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15 May 2009, Volume 30 Issue 10
Preparation and Characterization of β-cyclodextrin Inclusion Compound of Essential Oil from Rosa damascena Miller
WEN Zhen1,LIU Bo1,ZHENG Zong-kun1,YOU Xin-kui1,PU Yi-tao1,LI Qiong2
2009, 30(10):  29-32.  doi:10.7506/spkx1002-6630-200910001
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In order to improve the solubility in water and stability of essential oil from Rosa damascena Miller, the essential oil was included with β-cyclodextrin(β-CD) by saturated water solution-stirring method. The inclusion conditions were optimized through orthogonal test, and the inclusion compound was characterized by thin-layer chromatography (TLC), gas chromatography-mass spectrometry (GC-MS), Fourier transform infrared (FTIR) spectrometry and differential scanning calorimetry (DSC). The results showed that the optimal inclusion conditions of essential oil from Rosa damascena Miller were as following: mass ratio of essential oil to β-CD 1:10, inclusion temperature 60 ℃, and inclusion time 2 h. The inclusion ratio of essential oil was up to 80% under above conditions. The inclusion compound retained the main characteristic components of the essential oil and obviously improved its solubility in water and stability. This β-CD inclusion compound of essential oil from Rosa damascena Miller can be used as a solid immediate for the development of functional foods.

Optimization of Technical Parameters for Honey Pomelo Wine Debittering
LI Li-jun,XIAO An-feng,NI Hui,YANG Yuan-fan,YANG Qiu-ming,CAI Hui-nong*
2009, 30(10):  33-37.  doi:10.7506/spkx1002-6630-200910002
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The main bitter compounds in honey pomelo pulp are limonin and naringin. During the processing of honey pomelo wine from honey pomelo pulp, most the above two compounds would be retained. In this study, adsorption combined with adding bitter inhibitors method was applied to honey pomelo wine debittering. The combined debittering technology was optimized through single-factor and orthogonal tests. The results showed that strong basic anion exchange resin 201 × 7 presented low adsorption capacity, and diatomite had no obvious debittering, so both of them were unsuitable for honey pomelo wine debittering. The best addition amounts of macroporous adsorption resin Y7, activated carbon, silica gel, β-cyclodextrin and white sugar for honey pomelo wine debittering were 0.3%, 0.3%, 0.2%, 0.2% and 1%, respectively.

Optimization of Extraction Technology of Polysaccharides from Gracilaria lemaneiformis at Room Temperature and Their Immunocompetence
GONG Chun-yu1,2,ZHANG Jin-song2,TANG Qing-jiu2,LIU Yan-fang2,YE Li-bin3,DU Xiu-ju3,PAN Ying-jie1,*
2009, 30(10):  38-41.  doi:10.7506/spkx1002-6630-200910003
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The extraction technology of crude polysaccharides from Gracilaria lemaneiformis (GCp) at room temperature was optimized by orthogonal test, and the inducing effects of GCp and different fractions of GCp obtained by different methods on proliferation of mouse lymphocyte were investigated. The results indicated that extraction times and extraction time were the significant factors affecting the yield of GCp. The maximum yield of 9.96% was obtained by extracting three times for 12 h at the solid to liquid ratio of 1:20. 32% of protein contained in crude polysaccharide could be removed by Sevag method (repeated 5 times). The inducing effect of GCp extracted at room temperature on proliferation of mouse lymphocyte was significantly higher than thoseot obtained at 100 ℃ and 121 ℃ at the same concentration. Five kinds of polysaccharides were obtained by ultrafiltration, freeze-thaw and Sevag method (GCpF1 and GCpF2 by ultra-filtration, GCp-1 and GCp-2 by freeze-thaw, and GCp- S by Sevag method). The immunocompetence assay revealed that all GCp and the five polysaccharide fractions were able to induce proliferation of mouse lymphocyte in a concentration-dependent manner, and GCp, GCpF1 and GCpF2 were more active than GCp-1, GCp-2 and GCp-S.

Study on Ultrasound-assisted Enzymatic Preparation of Allicin
MO Ying-jie,WANG Jing,CAO Yan-ping,SUN Bao-guo*
2009, 30(10):  42-45.  doi:10.7506/spkx1002-6630-200910004
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When garlic is broken, the endogenous alliinase existing in cytoplasm and its natural substrate, alliin, existing in vacuole will contact each other and react, and then allicin will be formed. Based on this, allicin can be prepared by pounding garlic and then keeping the pounded garlic at suitable temperature for some time. In the present study, ultrasound was applied to preparation of allicin. The ultrasound-assisted enzymatic preparation technology of allicin were optimize by mixed-level uniform design. The results showed that the optimum preparation conditions were as follows: hydrolysis temperature 35 ℃, reaction time 30 min, ratio of garlic to water 1:1.5 (W/V), ultrasonic frequency 50 kHz, and ultrasonic intensity 0.4 W/cm2. Under these conditions, the allicin yield was up to 1.3 mg/g garlic, increased by15.83%, compared to the non-ultrasound-assisted enzymatic preparation technology.

Study on Acid Extraction Technology of Pepsin from Porcine Gastric Mucosa
ZHANG Li-ping,WANG Ying,CUI Su-ping
2009, 30(10):  46-48.  doi:10.7506/spkx1002-6630-200910005
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Objective: To optimize the extraction technology of pepsin from porcine gastric mucosa with hydrochloric acid. Methods: Based on single factor test, quadratic regression orthogonal rotational combination design was applied to establish a mathematical model with pepsin activity as a function of hydrochloric acid dosage, concentration of hydrochloric acid, temperature, and extraction time. Results: The mathematical model reflected the relationship between the above factors and pepsin activity well. The optimized extraction parameters were as follows: hydrochloric acid dosage 6.7 ml, concentration of hydrochloric acid 1.2%, temperature 48.1℃, and extraction time 60 min, and under these conditions the activity of extracted pepsin was up to 4677.0 U/g.

Study on Extraction Technology of Total Flavonoids from Longwangmao Sugary Almond (Prunus armeniaca)
HE Wen-xing,LI Hong-mei,XIAO Xia
2009, 30(10):  49-51.  doi:10.7506/spkx1002-6630-200910006
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The objective of this study was to optimize extraction technology of total flavonoids with ethanol by heat reflux extraction method. Based on single-factor test, the optimal extraction conditions of total flavonoids were determined by orthogonal test as follows: ethanol concentration 95%, extraction temperature 65 ℃, solid to liquid ratio 1:25, and extraction time 2 h. Under these conditions, the extraction yield of total flavonoids was 10.60%.

Study on Stepwise Enzymatic Hydrolysis of Defatted Rapeseed Meal
JIANG Shao-tong,LUO Lei-lei,PAN Mu,NIE Sheng-de
2009, 30(10):  52-55.  doi:10.7506/spkx1002-6630-200910007
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Defatted rapeseed meal was hydrolyzed with alcalase firstly and then with neutral protease to prepare compound amino acids and peptides. The two hydrolysis processes were optimized by orthogonal test with hydrolysis degree with investigation index. Moreover, the functional properties of the obtained hydrolysates were discussed. The results showed that the optimal conditions of alcalase hydrolysis were as follows: pH value 10.5, liquid to solid ratio 15:1, temperature 50 ℃, time 1.5 h, and enzyme dose 3250 U/g of substrate, and those of neutral protease hydrolysis were as follows: pH 9, temperature 45
℃, time 2 h, and enzyme dose 3250 U/g of substrate. Under the above conditions, the hydrolysis degree and nitrogen yield were 25.66% and 86.8%, respectively. In the range of pH 3 to 7, the nitrogen soluble index (NSI) of the obtained hydrolysates was higher than 72.19%. Their trichloroacetic acid (TCA)-NSI was 85.67%. Through hydrolysis, the contents of tannin, glucosinolate and phytic acid in defatted repeseed meal were decreased markedly .

Studies on Microwave-assisted Extraction of Total Flavonoids from Cryptotaenia japonica Hassk and Their Anti-oxidation Properties
ZHOU Zhi1,MO Kai-ju1,LIN Chun-xiao2,WANG Xing-ping1,*,TIAN Cheng1,CHEN Ye1
2009, 30(10):  56-59.  doi:10.7506/spkx1002-6630-200910008
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Crushed Cryptotaenia japonica Hassk was defatted with petroleum ether by heat trflux method. After dried at 60 ℃, the defatted Cryptotaenia japonica Hassk was used to extract total flavonoids with deionized water under the assistance of microwave. The microwave-assisted extraction technology of total flavonoids from defatted Cryptotaenia Japonica Hassk was optimized and their anti-oxidation properties were discussed in this study. The results demonstrated that the optimal extraction comditions were as follows: particle size of defatted Cryptotaenia japonica Hassk 80 mesh, material to loquid tatio 1:30 (W/V), extraction time 4 min, and extraction times 3. The crude flavonoids extract from Cryptotaenia japonica Hassk exhibited higher reducing power and hydroxyl radical scavenging capacity.

