simultaneous distillation and extraction (SDE) apparatus and analyzed by gas chromatography-mass spectrometry (GC-MS). A total of 99 compounds were identified in the extract resulting from 3 h extraction with ethyl ether, and the number of identified compounds was 76 when dichloromethane was used as an extraction solvent for 2 h extraction. The extracts obtained using the two solvents contained 138 volatile components in total, including 23 aldehydes, 19 ketones, 16 alcohols, 4 hydroxybenzenes, 11 esters, 11 acids, 34 hydrocarbons, and 20 other compounds, and the prominent compounds were oxocyclopentadeca-2-one, 8-acetamido-6- methoxyquinoline, isolongifolen-5-one, 6,10-dimethyl-5,9-undecadien-2-one, τ-selinene, α-cadinol, n-hexadecanoic acid, etc.
Isolation, Purification and Molecular Weight Determination of Antihypertensive Peptides Derived from Porphyra haitanesis
LIU Shu-ji,WANG Yin,WU Cheng-ye,SU Yong-chang,LIU Zhi-yu
2011, 32(2 ):  213-217.  doi:10.7506/spkx1002-6630-201102050
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Porphyra haitanesis was hydrolyzed with AS.1398 neutral protease, and the hydrolysate was filtrated sequentially through ultra-filtration membranes with molecular weight cutoff (MWCO) 2000 D and 8000 D to obtain the fraction with the highest ACE-inhibitory activity, of which the molecular weight was below 2000 D. The fraction was then purified by Sephadex G-15 gel permeation chromatography into 6 peaks, in which peak E had the strongest ACE inhibitory activity with an IC50 of 0.67 mg/mL, and peak E was further fractionated by RP-HPLC to obtain peak No.6 with the highest ACE-inhibitory activity, reaching up to 89.54%. In the end, peak No.6 was injected into RP-HPLC system once again, and two protein peaks were observed in the chromatogram, suggesting that peak No.6 is not a single component and is still in need of further purification. The amino acid composition of peak No.6 was mainly composed of Tyr, Val and Phe. Meanwhile, the MALDI-TOF-MS spectrum of peak No.6 displayed 8 major proton peaks, the peak with the strongest signal intensity was m/z 861.17, and 4 of them were fluctuated around m/z 860, indicating that the mean molecular weight of peak No.6 is approximately 860 D. We speculated that antihypertensive peptides derived from Porphyra haitanensis consisted of 3 Val residues, 2 Phe residues and 1 Tyr residue, of which at the N-terminal Val was located, and that the number of possible ranking sequences was 18.
Quantitative Structure-Retention Relationship Studies for Predicting GC-MS Retention Times of Aroma Compounds in Kuerle Fragrant Pear Wine
DU Xi-hua
2011, 32(2 ):  218-221.  doi:10.7506/spkx1002-6630-201102051
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This paper presents a predictive model for the retention times of aroma compounds in Kuerle fragrant pear wine on gas chromatography-mass spectrometry (GC-MS) based on quantitative structure-retention relationship (QSRR) analysis. Some of the molecular connectivity indexes and Kappa shape indexes of 54 aroma compounds in Kuerle fragrant wine were calculated by program according to molecular bonding valence state and topological environment, and were related with the retention times of these compounds on GC-MS through multiple linear regression based on the molecular topological theory to obtain the regression equation describing retention time/molecular connectivity and Kappa shape indexes relationship, which exhibited a correlation coefficient of 0.952. The robustness and predictive ability of the regression model was validated by jackknife method, and the results showed that the correlation coefficient was between 0.946 and 0.956.
GC-MS Analysis of Volatile Compounds in Soybean Paste
QIAO Xin,FU Wen,QIAO Yu,HUANG Hong-xia,KANG Xu,WANG Chao,LI Dong-sheng
2011, 32(2 ):  222-226.  doi:10.7506/spkx1002-6630-201102052
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In the present study, a preliminary evaluation of the sensory quality of the industrially-produced soybean paste SPM04 and the traditional homemade soybean paste SPS06 based on the scores scored by 10 trained panelists was made, along with analysis of the volatile compounds in them by HS-SPME/GC-MS. Totally 39 and 38 compounds were identified in SPM04 and SPS06, respectively, and the total number of compounds contained in them was 61, including 2 alcohols, 1 acid, 7 aldehydes, 4 ketone, 13 esters, 7 phenols, 8 alkanes, 5 nitrogen-containing heterocyclic compounds, 7 furans, and 7 other compounds. Benzoic acid ethyl ester, benzeneacetic acid ethyl ester, benzaldehyde, benzeneacetaldehyde, phenylethyl alcohol, maltol, ethanone 1-(1H-pyrrol-2-yl)- and 2-methoxy-4-vinylphenol were found in both soybean pastes, accounting for 43.1% and 48.49% of the total volatile compounds, respectively. Therefore, it can be concluded that these compounds play an important role in the flavor of soybean paste. In addition, SPS06 is superior to SPM04 in color, smell and body.