Preparation Techniques of Pigskin Collagen Powder and Its Functional Characteristics
HAN De-quan,JIN Ming-ji,WU Tong,CAO Xiang-hui
2009, 30(10):  60-64.  doi:10.7506/spkx1002-6630-200910009
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Pigskin soluble collagen was prepared by enzymolysis in addition of weak acid at 4 ℃, and then dried into powder, and the remaining pigskin was further grinded in the presence of ethanol to prepare insoluble collagen powder. The extraction technology of soluble collagen was optimized by orthogonal test, and the ethanol concentration for preparing insoluble collagen powder was selected. Besides, the collagen content and functional properties of the two collagen powders were analyzed. Results showed that the addition of acetic acid was able to enhance the swelling of pigskin and the dissolution rate of soluble collagen. The optimal extraction conditions of soluble collagen with pepsin were as follows: enzyme concentration 0.2%, solid to liquid ratio 1:15, pH 2.0 and hydrolysis time 48 h, and under the above conditions the yield of soluble collagen was 0.602%. 60% ethanol was the best for preparing insoluble collagen powder. The collagen contents of obtained soluble collagen powder and insoluble collagen powder were 95.1% and 82.9%, respectively. Both the two collagen powders exhibited good functional characteristics. The results suggested the feasibility of this technology for the production in plant scale.

Tenderization of Beef with Pineapple Juice
HUANG Ye-chuan1,2,LI Hong-jun1,*,LI Feng1,2
2009, 30(10):  65-68.  doi:10.7506/spkx1002-6630-200910010
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Pineapple juice contains bromelain can tenderize beef. Effects of several factors, such as pineapple juice amount, pH value, temperature and treatment time, on tenderization of beef with pineapple juice were investigated in this study. The optimal conditions for beef tenderization were determined as follows: pineapple juice amount 6%, pH 7.0, 50 ℃, and 60 min. Under these conditions, shear force of beef was reduced by 50%. Beef products tenderized with pineapple juice, ginger juice and papain were compared in terms of flavor, color and shear force. Results indicated that tenderization effect of pineapple juice was more pronounced in enhancing the beef flavor than that of ginger juice (p ≤ 0.05). Compared to the control, beef treated with papain yielded better flavor. Pineapple juice, ginger juice and papain were all able to increase the tenderness of beef while no significant differences were observed among them. Beef treated with pineapple juice possessed higher a and a/b values than control and this difference of a/b value disappears after cooking. The results suggested no effect of tenderization of pineapple juice on the color of beef products.

Optimization of Extraction Technology of Total Saponins from Arenaria kansuensis Maxim by Mathematical Model
XU Qian-xi1,HUANG Yong2,PENG Guang-hua1,*
2009, 30(10):  69-73.  doi:10.7506/spkx1002-6630-200910011
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Using statistical analysis, four-element quadratic regression orthogonal rotation combination was designed for extraction experiment of total saponins from Arenaria kansuensis Maxim. A mathematical model was established, with extraction time, extract temperature, concentration of ethanol and solid-liquid rate as the adjusting factors and the yield of total saponins from Arenaria kansuensis Maxim (y) as the objective function. After the simulated optimization by computer, the optimum ranges of extraction time, extraction temperature, concentration of ethanol and solid-liquid ratio were determined as 4.78 to 5.22 h, 77.91 to 82.78 ℃, 68.49% to 73.3% and 1:38.42 to 1:42.89, respectively. Furthermore, the interactions among various factors were also investigated. Altogether, the present study provided scientific basis for total saponins extraction from Arenaria kansuensis Maxim.

Study on Simultaneous Extraction Technology of Water Soluble Alkaloid and Essential Oil from Zanthoxylum bungeanum Seed
SHI Xue-ping1,ZHANG Yu-si2,ZHANG Wei-ming1
2009, 30(10):  74-76.  doi:10.7506/spkx1002-6630-200910012
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In the present study, the simultaneous extraction technology of water soluble alkaloids and essential oil from Zanthoxylum bungeanum was optimized by L9(34) orthogonal test. The results showed that the optimal extraction conditions were as follows: soaked time of Zanthoxylum bungeanum seed in deionized water 2 h, pH 2, ratio of material to deionized water 1:15 (W/V), and extraction time 3 h. Under these conditions, the yields of water soluble alkaloids and essential oil were 4.36% and 3.25%, respectively.

Determination of Gastrodin in Gastrodia elata Bl. by Reverse Phase (RP)-HPLC and Study on Its Extraction Technology
TIAN Yang1,XIAO Rong2,*,XU Kun-long2,SHI Chong-ying1,DAI Yi2
2009, 30(10):  77-81.  doi:10.7506/spkx1002-6630-200910013
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By investigating the effects of different detection wavelength, mobile phase and solvent on the peak profile of gastrodin, the present study improved the traditional RP-HPLC method for determining gastrodin in Gastrodia elata Bl.. Also, the effects of extraction solvent, extraction temperature, solid-liquid ratio and extraction time on the extraction rate of gastrodin were discussed. The results showed that the optimal working conditions of RP-HPLC were as follows: using Diamonsil C18 column (150 mm×4.6 mm, 5 μm) at ambient temperature, acetonitrile-water (3:97, V/V) as the mobile phase, flow rate 1.0 ml/min, detection wavelength 220 nm, and acetonitrile-0.05% phosphoric acid (3:97, V/V) as the solvent of gastrodin. The calibration curve was well linear in the range of 10 to 80 μg/ml, the regression equation was y = 4.0264x + 0.6311 with a determination coefficient of 0.9992. The limit of detection of this method was 2 ng. The relative standard deviations (RSDs) of precision and repeatability were 0.41% and 0.86%, respectively (n = 6), and the average spike recovery rate was 98.4% with a RSD of 0.84% (n = 6). The optimum extraction conditions of gastrodin from Gastrodia elata Bl. were determined as follows: 50% alcohol as extraction solvent, temperature 70 ℃, ratio of solid to liquid 1:6 (g/ml), and extraction time 3 h.

Application of Fat Substitutes in Low-fat Mayonnaise
LIU He1,ZHU Dan-shi1,XU Xue-ming2,3,GUO Shi-dong3,JIN Zheng-yu3
2009, 30(10):  82-85.  doi:10.7506/spkx1002-6630-200910014
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Fat substitute was prepared from gelatin and gum arabic through phase separation and applied in low-fat mayonnaise. The texture and sensory properties of low-fat mayonnaise containing the fat substitute in were investigated. The results showed that the difference in texture properties was marked between low-fat and full-fat mayonnaise but not in sensory properties. The texture defect could be counteracted by adding 0.04% of xanthan and 0.05% of carageenan as thickeners to low-fat mayonnaise.

Forward Extraction of Protein from Xanthoceras sorbifolia Bunge. Kernel Using Reversed Micelles
LI Zhao-di,DENG Hong*,FAN Xue-ceng,XU Hui-yan
2009, 30(10):  86-91.  doi:10.7506/spkx1002-6630-200910015
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Protein was extracted from Xanthoceras sorbifolia Bunge. kernel by using reversed micelles. Single-factor test combined with quadratic general rotary design was applied to study the effects of factors such as surfactant concentration, ion concentration, pH value, oil to water ratio and temperature. The optimal conditions of protein extraction from Xanthoceras sorbifolia Bunge. kernel by reversed micelles were determined as follows: cetyl trimethyl ammonium bromide (CTAB) concentration 0.03 mol/L, pH 10, oil to water ratio 1:1 and temperature 30 ℃. This optimal operating condition resulted in the high protein yield of 56.27%. In addition, a regression mathematical model was established, which could predict the extraction yield of protein from Xanthoceras sorbifolia Bunge. kernel accurately.

Optimization of Enzymatic Extraction Technology of Total Flavonoids from Celery by Response Surface Methodology
YI Jian-hua,ZHU Zhen-bao
2009, 30(10):  92-96.  doi:10.7506/spkx1002-6630-200910016
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Total flavonoids were extracted from celery (Apium graveolens L.) with enzymatic method. Based on single-factor test, response surface analysis was conducted to optimize the enzymatic extraction technology of total flavonoids. The singlefactor test showed that enzyme variety, enzyme concentration, treatment temperature and time markedly affected the extraction rate of total flavonoids, but material to liquid ratio presented little effect. The optimum extraction conditions were confirmed by response surface method as follows: cellulase concentration 2.3 U/ml, solid to liquid ratio 1:60, pH 4.7, enzymatic hydrolysis temperature 51.5 ℃, and time 2.2 h. Under these conditions, the extraction rate was 0.88%.

Study on Extraction Technology and Stability of Red Pigment from Suaeda salsa
WU Tao1,YAO Zhi-gang1,*,XU Jie2,WU Xing-jie3
2009, 30(10):  97-100.  doi:10.7506/spkx1002-6630-200910017
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With Suaeda salsa as the raw material, the extraction technology of red pigment and the effects of light, heat, pH value, reductant, oxide, sucrose and metal ion on its stability were investigated. The red pigment is insoluble in organic solvents but free in water, and its maximum absorption peak is at the wavelength of 538 nm. Therefore, it was primarily identified as betacyanin. Its optimum extraction conditions were confirmed as follows: using water as extraction solvent, ratio of material to water 1:25, extraction temperature 40 ℃, and time 10 min. This pigment was poor in resistance against light, heat and oxide, may endure reductant to some extent, and could be applicable in pH 4~7. Sucrose and metal ions such as Fe3+, Fe2+, Mg2+ and Ca2+ did not affect the stability of the pigment, but other ions such as Zn2+, Na+, K+ and Al3+ had faintly negative effects on its stability.

Development of A New Extraction Technique of Collagen from Channel Catfish Skin
BAO Shi-bao1,WANG Zhang2,*,XU Shi-ying2
2009, 30(10):  101-105.  doi:10.7506/spkx1002-6630-200910018
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Collagen was prepared from channel catfish skin by the steps of swelling in acetic acid, beating with blender, dissolving in diluted acetic acid, and neutralizing with sodium hydroxide solution (the final precipitate is collagen). In the present study, the conditions for swelling channel catfish skin in acetic acid were explored emphatically. The results showed that when channel catfish skin was swelled in 0.5 mol/L acetic acid for 6 h, the extraction yield of reached maximum, 92%. Subsequently, the obtained collagen was desalted by water-washing method, and then the impurity proteins in it were removed by neutral protease or alkaline protease. SDS-PAGE analysis indicated that no cleavage happed on α-chain of collagen during extraction and purification. Data from CD and X-ray showed that this purified collagen remained its structural integrity as triple-helix.

Optimization of Enzymatic Hydrolysis of Peanut Protein and Molecular Weight Distribution of Hydrolysates
LIU Li-na1,2,HE Dong-ping2,ZHANG Sheng-hua1,*
2009, 30(10):  106-110.  doi:10.7506/spkx1002-6630-200910019
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Peanut polypeptides were prepared from peanut protein by enzymatic hydrolysis. The effects of five factors such as enzyme kind, protease dose, hydrolysis time, hydrolysis temperature and pH value on degree of hydrolysis (DH) of peanut protein were investigated as well as the molecular weight distribution of hydrolysates. Quadratic regression rotational combination design was employed to optimize three key factors influencing hydrolysis of peanut protein. Results indicated that the optimum ranges for hydrolysis temperature, pH value and hydrolysis time were 44.9 to 47.6 ℃, 7.93 to 8.15 and 2.46 to 2.76 h, respectively. These optimized conditions resulted in the high DH of 19.61%. The peptides with molecular weight of below 1000 D accounted for over 84.73% of the obtained hydrolysates.

Optimization of Extraction Technology of Psidium guajava Seed Oil
GUO Shou-jun,YANG Yong-li,LUO Xue-yuan,HUANG Hai-tao,YI Zhen-qiang,SU Ting
2009, 30(10):  111-113.  doi:10.7506/spkx1002-6630-200910020
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Soxhlet method was applied to extract oil from Psidium guajava seed, in the present study. The extraction conditions were optimized by single-fact and orthogonal tests. Results indicated that the most significant factor influencing extraction yield of oil from Psidium guajava seed was temperature, followed by extraction time and solid to liquid ratio in turn. When extracting Psidium guajava seed with petroleum ether at the material to liquid ratio of 1 : 10 (W/V) ) for 3 h at 90 ℃, the best extraction effect could be obtained, and the extraction yield of Psidium guajava seed oil was 12.82%.

Effect of Steaming Process on Characteristics of Starch Granule in Steamed Rice Sponge Cake
CHEN De-wen1,2,SHEN Yi-liang1,WU Peng1,LI Xiu-juan1,XU Xiao-yun1,PAN Si-yi1,*
2009, 30(10):  114-117.  doi:10.7506/spkx1002-6630-200910021
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The characteristics of starch granule in steamed rice cakes at different pressures were analyzed by using SEM, Xray and DSC. Results indicated that with the pressure increasing, the starch granule structure was damaged gradually, and the characteristic diffraction peaks fell down and even disappeared, meanwhile the crystallinity declined and endothermic enthalpy reduced as well. When the pressure was 0.2 MPa, no crystal region was observed in the starch granule. In conclusion, high pressure could damage the starch granule structure in steamed rice cake.

Study on Desalination of Oat Protein Hydrolysate with Macroporous Adsorption Resin DA201-CⅡ
REN Qing1,ZHANG Xiao-ping1,ZHAO Shi-feng2,JIANG Qiong1, LIU Yong-guo1, DONG Yin-mao1,*
2009, 30(10):  118-122.  doi:10.7506/spkx1002-6630-200910022
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Several macroporous adsorption resins were applied to desalination of oat protein hydrolysate. The experiments of static adsorption and desorption showed that macroporous adsorption resin DA201-CⅡhad the highest adsorption-desorption capability and to oat peptides among 8 resins. In further study, the optimal desalination conditions of oat protein hydrolysate with the resin DA201-CⅡwere confirmed as follows: pH of oat protein hydrolysate 4.0, concentration of oat peptides 39 mg/ml, flow rate of water washing 1 BV/h, and desorption rate of 75% ethanol 1.5 ml/min. Under these conditions, the desaltion rate reached about 93.4%, and the recovery of oat peptides was about 72.3%.

Optimization of Storage Technology of Jiangshui Celery (Fermented Celery)
HE Ling1,YANG Gong-ming2,*
2009, 30(10 ):  123-126.  doi:10.7506/spkx1002-6630-200910023
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Effects of storage temperature, microwave treatment time, and potassium sorbate dose on storage of Jiangshui celery were investigated by three-factor quadratic general rotary design and a regression model with high reliability was established to optimize the above factors. Results showed that storage temperature and potassium sorbate dose had extremely significant effect on the sensory quality of Jiangshui celery (p < 0.01), but microwave treatment time took second place, exhibiting significant effect (p < 0.05). The optimal storage conditions of Jiangshui celery were as follows: storage temperature 0.5 ℃, potassium sorbate dose 0.45‰, and microwave treatment time 68.4 s (800 W).

Extrusion Functionalization of Corn Dietary Fiber and Effects of Particle Size on Its Physical Properties
ZHANG Yan-rong,BU Jia-ying,YANG Xiao-ying,WANG Da-wei*
2009, 30(10 ):  127-130.  doi:10.7506/spkx1002-6630-200910024
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Wet corn bran was washed with flowing water to remove residual starch and endosperm, centrifugalized, and dried. The dried corn bran was crushed and sieved into different particle sizes (60, 80, 100, 120 and 140 mesh) to prepare dietary fiber by removing fat, colored substances and odorous substances with supercritical carbon dioxide. Furthermore, the prepared corn dietary fiber was functionally treated by extrusion technology under 7 different combinations of water addition, extrusion temperature, feed rate and extrusion times. Effects of particle size of corn bran powder on oil retention capacity, expansion property, water holding capacity and water bonding capacity of prepared corn dietary fiber were investigated. The results showed that the comprehensive physical property of corn dietary fiber prepared from the corn bran powder with the particle size of 120 mesh (the particle size is 0.125 mm) was the best. When the extrusion was finished once under the conditions of water addition in corn dietary fiber 110%, temperature 180 ℃, feed speed 10 kg/h, the oil retention capacity and expansion property of extruded dietary fiber were the best, and the amount of soluble component was the highest.