Comparison of Two Pretreatment Methods for UPLC-MS/MS Determination of Enrofloxacin and Ciprofloxacin Residues in Freeze-dried Carp Meal
HAO Yan,WANG Li-min,LIU Yao-min,ZHANG Feng-ping
2011, 32(2 ):  227-230.  doi:10.7506/spkx1002-6630-201102053
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Sample pretreatment was achieved by two different methods, solid-phase extraction and liquid-liquid extraction, before the analysis of enrofloxacin and ciprofloxacin residues in freeze-dried carp meal on UPLC-MS/MS. The analytical results were compared to examine if the two pretreatment methods influence the accuracy of determination. The solid-phase extraction procedure was composed of extraction with EDTA-Mcllvaine buffer, clean-up on HLB column and blowing to dryness under nitrogen gas. Liquid-liquid extraction pretreatment was achieved sequentially through extraction with acidified acetonitrile followed by clean-up by liquid-liquid extraction with n-hexane and evaporation to dryness in a rotary evaporator. Both residues were dissolved in 1 mL of mixed solution of acetonirile and 0.2% formic acid (1:9, V/V) prior to injection into UPLC-MS/MS system. For the quantitation of enrofloxacin and ciprofloxacin, external standard method was used. Average spike recoveries of solid-phase extraction and liquid-liquid extraction ranged from 95% to 112% and from 75% to 90%, with relative standard deviations between 2.9% and 7.4% and between 1.0% and 4.6%, respectively (n = 6). The limits of detection (LOD) of solidphase extraction for the two analytes were both 1.0μg/kg, and the LOD of liquid-liquid extraction was 0.1μg/kg for enrofloxacin and 0.2μg/kg for ciprofloxacin. As a conclusion, both methods are characterized by simplicity, rapidity, good reproducibility and high selectivity, and therefore can be used to determine enrofloxacin and ciprofloxacin residues in fish meat and freeze-dried carp meal.
Simultaneous HPLC Determination of 16 Benzimidazoles Residues in Animal Tissue
2011, 32(2 ):  231-236.  doi:10.7506/spkx1002-6630-201102054
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A high performance liquid chromatography (HPLC) method was developed for the simultaneous determination of 16 benzimidazoles residues in animal tissue. Animal tissue samples were extracted with ethyl acetate-50% potassium hydroxide-1% BHT (20:0.15:1, V/V) , followed by treatment with n-hexane for defatting and further clean-up on MCX solid phase (SPE) cartridge. The chromatographic separation was performed on a C18 column with a mobile phase consisting of acetonitrile and 0.025 mol/L ammonium acetate solution at a flow rate of 1.0 mL/min by gradient elution. Detection wavelength was set at 292 nm, and the quantitation method used was external standard method. The calibration curves of 16 benzimidazoles exhibited good linearity over a concentration range from 0.025 to 1.0 mg/L, with correlation coefficients above 0.99. The average recoveries for 16 benzimidazoles in meat and liver tissues from three different animal species ranged from 81.6% to 110% at spike levels of 10, 50μg/mL and 100μg/mL, and the relative standard deviations were between 1.8% and 13.1% (n = 10). The limit of quantification was 10μg/kg. This method is sensitive, reproducible and suitable for the determination of benzimidazoles in animal tissue.
Fatty Acid Composition in Fruit of Wild Actinidia arguta Sieb.et Zucc
LIANG Pan,LI Shu-qian,ZHANG Bo,LIU Chang-jiang,XIN Guang
2011, 32(2 ):  237-239.  doi:10.7506/spkx1002-6630-201102055
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The fatty acid composition of the whole fruit and seeds of Actinidia arguta Sieb.et Zucc wildly grown in South Liaoning was analyzed by Soxhelt extraction and subsequent methyl esterification coupled to gas chromatography-mass spectrometry (GC-MS). Seven fatty acids were identified in the whole fruit of Actinidia arguta Sieb.et Zucc, including hexadecanoic acid (6.66%), 9,12-octadecadienoic acid (Z,Z)- (10.57%), 9,12,15-octadecatrienoic acid (77.78%), octadecanoic acid (3.09%), 10,13-octadecadienoic acid (0.2%), 11-eicosenoic acid (0.8%), and eicosanoic acid (0.14%). The seeds of the plant, however, contained 4 identified fatty acids, namely, hexadecanoic acid (3.24%), 9,12-octadecadienoic acid (Z,Z)- (5.40%), 9,12,15-octadecatrienoic acid (42.49%) and octadecanoic acid (2.39%).The compounds with the highest contents in the whole fruit and seeds of the plant were both 9,12,15-octadecatrienoic acid, which were 77.78% and 42.49% respectively.
Supercritical Carbon Dioxide Fluid Extraction and GC-MS Analysis of Volatile Flavor Compounds in Coprinus comatua Fruiting Body
LI Shuang-shi,LAN Rong,ZHANG Xiao-hui,MA Yue,CHEN Liang
2011, 32(2 ):  240-243.  doi:10.7506/spkx1002-6630-201102056
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The extraction of volatile compounds from the fruiting body of Coprinus comatua was carried out using supercritical carbon dioxide fluid extraction technique, and the effects of the pressure and temperature for extraction and separation on extract yield were investigated by 9-run orthogonal array design experiments. The optimal temperature and pressure were 55 ℃ and 20 MPa for extraction and 25 ℃ and 8 MPa for separation. In the extract obtained under these conditions, 25 major components was identified by GC-MS, such as 9,12-octadecadienoic acid (52.67%), octadecenoic acid (27.77%) and hexadecenoic acid (13.66%).
Purification of Gamma-Aminobutyric Acid from the Supernatant after S. salivarius subsp. thermophilus Y-2 Transformation Reaction
YANG Sheng-yuan,LU Zhao-xin,BIE Xiao-mei,LU Feng-xia
2011, 32(2 ):  244-247.  doi:10.7506/spkx1002-6630-201102057
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The concentrated supernatant after S. salivarius subsp. thermophilus Y-2 transformation reaction rich in gammaaminobutyric acid (GABA) was adjusted to pH 3.22 for precipitate L-Glu, followed by injection into 732 type strong acidic cation exchange resin column and elution with 0.15 mol/L NH3·H2O. After freeze-drying, GABA was obtained as a white solid powder, with 84.13% recovery. The powder contained (97.81±0.67)% of GABA, (0.449±0.002)% of ash, and exhibited a dry weight loss of (1.79± 0.06)%, and the contents of Pb, As and Hg in it were (0.4093±0.0001), (0.0511 ± 0.0001) mg/kg and (0.0950 ± 0.0000) mg/kg, respectively. Moreover, its quality was in accordance with relevant food additive standards. Thus, the purification strategy is highly efficient.
Comparative Analysis of Chemical Composition of Commercially Available Garlic Oils and Garlic Oil Extracted by Two-stage Molecular Distillation by GC-MS
CUI Gang
2011, 32(2 ):  248-251.  doi:10.7506/spkx1002-6630-201102058
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Three brands of commercially available garlic oils and garlic oil extracted by two-stage molecular distillation were comparatively studied for their chemical composition by means of GC-MS analysis, computer-aided searching and contrast with the standard mass spectra. The garlic oil extracted by two-stage molecular distillation mainly consisted of diallyl sulfide, diallyl disulfide, methyl disulfide, 2-propene-1-sulfinothioic acid-5-p ropenyl ester and trisulfide. Neither cyclic disulfide nor tetra-sulfide, however, was found in it.
Determination of Volatile Compounds in Sichuan Bran Vinegars Using Head Space-solid Phase Micro-extraction coupled with Gas Chromatography-Mass Spectrometry
XIONG Yue,HE Zhi-fei,LI Hong-jun,QIN Gang,WANG Ting
2011, 32(2 ):  252-255.  doi:10.7506/spkx1002-6630-201102059
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The volatile compounds of six Sichuan bran vinegars from three different factories were isolated by headspace solid phase micro-extraction, and analyzed using GC-MS. Totally 75 aroma constituents were isolated and identified, and the main constituents were acids, esters, alcohols, ketones, aldehydes, furanes, pyrazines, etc. Totally 12 volatile compounds were detected in all the six samples, of which the contributions to the overall aroma of bran vinegar were evaluated in terms of odor threshold and relative odor activity value (ROAV). The results showed that ethyl acetate, 2,3-butanedione, nonanal, acetic acid, decanal and benzaldehyde were the key aroma compounds of Sichuan bran vinegar. Also, furfural and 4-ethyl-2-methoxy-phenol contributed to the overall aroma of bran vinegar.