Study on Determination and Extraction of Total Polyphenols from Leaves of Punica granatum L.
QIU Tao-tao1,WANG Hua2,*,MAO shi-hong1
2009, 30(10):  131-134.  doi:10.7506/spkx1002-6630-200910025
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Folin-Ciocalteu method was used to determine the content of total polyphenols from leaves of Punica granatum L.. The effect of extraction conditions on the extraction rate of total polyphenols from extracts was evaluated by single factor and orthogonal tests. The optimal extraction conditions of total polyphenols from leaves of Punica granatum L. are as follows: 75% alcohol as extraction solvent, temperature 70 ℃, extraction time1.5 h, material to liquid ratio 1:20 and 1 mm of particle size. Under these conditions, the maximum extraction rate of total polyphenols from leaves of Punica granatum L. was 16.63%.

Determination of Aflatoxin B1 in Food by Laser Induced Fluorescence-High Performance Capillary Electrophoresis
MA Liang1,2,ZHANG Yu-hao1,2,LI Pei-wu3,*
2009, 30(10):  135-139.  doi:10.7506/spkx1002-6630-200910026
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With self-made detection platform, a laser induced fluorescence-high performance capillary electrophoresis (LIFHPCE) method was developed for detecting aflatoxin B1 (AFB1) in food. AFB1 was separated under micellar electrokinetic capillary chromatography (MECC) mode (voltage 15 kV, and current 104 μA), excited by laser at the wavelength of 375 nm, and detected by LIF at the wavelength of 440 nm. The data showed that the linear relationship of AFB1 was nice (r = 0.9994) in 0.5 to 50 μg/kg concentration range. The lowest detection limit was 1.7×10-13g (S/N = 3) and the lowest quantitative limit of AFB1 was 5.6 ×10-13g (S/N=10). The repeatability and the precision expressed as RSD values are about 5%. The spike recovery was in the range of 84. 1% to 96.1% for AFB1 in food. This LIF-HPCE method can complete analysis within 10 min without derivative reaction or fluorescence labeling, and is suitable for high sensitivity determination of aflatoxins in food.

Analysis of Syringin Content in New Resource Acanthopanax.sessiliflorus (Rupr.et Maxim.) Seem and Other Seven Species of Acanthopanax Miq. by RP-HPLC
LI Li-li1,ZHENG Li-sheng1,LIU Xiang-qian1,*,ZHANG Xiao-dan1,OH Se-wook2
2009, 30(10):  140-143.  doi:10.7506/spkx1002-6630-200910027
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The objective of this study was to determine the contents of syringin in 8 species of Acanthopanax Miq. such as A. sessiliflorus (Rupr. et Maxim.) Seem, A. leucorrhizus (Oliv.) Harms var. fulvescens Harms et Rehd., Acanthopanax giraldii Harms, A. senticosus (Rupr. et Maxin) Harms, A. divaricatus var. albeofructus Yook, A. koreanum Nakai, A. gracilistylus W.W. Smith, and A.trifoliatus (L.) Merr by RP-HPLC. The column, mobile phase, flow rate, detection RP-HPLC were ODS C18 as An orthogonal experimental design was employed to optimize the extraction conditions of syringin. The method displayed good linearity within the concentration range of 0.0148 to 0.074 mg/ml (r = 0.9999) and a regression equation of Y = 15234560 X- 7 881.767 (R2 = 0.9999) was obtained. The average spike recovery was 98.24%. Acanthopanax leucorrhizus var.fulvescens Harms et Rehd. Had the highest content of syringin among the 8 species of Acanthopanax Miq., followed by A.sessiliflorus (Rupr. et Maxim.) Seem. The optimum extraction process of syringin was adding material to 15 times volume water and then boiling the water for 3.5 h. Our results suggested the simplicity and high reliability of this method to analyze syringin.

Optimization of Models for Quantitative Analysis of Tea Polyphenols in Green Tea by Near Infrared Spectrophotometry
LIN Xin,NIU Zhi-you*
2009, 30(10):  144-148.  doi:10.7506/spkx1002-6630-200910028
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158 non-comminuted and comminuted green tea samples were scanned by NIR Systems 6500 and InfraXact NIR analyzers. An analysis model for quantitation of polyphenols in green tea was developed through orthogonal test design and validated with principle component regression (PCR), partial least square (PLS) and modified PLS. The models were evaluated by the objective function method and the applicability of the optimal models was validated. The optimal model was obtained by using the NIR Systems 6500 analyzer with comminuted samples by modified PLS and the optimum analytic conditions for spectral data preprocessing were standard normal variate (SNV)/detrend scatter, second derivative treatment (the interval for one point), smoothing interval for four points and the secondary-smoothing interval for eight points. This optimal condition leaded to the objective function value of 95.74% and RSD and RPD of validation of 4.52% and 2.52, respectively. The results showed that orthogonal experiment design could comprehensively evaluate the effect of methods for validation and spectral data preprocessing on the models. Quantitative analysis of polyphenols could be realized by NIRS and this optimal NIRS model had very good precision and applicability.

Determination of Polycyclic Aromatic Hydrocarbons in Skin of “Peking Roast Duck” by High Performance Chromatography-Fluorescence Detection
LIAO Qian1,GAO Zhen-jiang2,ZHANG Shi-xiang3,LI Kai-xiong1,*
2009, 30(10):  149-152.  doi:10.7506/spkx1002-6630-200910029
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In the process of “Peking Roast Duck” with a novel heating technique, namely air jet impingement, polycyclic aromatic hydrocarbons (PAHs) may be formed. A method of HPLC coupled with fluorescence detector was developed for the determination of PAHs in fat- and protein-rich foods, such as “Peking Roast Duck”. Homogenized duck skin samples were pretreated by using methanol containing 2 mol/L KOH-water (8:2, V/V) for saponification, issoctane for extraction, methanolwater (1:1, V/V) for washing, DMF-water-issoctane (1:1:1, V/V) for liquid-liquid partition, and Florisil solid-phase column for cleaning up. Results showed that the recoveries of benzo[a]pyrene (B[a]P), dibenzo[a,h]anthracene (DB[a.h]A) and 7,12- dimethylbenzene[a] anthracene (7,12-DMB[a]A) in blank sample at the spiked amounts of 2 × 10-8 and 1 × 10-7 g were between 83.59% and 92.97%, and their recoveries at the spiked amount of 1, 2 and 2 μg/kg respectively, were 73.85% to 80.31%, and the RSDs were less than 10%. Their contents in roasted duck ranged from 0.56 to 3.19 μg/kg, but no these three compounds were found in raw duck. Our results suggested the high clean-up efficiency and recovery of this method and the sensitivity and accuracy of detection could meet the requirements for analysis of trace compounds in complex matrices. The B[a]P content of 0.56 μg/kg is far less than the maximum limit value of 5 μg/kg in the smoked and roasted foods in term of the national standards.

Ion Chromatography for Content Determination of Various Phosphate Forms in Tripolyphosphate
DENG Guang-hui1,2,HU Wei2,HUANG Ke-lin3,LI Shao-yan3,ZHANG Gui-hua1
2009, 30(10):  153-155.  doi:10.7506/spkx1002-6630-200910030
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An ion chromatography method was developed for determination of contents of various phosphate forms in tripolyphosphate, in the present study. Phosphates were eluted with100 mmol/L NaOH solution in gradient at a flow rate of 1.0 ml/ min. The method presented good linearities between the peak areas and concentrations of orthophosphate, pyrophosphate, tripolyphosphate, and trimetaphosphate and their detection limit ranged from 0.010 to 0.063 mg/L. The relative standard deviations (RSD) of the retention time varied between 0.38% and 0.79% and the RSD of the peak area was between 2.21% and 6.96%. The recoveries of the above phosphates in spiked tripolyphosphate sample ranged from 97.45% to106.89%. This complete analysis procedure lasted 10 min. Our results indicated that this method is rapid and accurate with a wide linear range and less consumption of chemicals.

Determination of Benzoyl Peroxide in Flour by Spectral Probe of Rhodamine B
DU Juan,SUN Dan
2009, 30(10):  156-158.  doi:10.7506/spkx1002-6630-200910031
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A new oxidation system, in Na2HPO4-KH2PO4 buffer (pH 6.84), with rhodamine B as the spectral probe was proposed for determination of benzoyl peroxide (BPO) in flour. Results indicated that this rhodamine B-BPO had an absorption maximum at 550 nm and the apparent molar absorption coefficient was 1.1×104 L/mol·cm. Beer's law was obeyed within the concentration of 0.00 to 0.80 mg/ml. The BPO detection limit by this method was 0.056 mg/ kg. The spike recoveries were between 97.5% and 101.0%, and the RSD were between 1.46% and 2.53%. Due to its easy operation and high recovery, this method could be applied directly to analyze trace benzoyl peroxide in flour.

Determination of Cyclopentadecanolide Synthesized from Malania oleifera Chun et S.K. Lee Kernel Oil by Gas Chromatography with External Standard Method
LAI Fang,LIU Xiong-min*,LI Wei-guang,MA Li
2009, 30(10):  159-161.  doi:10.7506/spkx1002-6630-200910032
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Gas chromatography (GC) with area-external standard method was applied to quantitative analysis of cyclopentadecanolide in its synthesis from Malania oleifera Chun et S.K. Lee kernel oil. A linear regression equation was obtained, which was A = 2238.7C (r = 0.9993), where A was the GC peak area, and C was the cyclopentadecanolide concentration, and the standard curve was validated by single-point external bracketing standard. The recoveries of cyclopentadecanolide in 3.578 mg of sample at the spiked amounts of 1.977, 3.954 and 5.931 mg were 95.11% to 103.3%, the RSDs were 1.51% to 2.19% (n = 3). The determination results of cyclopentadecanolide content in four prepared sample solutions were 2.14 to 4.52 mg/ml, and the RSDs were 0.66% to 2.36% (n = 3).

GC-MS Analysis of Fatty Acid Compositions in Fruits of Evodia rutaecarpa Benth. and E. lenticellata Huang.
ZHAO Hua1,TIAN Guang-hui2,GONG Hai-ming1,3
2009, 30(10):  162-165.  doi:10.7506/spkx1002-6630-200910033
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The liposoluble components were extracted from the fruits of Evodia rutaecarpan Benth. and Evodia lenticellata Huang. by Soxhlet extraction respectively. Their polar components were identified and determined by gas chromatographymass spectrometry (GC-MS) after methyl esterification treatment, and the relative percentage of each component was confirmed by peak-area normalization method. Total 45 kinds of fatty acid, including 14 unsaturated fatty acids and 31 saturated fatty acids, were identified from fruit oil of E. rutaecarpa Benth.. The main components of unsaturated fatty acids were tetradecdienoic acid (13.626%), 9,12-octadecadienoic acid (13.992%), 9,12,15-octadecatrienoic acid (10.153%), tetradectrienoic acid (4.603%), and (Z)-9-octadecenoic acid (2.207%), etc. While the main components of saturated fatty acids were hexadecanoic acid (15.506%), nonanedioic acid (5.363%), isoheptadecanoic acid (3.82%), octadecanoic acid (3.306%), and ferulic acid (2.909%), etc. Total 35 kinds of fatty acid, including 11 unsaturated fatty acids and 24 saturated fatty acids, were identified from the fruit oil of E. lenticellata Huang.. The main components of unsaturated fatty acids were tetradecdienoic acid (29.818%), 9,12-octadecadienoic acid (9.25%), 9,12,15-octadecatrienoic acid (6.699%), (Z)-9-hexadecenoic acid (2.736%), and (E)-9- hexadecenoic acid (2.717%), etc. While the main components of saturated fatty acids were hexadecanoic acid (16.411%), erulic acid (2.139%), octadecanoic acid (2.134%), m-coumaric acid (1.567%), and vinillic acid (1.475%), etc. It was shown that there are some important fatty acids in the fruits of E. rutaecarpa Benth. and E. lenticellata Huang., and both Evodia rutaecarpa Benth. and Evodia lenticellata Huang. have a potential development and application value in food nutrition and health care.

Rapid Determination of Common Sweeteners in Milk Beverage by HPLC
LU Lin1,2,HANG Yi-ping1,*,GAO Yan-hong2
2009, 30(10):  166-168.  doi:10.7506/spkx1002-6630-200910034
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To establish a rapid analysis method for determination of common sweeteners such as acesulfame potassium, saccharin sodium, sodium cyclamate, aspavtame, and alitame in milk beverage by HPLC. After the pretreatments of dilution, protein precipitation, and high-speed centrifugation, the sample was separated by Symmetry C18 column with phosphate buffer (pH 5.0) and acetonitrile as mobile phase, eluted gradiently, and detected at the UV wavelength of 205 nm. The analysis of one sample costs 12 min, and all five sweeteners could be well separated. The average spike recoveries of the above five sweeteners were 86.0% to 102%, and the RSDs were 2.1% to 5.6% (n = 6). This method is simple, quick, and of good reproducibility and selectivity, therefore it is an effective way to determine sweeteners in milk drink.

Determination of Trace Copper (II) in Foods by p-Phenanthroline-activated Catalytic Discoloring Spectrophotometry
ZHAO Li-jie1,ZHAO Li-ping1,CHANG Yong1,BAI Xiao-lin1,LIU Yong-hong2
2009, 30(10):  169-172.  doi:10.7506/spkx1002-6630-200910035
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With the activation of p-phenanthroline, potassium bromate oxidized methyl violet fading reaction catalyzed by copper (II) was investigated, and a new catalytic discoloring spectrophotometry for determining trace copper was proposed. The effects of acidity, reagent dosage, reaction temperature, reaction time, surfactant and coexisting ions on the reaction were discussed and the optimal conditions were investigated. After reaction at 72 ℃ for 15 min in a 25 ml volumetric flask, the calibration curve was drawn for the relationship of absorbance difference between copper (II) containing solution and non-copper (II) containing solution with copper (II) mass concentration, and then the content of trace copper (II) was determined by the absorbance difference. The detection wavelength of this method was 578 nm, the linear range was between 2.4×10-3 and 5.12× 10-2 μg/ml, and the detection limit was 2.4×10-6 g/L. When this method was applied to the determination of copper in green tea, wheat flour, rice, milk powder, and dried kelp, the maximum relative standard deviation was 4.22%, and the spike recoveries were 96.0% to 104.0%.

Analysis of Chemical Compositions of Seed Melon (Citrullus lanatus ssp. vulgaris var. megakasperms Lin et Chao) Seed by GC-MS
GUO Hua,HOU Dong-yan*,HUI Rui-hua,DIAO Quan-ping
2009, 30(10):  173-175.  doi:10.7506/spkx1002-6630-200910036
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Fatty acids were extracted from seed melon seed by Soxhlet extraction and 10 fatty acids were isolated and identified by gas chromatography-mass spectrometry (GC-MS). Linoleic acid, hexadecanoic acid and octadecanoic acid were the major fatty acids, accounting for more than 89.01% of total fatty acids. Volatile oil obtained by simultaneous distillation extraction method from seed melon seed was analyzed by GC and GC-MS. A total of 30 compounds were identified and alkane (22.44%), alcohol (17.22%), organic acids (12.86%) and ketone 2.36%) were the major components representing more than 60.55% of the oil.

Determination of Indoxacarb Residues in Vegetables and Fruits by Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry (UPLC-MS/MS)
JIANG Bin-wei
2009, 30(10):  176-178.  doi:10.7506/spkx1002-6630-200910037
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A new method was developed with ultra-performance liquid chromatography-tandem mass spectrometry (UPLCMS/MS) to determine indoxacarb pesticide residue in vegetables and fruits. Samples were extracted by acetonitrile and cleaned up on a solid-phase extraction (SPE)-PAK C18 cartridge column. The reconstituted sample solution was analyzed by UPLC-MS/MS under positive ion mode. Waters BEH C18 was taken as the analytical column, and 20 mmol/L ammonium acetate aqueous solution containing 0.1% formic acid-acetonitrile containing 0.1% formic acid was taken as the mobile phase. When fresh cabbage was the matrix, the spike recoveries of indoxacarb were 89.5% to 101.2% (n = 6), and the average recovery was 93.45%. When freezedried cabbage was the matrix, the spike recoveries of indoxacarb were 82.4% to 105.3% (n = 6), and the average recovery was 90. 6%. Both the within-day and inter-day RSDs (n = 6) were less then 5.0%. The detection limit of indoxacarb by this method was 0.05 μg/L (S/N = 3).

Determination of Fructoes, Glucose and Sucrose in Pumpkin by High Performance Liquid Chromatography- Evaporative Light Scattering Detection
WANG Pei-pei,SUN Ai-ling,LI Ai-feng,ZENG Qing-hua,LIU Ren-min*
2009, 30(10):  179-181.  doi:10.7506/spkx1002-6630-200910038
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Objective: To develop a simple, accurate and sensitive method for determination of fructose, glucose, sucrose, maltose and lactose in pumpkin. Methods: The sugars in pumpkin were extracted with hot water, separated on Kromasil NH2 column (250 mm × 4.6 mm, 5 μm) using acetonitrile and water (80:20, V/V) as the mobile phase, and examined using an evaporative light scattering detector. Results: The linear ranges of fructose and glucose, sucrose, were maltose and lactose 0.5 to 3 g/L, 0.75 to 5 g/L, 0.5 to 5 g/L, 1 to 10 g/L and 1 to 10 g/L respectively. Their detection limits were 1.90, 2.40, 1.80, 2.50 and 2.60 μg/L, respectively. The average spike recoveries were 99.0%, 97.1%, 98.9%, 99.5% and 102.4%, respectively, and the relative standard deviations were 1.02%, 1.41%, 1.27%, respectively. The determination results of fructose, glucose and sucrose in five saled pumpkin samples were 1.05% to 3.80%, 0.823% to 4.49%, and 0.090% to 5.19%, respectively, while no maltose and lactose were found in these pumpkin samples. Conclusion: This method is simple, fast and accurate, and can be applied to the determination of fructose, glucose and sucrose in pumpkin with satisfactory results.