Optimization of Extraction Conditions of Beer Yeast Polysaccharides and Its Effects on the Development of Chick Immune Organs
WANG Yuan-xiu,ZHANG Gui-xiang,LI Feng,YUAN Jian-guo
2011, 32(2 ):  256-259.  doi:10.7506/spkx1002-6630-201102060
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Polysaccharides were extracted from beer yeast mud with citric acid, and the effects of pH, extraction temperature and citric acid concentration on polysaccharide extraction were investigated by single factor and orthogonal array design methods to determine the optimal values of the three parameters for maximizing polysaccharide yield. The dried polysaccharide extract obtained was identified for its monosaccharide composition by thin layer chromatography (TLC) and UV spectrometrically measured for its water-soluble polysaccharide content. Additionally, chickens developed under identical feeding conditions were randomly divided into two groups, control group (given 10 mL of tap water per chicken every day) and trail group (given the same volume of tap water supplemented with the extract per chicken every day). At 20 days of age, the weights of spleen, thymus and bursa of Fabricius and cecal tonsil area of chicken were measured. The optimal extraction conditions of beer yeast polysaccharides were as follows: pH, 7.2; temperature, 40 ℃; and citric acid concentration, 20 mmol/L. The major monosaccharide in beer yeast polysaccharides was glucose. Beer yeast polysaccharides could stimulate the development of immune organs in chicken, as evidenced by higher indexes of thymus gland, spleen, bursa folds, and weight or size increase of cercal tonsil in the treatment group compared with those in the control group.
Enzymatic Extraction of Seabuckthorn Fruit Oil and Its Fatty Acids Profile Analysis
KANG Jian,GU Jing-jing,WANG Ji-guo,WU Tong,ZHANG Li-xia
2011, 32(2 ):  260-262.  doi:10.7506/spkx1002-6630-201102061
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For the extraction of seabucthorn fruit oil, pectinase and pepsin were used to simultaneously hydrolyze seabucthorn fruit pulp, and the enzymatic extraction process was optimized by single factor experiments in combination with orthogonal array design method. Pectinase dose of 0.50%, pepsin dose of 0.15%, extraction time of 6 h, hydrolysis temperature of 55 ℃ were found optimum, and a maximum oil yield of 4.946% was achieved under these conditions, and the recovery of the optimized extraction process was calculated to be 82.16% - 97.17% based on 5.09% - 6.02% theoretical oil content of seabucthorn fruit. In addition, the fatty acid composition of seabucthorn fruit oil was analyzed by GC-MS. Eleven fatty acids were identified in seabucthorn fruit oil, mainly including 35.07% palmitoleic acid, 35.61% palmitic acid, 12.77% linoleic acid, 6.19% cis-11-octadecenoic acid, and 7.26% (12E)-12-octadecenoic acid, and unsaturated fatty acids occupied 61.56% of the total fatty acids. In conclusion, the extraction process has the benefits of mild conditions, safe, nontoxic and thorough reaction, high extraction efficiency, and ease of clarification of fruit juice after oil extraction.
Determination of Sodium Nifurstylenate in Milk and Dairy Products by High Performance Liquid Chromatography
LI Hai-yan,GUO Ping,ZHAN Chun-rui
2011, 32(2 ):  263-265.  doi:10.7506/spkx1002-6630-201102062
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A HPLC method was developed for the determination of sodium nifyrstylenate in milk and dairy products. Samples were extracted with acetonitrile, followed by clean-up by liquid-liquid extraction with n-hexane. Chromatographic peak area was linearly correlated with sodium nifyrstylenate concentration within a range of 10.0 to 200.0 ng/mL, with a correlation coefficient of larger than 0.9996. The limit of detection of the method was 20.0μg/kg. This method is simple and quick, and is therefore suitable for the monitoring and determination of massive export and import samples.
Packaging & Storage
Effects of Cutting Shapes and Packaging Methods on the Quality and Physiological Properties of Fresh-cut Pineapple
SHAO Yuan-zhi,LI Xue-ping,CHEN Jiao,WU Rui-gang,FU Yan-yan,LI Wen
2011, 32(2 ):  266-269.  doi:10.7506/spkx1002-6630-201102063
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The effects of cutting shapes and packaging methods on the sensory quality and the activities of enzymes related to browning of fresh-cut pineapple (Bali variety, from Hainan) during storage were investigated. Slicing in combination with either wrapping with polyethylene (PE) film or packaging in a PE bag was able to more effectively inhibit the softening of freshcut pineapple and the reduction of total soluble solid (TSS), titratable acid (TA) and vitamin C (VC) contents when compared to block cutting in combination with either PE wrapping or PE packaging, and maintain the activities of olyphenoloxidase (PPO) and peroxidase (POD) at a lower level during the entire storage period of 15 days and before the 6th day, respectively. Therefore, slicing in combination with either PE wrapping or PE packaging seems to be the most beneficial strategy for preventing the browning, maintaining the overall quality and extending the shelf life of fresh-cut pineapple.