Determination of Lead and Cadmium in American Ginsengs (Panax quinquefolium L.) of Different Years
QIN Gong-wei1, 2,CAO Xiao-yong1, 2,WANG Jing1,LI Jing1
2009, 30(10):  182-184.  doi:10.7506/spkx1002-6630-200910039
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The contents of toxic and harmful elements lead (Pb) and cadmium (Cd) were detected by microwave digestiongraphite furnace atomic absorption spectrometry (GFAAS) in American ginsengs of different years or from different plots. The results showed that the contents of cadmium and lead in American ginseng increased year by year in the same plot, while the contents in American ginseng of the same age had a certain difference among different plots. The limits of detection of Pb and Cd were 3.545 ng/ml and 0.225 ng/ml, respectively. The relative standard deviations of precision for Pb and Cd were 1.5% and 1.0%, respectively. The spike recoveries of Pb and Cd were 113.57% and 94.28%, respectively.

Improved Pre-treatment Method for HPLC Detection of Antiseptics in Wine
ZHAO Rong-hua,LI Ji-ming,LIANG Dong-mei
2009, 30(10):  185-187.  doi:10.7506/spkx1002-6630-200910040
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A new pre-treatment method was studied for detecting antiseptics in wine by HPLC method. Under acidic condition, wine sample was pre-treated by steam distillation (SD), and this approach was compared with general distillation and the national standard methods. Results showed that steam distillation was better than other two methods, and the recoveries of benzoic acid and sorbic acid reached 99.2% and 99.6%.

Optimization of Ultrasonic-assisted Extraction Conditions for Determination of Phytic Acid in Wheat Bran by FeCl3 Titration Method
WANG Guo-rong1,WAN Wen-gui1,WANG Li1,XIAO An-hong1,2,*
2009, 30(10):  188-190.  doi:10.7506/spkx1002-6630-200910041
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In order to determine phytic acid content in wheat bran, it was extracted with hydrochloric acid under the assistance of ultrasonic. The extraction conditions of phytic acid were optimized through single-factor and orthogonal tests. The results showed that the best extraction process was as follows: extracting wheat bran with 0.8 mol/L hydrochloric acid in 50 ℃ water bath for 1.5 h under the assistance of ultrasonic treatment at 700 W and 20 to 25 kHz for 15 min. Compared with non-ultrasonic method, the extraction time was shortened from 5 h to 1.5 h, while the phytic acid content was promoted from 5.5049% to 6.6341%.

Catalytic-kinetic Photometric Determination of Trace Formaldehyde in Yuba (Dried Beancurd Stick)
ZHOU Fu-lin,SONG Shao-fei,ZHANG Wen-chan,YANG Hui-juan
2009, 30(10):  191-194.  doi:10.7506/spkx1002-6630-200910042
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Based on the catalytic effect of formaldehyde on the reaction between potassium periodate and methyl red, a new catalytic-kinetic photometric method for the determination of trace formaldehyde was developed in the present study. The factors affecting the rate of catalytic fading reaction were investigated. Under the optimal conditions, the formaldehyde concentration within a range of 2.25×10-4 to 1.35×10-2 μg/ml had a good linear relationship with absorbance at 516 nm, the detection limit was 4×10-5 μg/ml, and the relative standard deviation (RSD) was 0.1% for determining 0.0041 μg/ml formaldehyde solution (n = 11). The method had high sensitivity and selectivity. When it is applied in the detection of trace formaldehyde in yuba, the spike recoveries were between 93% and 106%.

Determination of Azithromycin Residues in Chicken Tissues by HPLC-UV Detection
XU Guang-wei1,HUANG Chun-gui2,WANG Zhen1,YAN Wen-qin3,*
2009, 30(10):  195-198.  doi:10.7506/spkx1002-6630-200910043
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Objective: A highly sensitive and specific method for determination of azithromycin residues in chicken tissues by reverse-phase high-liquid chromatography was developed. Methods: Based on separation on a C18 column (4.6 mm×250 mm, 5 μm) at 210 nm with the mobile phase of acetonitrile-lsopropylalcohol-0.002 mol/L phosphate (60:15:25, V/V), samples were extracted by using chloroform-lsopropylalcohol (95:5, V/V), dried by nitrogen flow, and injected after dissolution in the mobile phase. Results: A good linear relationship was obtained in the concentration range of 0.05 to 5.0 μg/g (r>0.990). The limit of detection in serum was 0.02 μg/ml and the limit of quantification in tissue was 0.05 μg/g. The average recoveries were over 83% in serum and over 77% in tissues, respectively, and both the intra-day and inter-day relative standard deviations were less than 5%. Conclusion: The method is quick and accurate, has good repeatability, and accords with the requirement for determining residues of azithromycin in chicken tissues.

GC-MS Analysis of Volatile Oil Extracted from Indocalamus latifolius Leaves by Simultaneous Distillation and Extraction
ZHOU Yi,TAN Xing-he*,LI Qing-ming
2009, 30(10):  199-202.  doi:10.7506/spkx1002-6630-200910044
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The volatile components were extracted from leaves of Indocalamus latifolius by simultaneous distillation and extraction, and analyzed by gas chromatography-mass spectrum (GC-MS). From total 86 components, 64 components were identified, which accounted for 83.86% of the total peak area of the volatile oil. Among them, the major componnets were hexadecanoic acid (18.57%), anethole (11.16%), 6,10,14-trimethyl-2-pentadecanone (7.15%), oleic acid (3.31%), phytol (3.06%), ionone (3.04%), 2-methoxy-4-vinylphenol (2.51%),3-(2-hydroxyphenyl)-2-propenoic acid (2.51%), nonanal (1.22%), 2,6,6-trimethyl-1-cyclohexene-1-ethanol (1.20%), 5,6,7,7a,-tetrahydro-4,4,7a-trimethyl-2(4H)-benzofuranone (1.17%), 4-(2, 6,6-trimethyl-2-cyclohexen-1-yl)-2-butanone (1.16%), 1-methoxy-4-(2-propenyl)-benzene (1.11%), octadecanal (1.08%), (E)- 2-hexenal (0.94%), isophytol (0.89%), bis(2-ethylhexyl)phthalate (0.87%), benzene acetaldehyde (0.79%), pinane (0.79%), and cedrol (0.72%).

Quantitative Analysis of Rutin in Rosa roxburghii Tratt Fruit by HPLC
TIAN Hong-zhe,ZHOU Yan-ming,ZHAO Ying-bo,ZANG Jian,HU Rui
2009, 30(10):  203-205.  doi:10.7506/spkx1002-6630-200910045
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A method for determining rutin in Rosa roxburghii Tratt fruit by high performance liquid chromatography (HPLC) was developed. The powder of Rosa roxburghii Tratt fruit was extracted with ethanol under the assistance of ultrasonic, and the rutin extract was filtrated, concentrated by a rotary evaporator and centrifuged. The supernatant was filtered through a 0.45 μm filter membrane, diluted with mobile phase, and analyzed by reversed-phase liquid chromatography. The linear range of this method was 0.1 to 200 μg/ml, and the determination coefficient was 0.9988. The precision RSD was 2.10% (n = 5). The average spike recovery of rutin was 94.21%, and the RSD was 2.34%.

Continuous Determination of Lead, Chromium and Cadmium in Fruit and Vegetable by Microwave Digestion-Graphite Furnace Atomic Absorption Spectrometry
XU Xiao-yan,SUN Yuan-ming,SU Wen-zhuo,XIE Yu-wen
2009, 30(10):  206-208.  doi:10.7506/spkx1002-6630-200910046
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An effective method was developed for continuous determination of Pb, Cr and Cd in fruit and vegetable by using graphite furnace atomic absorption spectrometry (GFAAS) with microwave digestion. The effects of digestive reagent, digestion time and temperature on sample preparation were discussed, and the determination conditions by GFAAS were optimized. Under the optimum conditions, the linear ranges of Pb, Cr and Cd were 0 to 40 μg/L, 0 to 80 μg/L and 0 to 3μg/L and their detection limits were 0.293 μg/L, 0.037 μg/L and 0.850 μg/L, respectively. The precision relative standard deviations were between 2. 1% and 5.3% for determining the above three elements in flowering Chinese cabbage and snow pear by this method, and the spike recoveries range from 95.0% to 101.9%.