Effect of Delayed Ice Exposure on the Quality Changes of Pseudosciaena crocea during Ice Storage
Jiang Xing-wei,XU Zhong,YANG Xian-shi,GUO Quan-you,LI Xue-ying1
2011, 32(2 ):  270-274.  doi:10.7506/spkx1002-6630-201102064
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Living Pseudosciaena crocea was sacrificed, and then ice-stored immediately (as a control) or after 4 or 8 h delay in 25 ℃ environment, and the microbial, chemical and sensory parameters of Pseudosciaena crocea during 800 h of ice storage were periodically measured in order to assess the effect of delayed ice exposure on the quality changes of Pseudosciaena crocea during ice storage. In comparison with the control, delayed ice exposure led to significant increases in the counts of total viable bacteria (TVC), Psychrobacter spp., Pseudomonas spp. and H2S-producing bacteria as well as total volatile basic nitrogen (TVB-N) content, and a significant decrease in the sensory quality, but no significant change in rimethylamine nitrogen (TMA-N) throughout the period of storage. These findings reveal that delayed ice exposure is able to significantly promote the growth of various microbes during ice storage, accelerate the generation rates of TVB-N and TMA-N and the production of off-odor, and substantially shorten the shelf life of Pseudosciaena crocea. According to the sensory evaluation results given by 5 trained panelists, the shelf lives of icestored Pseudosciaena crocea after 0, 4 h and 8 h delay were 648, 550 h and 408 h, respectively. Therefore, immediate ice exposure prolongs the shelf life of Pseudosciaena crocea by 98 h and 240 h when compared to 4 and 8 h delay, respectively.
Effect of Harvest Time on Storage Quality and Antioxidant Enzyme Activities of Lentinus edodes
MENG De-mei,SONG Tian-zi,SHEN Lin,ZHANG Xin-hua,SHENG Ji-ping
2011, 32(2 ):  275-279.  doi:10.7506/spkx1002-6630-201102065
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Two groups of shiitake mushroom (Lentinus edodes) with different harvest times (early commercial maturity stage when cap is closed and later stage when cap is open) were stored at 15 ℃, and dynamic changes in cap opening, weight loss rate, respiratory intensity, moisture content, ascorbic acid content and the activities of superoxide dismutase (SOD), peroxidase (POD) and catalase (CAT) were determined. Throughout the storage, the pileus diameter and respiratory intensity of shiitake mushroom with closed cap were 1.5 - 2.5 and 1.2 - 1.8 times higher than those of shiitake mushroom with open cap, respectively. At the end of the storage, moisture content of late-harvested shiitake mushroom was only half of that of earlyharvested shiitake mushroom, and the decline of ascorbic acid content was 21.8% higher than that of early-harvested shiitake mushroom. Furthermore, the activities of SOD, POD and CAT in early-harvested shiitake mushroom were always maintained at higher levels during the storage (P < 0.05). The results show that early-harvested shiitake mushroom has better storage qualities and higher antioxidant ability in comparison with late-harvested shiitake mushroom.
Fresh-keeping Effect of Chitosan Coating on Zizyphus jujuba Mill Fruits
LI Shu-gang,CHEN Dong-mei,LIU Hua-ying,HOU Xu-jie,YU Jun
2011, 32(2 ):  280-284.  doi:10.7506/spkx1002-6630-201102066
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After receiving coating treatment with different concentrations (0.50%, 1.00%, 1.50%, 2.00% and 2.50%) of chitosan solutions, round crisp dates (Zizyphus jujuba Mill fruits) were stored under the conditions of -1℃-0 ℃ and 90%-95% relative humidity for 70 days, and changes in the sensory, physical and chemical characteristics of round crisp dates were measured during the storage period. Coating treatment with 1.50% chitosan solution revealed the best fresh-keeping effect on round crisp dates, and the percentage of rotten fruits, fruit weight loss rate, firmness and the contents of titratable acid, vitamin C and soluble solid at the end of the storage period were 30.60%, 11.35%, 9.88 kg/cm2, 0.31%, 412.56% and 22.22%, respectively. The control group without receiving any fresh-keeping treatment, however, showed 92% of rotten fruits and completely lost commercial value. These data suggest that chritosan coating can noticeably retard post-harvest fruit senescence and extend the shelf life of round crisp dates.
Changes in Freshness Parameters and Shelf Life of Turbot (Scophthalmus maximus) during Cold Storage
CUI Zheng-cui,XU Zhong,YANG Xian-shi,GUO Quan-you,LI Xue-ying
2011, 32(2 ):  285-289.  doi:10.7506/spkx1002-6630-201102067
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Freshness change of turbot (Scophthalmus maximus) stored aerobically at 0 (in ice), 3, 7 or 10 ℃ was investigated by periodically determining sensory, chemical, and microbiological indices during storage. The identity among these indices in evaluating the shelf life of turbot was probed. Turbot samples stored at 0, 3, 7 and 10 ℃ showed better quality within 433, 197, 93.5 h and 68 h, respectively, and shelf lives of 602, 362, 165 h and 116 h. Averagely, total viable counts (TVC) at the ends of better-quality periods and shelf lives at the above storage temperatures were (5.74 ± 0.31) lg(CFU/g) and (6.99 ± 0.39) lg (CFU/g), Pseudomonas counts (5.48 ± 0.24), (6.26 ± 0.71) lg(CFU/g), total volatile base nitrogen (TVB-N) values (2.73 ± 0.12)% and (10.71± 0.81)%, and trimethylamine (TMA-N) values (2.73 ± 0.12)% and (10.45± 0.95)%, respectively. There were no significant differences (P > 0.05) among the above indices at the ends of better-quality periods and shelf lives at various temperatures. This means that all TVC, Pseudomonas count, TVB-N and TMA-N have good identity to sensory evaluation in indicating turbot shelf life as freshness parameters.
Application of ε-Polylysine to Keep Chilled Pork Fresh
ZHANG Quan-jing,FENG Xiao-hai,XU Hong,ZHANG Yang,CAO Yu-juan
2011, 32(2 ):  290-296.  doi:10.7506/spkx1002-6630-201102068
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ε-Polylysine (ε-PL) treatment was used to keep chilled pork fresh, and the change of total viable count (TVC) in fresh pork treated under different conditions of ε-PL concentration, accessory reagent type and soaking time during storage at 4 ℃ in order to optimize the three treatment conditions. Along with this, the effect of optimized ε-PL treatment on the sensory, microbiological and physiochemical properties of chilled pork were investigated. Treatment with 400 mg/L ε-PL alone markedly inhibited the decline in sensory quality, the growth of microorganisms, the increase of pH and the accumulation of total volatile base nitrogen (TVB-N). Better fresh-keeping effect was observed when ε-PL and acetic acid were used together, especially more significant inhibitory effect on microbial growth. The combined antimicrobial effects of ε-PL and acetic acid were largely affected by soaking time in a positive way. Collectively considering antimicrobial effect as well as treatment cost and efficiency, the optimal ε-PL concentration, accessory reagent type and soaking time were 400 mg/L, 02% acetic acid and 5 min. The optimized ε-PL treatment increased the shelf life of chilled pork from 2 to 8 d. These results demonstrate that ε-PL will have extensive application prospects as a biological fresh-keeping agent for chilled pork.
Quality Changes of Blood Orange Juice during Storage
CAO Shao-qian,LIU Liang,PAN Si-yi
2011, 32(2 ):  297-301.  doi:10.7506/spkx1002-6630-201102069
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Quality-related physico-chemical indexes of blood orange juice were determined during storage at different temperatures, and the effect of low temperature on the quality of blood orange juice was investigated. Results indicated that blood orange juice was abundant in anthocyanins (68.84 mg/L), flavonoids (0.18 mg/mL), ascorbic acid (0.63 mg/mL), amino acids (43.012 mg/mL) and sugars (128.3 mg/mL). Meanwhile, the juice contained essential trace elements such as Ca, Mg, Zn, Fe and Cu. HPLC analysis showed that soluble sugars in the juice were mainly glucose (2.1 g/100 mL), sucrose (7.4 g/100 mL) and fructose (2.2 g/100 mL). During the storage of blood orange juice, the attractive red color was lost along with the decrease in anthocyanin content, the content of ascorbic acid decreased significantly, by around 52% after 40 days, reducing sugar content changed slowly, and total acid content increased smoothly.