Determination of Clopidol Residue in Chicken by Ultra Performance Liquid Chromatography
YAN Xiao-feng,SUN Zhi-wen*
2009, 30(10):  209-211.  doi:10.7506/spkx1002-6630-200910047
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An ultra performance liquid chromatography (UPLC) method for determination of clopidol in chicken was developed. The clopidol residue in chicken was extracted by acetonitrile, defatted by n-hexane, purified by alumina B cartridges, analyzed by HPLC with UV detector at 267 nm and acetonitrile-water (10:90, V/V) solvent as mobile phase, and quantified by using external standard calibration curve. The results showed that there was a nice linear relationship (r > 0.999) when clopidol concentration was in the range of 10 to 1000 μg/L. The average recoveries at three addition levels (10, 50 and 100 μg/kg) were 60.5% to 94.6%. The within-day and inter-day variation coefficients were between 4.2% and 10.2% and between 6.6% and 12.7%, respectively. The limit of detection was 5 μg/kg, and the limit of quantification was 15 μg/kg.

Determination of Six Benzimidazoles Residues in Pork by SPE-HPLC
LIU Yong-jun,WU Yin-liang,JIANG Yan-bin,LIU Xing-guo,WANG Hai
2009, 30(10):  212-214.  doi:10.7506/spkx1002-6630-200910048
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Pork sample was extracted with ethyl acetate and purified by SPE- HLB cartridge. The analytes were further separated by HPLC and determined using PDA detector and quantified using external standard method. The results showed that there were good linear relationships between the peak areas and the concentrations of six benzimidazoles in the range of 20 to 1000 ng/ml (r> 0.99). The average spike recoveries of six benzimidazoles were 68.5% to 83.7% at the spiked levels of 0.05, 0.1 and 0.15 mg/L for blank sample, and the precision RSDs were 1.6 to 7.3.

Determination of Five Flavor Nucleotides in Penaeus chinensis Meat by RP-HPLC
CHEN Li-hua1,ZHANG Jian1,CHEN Pei-qiong1,ZHOU Pei-gen2
2009, 30(10):  215-218.  doi:10.7506/spkx1002-6630-200910049
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Contents of flavor nucleotides such as cytidine monophosphate (CMP), uridine monophosphate (UMP), guanosine monophosphate (GMP), inosine monophosphate (IMP) and adenosine monophosphate (AMP) in Penaeus chinensis meat were determined by reverse-phase high performance liquid chromatography(RP-HPLC). The detection was carried out on an Agela Alasil- C18 column at the wavelength of 260 nm with the mobile phase of CH3OH-0.05 mol/L KH2PO4 solution (1:1, V/V) at 0.8 ml/min. Five linear regression equations were obtained in the range of 0.00 to 0.10 mg/ml and the determination coefficients ranged from 0.9902 to 1.0000. The average spike recoveries of five flavor nucleotides were from 99.96% to 100.34% (n = 3) and the coefficients of variation were in the range from 0.040% to 0.39%. The contents of the above five flavor nucleotides in Penaeus chinensis meat were 18.86 ± 0.28, 0.95 ± 0.13, 44.35 ± 0.81, 50.79 ± 0.57, 139.96 ± 5.15 mg/100 g, respectively.

Determination of Tea Polyphones by Flow Injection Resonance Light Scattering Method
ZHONG Ming-hua
2009, 30(10):  219-221.  doi:10.7506/spkx1002-6630-200910050
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To establish a new flow injection resonance light scattering method for the determination of tea polyphones (TP), PbTP was determined by resonance light scattering method in acetic acid buffer medium at pH 7. The amount of TP can be determined directly by mensuring the resonance light scattering intensity of PbTP that is precipitated by reaction of TP with Pb (Ⅱ), and thus a flow injection analysis-resonance light scattering method was proposed to determine TP. The linear range of determination was 20 to 400 μg/ml. The detection limit was 6.62 μg /ml. This method was simple, consumed less reagent and had wide linear range. It can be applied to the determination of TP in tea.

Determination of Trace Elements in Seafood by Non-complete Digestion-Suspension Sampling-Flame Atomic Absorption Spectrometry
LIN Jian-yuan,NI Ming-feng
2009, 30(10):  222-224.  doi:10.7506/spkx1002-6630-200910051
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After dried, crushed and sieved, sea food samples (such as shrimps, crabs and pomfrets) were digested with concentrated nitric acid under heating condition until the solution became transparent. The digestion solution was mixed with emulsifier OP, and then suspended in 1.5 g/L agar solution. Finally, non-complete digested suspension was obtained to determine calcium, zinc and copper in these see food samples by flame atomic absorption spectrometry (FAAS). La2O3 was used as releasing agent to eliminate chemical interference to calcium determination. The relative standard deviations of determination were less than 3.0%. The non-complete digestion method-suspension sampling-flame atomic absorption spectrometry technique proved to be feasible for determining trace elements in seafood samples. This method is simple, fast and accurate.

Direct Determination of Harmful Elements in Food Additive DL-Tartaric Acid by Axial View Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES)
LU Dan
2009, 30(10):  225-227.  doi:10.7506/spkx1002-6630-200910052
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A new method was developed for the direct determination of harmful elements, such as Pb and As, in food additive DL-tartaric acid with axial view ICP-AES through simultaneous elevation of RF emission power and atomization gas flux. The working parameters of ICP-AES were optimized in this study. The results showed that the limits of detection (LODs) of Pb and As by this method were 0.003 mg/L and 0.005 mg/L, respectively, and the limits of quantification (LOQs) were 0.25 mg/kg and 0.41 mg/kg, respectively. The recoveries of Pb and As at two spiked amounts of 0.50 mg/kg and 1.00 mg/kg were 96.2% to 105.6%, and the relative standard deviations were 1.82% to 2.42%. In conclusion, this method can meet the demand of determining harmful elements in food additive DL-tartaric acid.

Microwave Digestion-Inductively Coupled Plasma Atomic Emission Spectrometric (ICP-AES) Determination of Iron, Zinc, Copper and Manganese in Osmanthus fragrans Flower Tea Substitute
YANG Wen-qiong1,DENG Zhen-ping2,*
2009, 30(10):  228-230.  doi:10.7506/spkx1002-6630-200910053
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A method was developed for simultaneous determination of multi-elements, such as Fe, Zn, Cu, and Mn in Osmanthus fragrans flower tea substitute by microwave digestion-ICP-AES. The parameters and working conditions of ICP-AES were optimized in this study. The results showed that the detection limits of Fe, Zn, Cu, and Mn were 1.6 × 10-3, 6.1 × 10-3, 2.5 × 10-3 and 5.3×10-3 mg/L, respectively. And the linear ranges were 0.0 to 20.0 mg/L, 0.0 to 5.0 mg/L, 0.0 to 5.0 mg/L, and 0.0 to 5.0 mg/L, respectively. The spike recoveries were 95% to 105% and the relative standard deviations (RSDs) were 0.88% to 2.74% (n = 12). This method is suitable for determining Fe, Zn, Cu, and Mn in Osmanthus fragrans flower tea substitute.

Development of One-step Enzyme-linked Immunoassay for Determining Enrofloxacin Residues in Sea Foods
LI Zong-yan,CAO Li-min*,LIN Hong,SUI Jian-xin
2009, 30(10):  231-235.  doi:10.7506/spkx1002-6630-200910054
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In this study, horseradish peroxidase (HRP) was used to label anti-enrofloxacin antibody through a sodium periodate oxidation method. A one-step competitive direct enzyme-linked immunosorbent assay (ELISA) was developed for determining enrofloxacin in sea foods. The results showed that the titer of labeled antibody was was higher than 10000, and no significant cross-reactivity was observed with other fluoroquinolones and other groups of antibiotics. The detection limit was 10 μg/kg. For eel samples spiked with enrofloxacin from 10 to 40 μg/kg, the average recoveries were above 70% and the relative standard deviations were lower than 6%. The determination time by this method was shortened to less than 2 h due to pre-coating and blocking in microplates, which was about half of that by traditional two-step ELISA.