Effect of Hypobaric Treatment on Physiological Properties of Cauliflower during Storage
DIAO Xiao-qin,GUAN Hai-ning,ZHANG Run-guang,ZHANG You-lin,GUO Li,MA Song-yan
2011, 32(2 ):  302-304.  doi:10.7506/spkx1002-6630-201102070
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Cauliflower was stored under different levels of pressure (20.3, 40.5, 60.7, 80.1 kPa and 101.3 kPa) at (1.0 ± 0.5) ℃, and the effect of hypobaric treatment on physiological properties of cauliflower during storage was studied. Compared with the control (101.3 kPa), hypobaric treatment at 60.7 kPa decreased respiration rate by 43%, polyphenol oxidase (PPO) activity by 28.8% and peroxide dismutase (POD) activity by 32.7% and increased vitamin C content by 55.6%, and the browning index of treated cauliflower was only 0.21 after 40 days of storage. Therefore, appropriate pressure treatment can delay the browning and senescence of cauliflower tissue with good fresh-keeping effect.
Effect of High Oxygen and High Carbon Dioxide Atmosphere Treatment on Senescence of Postharvest Green Asparagus
TU Bao-jun
2011, 32(2 ):  305-309.  doi:10.7506/spkx1002-6630-201102071
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The effect of modified atmosphere package (MAP) with high oxygen at different concentrations and high carbon dioxide (20%) on the sensory quality, lignin content, the activities of superoxide dismutase (SOD), catalase (CAT) and polyphenol oxidase (PPO) and total phenol content of green asparagus spears during storage at (4 ± 1)℃ were studied using ambient atmosphere as a control. Results indicated that package with oxygen at concentrations of over 60% and 20% carbon dioxide could delay the deterioration of sensory quality, the decline of total soluble solid and total polyphenol content, keep the activities of SOD and CAT and inhibit the increase of PPO activity. The green asparagus packaged in 80% O2+20% CO2 showed the best storage quality. As a conclusion, the atmospheric condition will have potential application prospects in delaying the postharvest senescence of green asparagus.
Effect of 1-Methylcyclo-propene Treatment on Post-harvest Physiology of Mulberry
HUO Xian-qi
2011, 32(2 ):  310-313.  doi:10.7506/spkx1002-6630-201102072
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Mulberry was treated with 1-methylcyclo-propene (1-MCP) before storage at 0-2 ℃, and changes in vitamin C, chlorophyll, titratable acid, hardness, respiration intensity and decay during the storage were determined. Results showed that 1-MCP treatment delayed the decline of hardness, vitamin C content and chlorophyll after 48 hours, and titratable acid content even with a slight increase in the beginning. Also, 1-MCP treatment decreased the rate of decay of mulberry. Meanwhile, no obvious decrease in respiration intensity of mulberry was observed. However, no linear correlation between the rate of decay and the concentration of 1-MCP was found, which suggests that there is an optimum 1-MCP concentration for preventing the decay of mulberry.
Screening and Fresh-keeping Effect of Composite Preservatives on Pleurotus ostyeatus
ZHANG Li,LIU Lin-de,DING Juan,HUANG Qing-rong
2011, 32(2 ):  314-317.  doi:10.7506/spkx1002-6630-201102073
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The fresh-keeping effects of citric acid, phytic acid, vitamin C, chitosan and salt on Pleurotus ostreatus were comparatively investigated, and citric acid, phytic acid and vitamin C showed relatively stronger effect. Then a composite preservative consisting of the above three compounds at different concentrations was developed, and its fresh keeping effect was evaluated by measuring weight loss, degree of browning, respiratory intensity and sensory indexes (including color, smell, viscosity, degree of decay, etc.) of composite-preservative-treated Pleurotus ostreatus during storage at 8 ℃. Results showed that when used separately, the optimum concentration ranges of citric acid, phytic acid and vitamin C were 5-10, 1.5-2.0 g/L and 0.9 - 1.3 g/L, respectively, and when formulated, their optimal concentrations were determined by orthogonal array design experiments to be 10, 1.5 g/L and 1.3 g/L, respectively.
Technology Application
Optimization of Orange Juice Milk Formulation
LI Yuan-hu,WANG Hua
2011, 32(2 ):  318-323.  doi:10.7506/spkx1002-6630-201102074
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The formulation of an orange juice milk was optimized by single factor experiments and Behnken central composite design combined with response surface analysis. Using 0.23% CMC-Na, 0.15% sodium alginate and 0.07% pectin together as stabilizer resulted in the lowest sedimentation rate at 2.86%. The product consisting of 24.76% milk, 21.06% orange juice, 5.22% sugar, and 0.10% citric acid had the best quality and flavor with a sensory score of 86.63/100.
Effect of Konjac Glucomannan on Staling of Steamed Bread
CHEN Wen-ping,WANG Chao,JIAN Mei-yun,ZHONG Xiao-ling,NI Xue-wen,JIANG Fa-tang
2011, 32(2 ):  324-327.  doi:10.7506/spkx1002-6630-201102075
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The staling of steamed bread is a critical problem hindering the industrialization of steamed bread. In the present study, konjac glucomannan (KGM) was added in steamed bread processing to investigate its anti-staling effect. Meanwhile, the parameters in steamed bread processing were optimized using the Plackett-Burman experimental design and orthogonal array design. Results showed that adding KGM in the wheat flour improved the anti-staling property of steamed bread, and the processing conditions were as follows: wheat flour 200 g, KGM 5.0 g, yeast 1.7 g, white granulated sugar 1 g, preparation time 1 h and dough time 2.5 h. Steamed breads produced under the optimized conditions presented smooth surface, lofty shape, big specific volume and exquisite internal structure, with improved staling rate.
Preparation of Germinated Soybean Yogurt
LI Xiao-mei
2011, 32(2 ):  328-332.  doi:10.7506/spkx1002-6630-201102076
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Germinated soybean yogurt was prepared by using skimmed milk powder and four-day germinated soybean as raw materials. Product quality was evaluated through sensory evaluation. Germinated soybeans were mixed with water at a ratio of 1:4.5 (m/m) and homogenized to obtain soybean homogenate. Skimmed milk powder was dissolved in a 5-fold volume of water, and mixed with the germinated soybean homogenate, followed by sucrose addition, inoculation and fermentation with mixed lactic acid bacteria. The fermentation conditions were optimized by orthogonal array design, and the results showed that the optimal preparation process for germinated soybean yogurt was sequentially composed of mixing of milk liquid with soybean homogenate (60:40, m/m) and sucrose (6 g/100 mL of soybean homogenate), inoculation with mixed lactic acid bacteria (5 mL per 100 mL of soybean homogenate), and fermention for 7 h. The effect of post-ripening on product flavor was also studied, which revealed that the optimum flavor was obtained after storage at 4℃ for 16h. The germinated soybean yogurt prepared by this method had the characteristic flavor of concentrated yogurt.
Development of A New ELISA Kit for Tetracycline Residue Detection in Foods
GUO Zhan-bao,WU Yu-xiang,TIAN Wen-li,ZHAO Ya-zhou,PENG Wen-jun,LIU Jia-peng
2011, 32(2 ):  333-337.  doi:10.7506/spkx1002-6630-201102077
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A competitive ELISA kit for tetracycline (TC) residues detection was developed by employing TC monoclonal antibody prepared by hybridoma technology using anti-TC monoclonal antibodies secreted by immunized BALB/c mouse. Performance tests showed that the logit/log calibration curve of the kit was y = -2.3x + 2.79 (correlation coefficient, r = 0.9971), with a linear range from 0.05 to 4.05 ng/mL, the half inhibitory concentration (IC50) was 0.293 ng/mL, the sensitivity was 0.05 ng/mL and the detection limit ranged from 3 to 5 ng/mL. The recovery for spiked TC in muscle, milk, and honey was (90 ± 10)%, ( 85 ± 10)% and (90 ± 10)%, with coefficient of variations (CV%) less than 15%, respectively. Cross-reactivity between TC and CTC was more than 60%, and there was no cross-reactivity between TC and other antibiotics. This ELISA Kit could be stored at 4 ℃ for more than six months.
Analysis & Detection
Construction of Standard Reference Molecule and Its Application in Event-specific Transgenic Detection of Genetically Modified Maize 59122
LU Jiao,YANG Rong,HUANG Kun-lun,ZHAO Wei-wei,LUO Yun-bo,YUAN Yan-fang,XU Wen-tao
2011, 32(2 ):  136-140.  doi:10.7506/spkx1002-6630-201102032
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Transgenic event-specific primers and Taqman probes based on the left-flanking sequence of 59122 were
designed, and a real-time PCR method was developed to quantitatively detect the event-specific genetically modified maize
59122. The standard reference molecule (integration of the reference gene sequence and the left-wing sequence) with a
gradient range of 101-105 and a quantitative range of 0.01%-100% were obtained by a recombinant PCR method. Two
standard curves of the reference gene sequence and the left-wing sequence were established with acceptable CV (coefficient
of variance), SD (standard deviation) and R2 (correlation coefficient). Five mixed samples with known genetically modified
contents of 0.1%, 0.5%, 1%, 2% and 5% were determined with the results of 0.12%, 0.56%, 1.04%, 1.61% and 4.66%,
respectively. The experimental error was less than 25%. The assay can be applied to analyze genetically modified content (raw
materials as well as processed food) and will provide a technical support for the preparation of standard reference molecule.