Determination of o-Tyrosine in γ-Ray Irradiated Food by HPLC
WANG Dong-hui1,WANG Min2,*,HAN Li2,DENG Xiao-jun2,SHENG Yong-gang2
2009, 30(10):  236-238.  doi:10.7506/spkx1002-6630-200910055
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Objective: To develop a determination method of o-tyrosine in g-ray irradiated protein-rich foods by highperformance liquid chromatography coupled with pre-column derivatization. Methods: Sample was homogenized and purified by eliminating fat and sugars with the mixture of acetone and chloroform (3:1, V/V), and then deproteinated by means of hydrolysis with hydrochloric acid at 110 ℃ for 24 h. After reacting with derivative reagent, the sample digestion solution was subjected to HPLC analysis by external reference method. Results: The detection limit of o-tyrosine by this method was 5 mg/kg. The recoveries of o-tyrosine at the spiked amounts of 5, 10, and 50 mg/kg were 62.1% to 88.3%, and the coefficients of variation were 3.91% to 9.38% (n = 6). Conclusion: The o-tyrosine content in chicken and pork irradiated with 5 kGy and above ofγ-ray can be successfully detected, which is obviously higher than that in unirradiated meat samples and presents linear relationship with irradiation dose. After 3-month storage at -20 ℃, the o-tyrosine is still detectable in chicken and pork irradiated with 5 kGy and above ofγ-ray.

Identification of Anthocyanins from Daxing’anling Wild Vaccinium uliginosum Fruit
HU Ji-mei,JI Bao-ping*,ZHOU Feng,HAN Yong,SHUI Ming-lei
2009, 30(10 ):  239-241.  doi:10.7506/spkx1002-6630-200910056
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In this study, anthocyanins were extracted from Daxing’anling wild Vaccinium uliginosum fruit with 70% ethanol under the assistance of unltrasonic, and were subjected to qualitative and quantitative analysis by pH differential method. Furthermore, the extracts were separated into phenolic acids, anthocyanins and flavanones on Sephadex LH-20 column with different elution solutions. 13 kinds of anthocyanins were identified by HPLC-MS.

Development of Enzyme-linked Immunoassay for Detection of Gentamicin
MA Wei,WANG Bao-huan,LI Juan,XU Chuan-lai*
2009, 30(10 ):  242-244.  doi:10.7506/spkx1002-6630-200910057
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An immunogen, gentamicin-bovine serum albumin (BSA), was prepared by glutaraldehyde coupling method, and was identified by SDS-PAGE. New Zealand white rabbit was immunized with this immunogen three times. After immunization the antiserum with the titer of higher than 512000 was obtained. After purified by salting-out with ammonium sulfate, the obtained anti- gentamicin antibody was used to develop an indirect enzyme-linked immunosorbent assay (ELISA) for detection of gentamicin, with the detection limit of 0.1 ng/ml.

Determination of Aflatoxin B1 in Dry Capsicum by Enzyme-linked Immunosorbent Assay (ELISA)
XU Zhou1,TAN Shu-ming2,*,JIAO Yan-chao2,ZHANG Yun-fang3
2009, 30(10):  245-247.  doi:10.7506/spkx1002-6630-200910058
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In this study, aflatoxin B1 in dry capsicum was detected with ELISA kit, and the prevention and control measures of aflatoxin B1 were proposed. The results showed that the detection sensitivity was 0.1 μg/kg, the relative standard deviation (RSD) in 6 parallel determinations was less than 3% and the average spike recovery rate was 97%. This method is accurate, and has well stability and reproducibility, so it can be applied to detect effectively aflatoxin B1 in dry capsicum. Reducing oxygen content and controlling relative humidity below 80% in storage environment of dry capsicum is favorable for preventing aflatoxin B1 generation. The physical methods (adsorption, heat treatment and ray irradiation), chemical methods (oxidation and reduction, acid and alkali treatment) and biological methods (microbes and enzymes) are available to reduce aflatoxin B1 content.

Comparison and Analysis of Chemical Constituents in Volatile Oils from Myrica rubra Fruit and Leaves
XU Ling-ling1,YANG Xiao-dong1,*,HAN Zheng2,WU Yong-jiang2,ZHANG Qing-hui3
2009, 30(10):  248-251.  doi:10.7506/spkx1002-6630-200910059
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Objective: In order to provide theoretical bases for developing Myrica rubra leaves and processing and preserving Myrica rubra fruit, the chemical constituents in volatile oils from Myrica rubra cv Dongkui leaves, fresh fruit and stale fruit were analyzed and compared. Methods: Direct distillation extraction method (DDE) was applied to extract volatile oils, and the chemical constituents in the volatile oils were analyzed by GC-MS. Results: Great changes occurred in the kind and content of chemical constituents in the volatile oil from Myrica rubra cv Dongkui fruit during storage. The volatile oil from Myrica rubra cv Dongkui leaves contained some flavor components, such as caryophyllene and nerolidol, and antibacterial components. Conclusion: The kind and content of chemical constituents in the volatile oil from Myrica rubra cv Dongkui fruit, such as terpenes, aldehydes, ketones and esters, reduce evidently in the volatile oils of Myrica rubra fruit during storage, especially caryophyllene content, which may lead to flavor change and decay. The chemical components in the volatile oil from Myrica rubra leaves have certain preservation effect on Myrica rubra cv Dongkui fruit.

Analysis of Changes in Aroma Components of Pu-erh Tea during Post-fermentation Process
LU Cai-you1,2,SHAN Zhi-guo3,LIU Qin-jin1,*
2009, 30(10 ):  252-256.  doi:10.7506/spkx1002-6630-200910060
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Objective: To reveal the origin of aroma substances in ripe Pu-erh tea and provide guidance for the production of ripe Pu-erh tea by exploring the changes in aroma components during post-fermentation process. Methods: Simultaneous distillation-solvent extraction was applied to extract aroma compounds from Pu-erh tea samples at different post-fermentation stages, and the aroma compounds were analyzed by GC-MS. Besides, these Pu-erh tea samples were subjected to sensory evaluation. Results: 65 kinds of aroma components were totally identified in Pu-erh tea samples at different post-fermentation stages, including 11 hydrocarbon kinds, 10 alcohol kinds, 13 aldehyde kinds, 10 ketone kinds, 6 acid kinds, 6 ester kinds, and 9 other compound kinds. The main aroma components of sunshine withering tea were linalool, 4-phenyl-pyridine, phytol, 3,7 dimethyl-1,6- octadiene-3-alcohol, n-palmitic acid, and 4-methyl-2-propyl-1-pentanol, and those of ripe Pu-erh tea were npalmitic acid, dihydro-kiwi lactone, dihydro lactone anemones, diethyl-2-13 methyl alcohol, and trans-keto-β-malaysia. The relative contents of ketones, aldehydes, acids, and esters increased, but those of alcohols and other compounds decreased over the post-fermentation process. Both type and quantity of methylated substances presented rising trend with the post-fermentation extending. The sensory evaluation indicated that the change from clean aroma to stale flavor occurred in the process from sunshine withering tea to ripe Pu-erh tea.

Analysis on Aroma Compounds in Dry Red Wine of Cabernet Sauvignon in Hexi Corridor
SONG Hui-li1,HAN Shun-yu1,*,JIANG Yu-mei1,CHEN Yan-xiong2,ZHU Xia1
2009, 30(10):  257-260.  doi:10.7506/spkx1002-6630-200910061
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Aroma compounds in juice and dry red wine of Cabernet Sauvignon planted in Hexi Corridor were determined by headspace solid-phase microextraction-gas chromatography-mass spectrometry. 130 aroma compounds were identified totally, in which, 35 kinds of aroma compounds were common in Cabernet Sauvignon juice and dry red wine, 40 kinds of aroma compounds were unique in Cabernet Sauvignon juice, and 52 kinds of aroma compounds were unique in Cabernet Sauvignon red wine. The result of comparative analysis showed that the relative contents of isoamyl alcohol, isobutanol, phenethyl alcohol, ethyl caprate and ethyl octanoate in the dry wine were higher than them in the juice about 41.83%, 5.32%, 0.81%, 10.93% and 3.7% respectively.

High Performance Liquid Chromatography (HPLC) for Detection of Cyclamate in Liquor
ZANG Guang-lou1,DONG Ming-sheng2,*
2009, 30(10 ):  261-264.  doi:10.7506/spkx1002-6630-200910062
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A HPLC method was developed for detect cyclamate content in liquor. The regression equation between peak area (y) and cyclamate concentration (x) was established as following: y = 0.0008x + 0.0147(R2 = 0.9991). The recovery rates cyclamate at the spiked amounts of 2 to 100 μg/ml ranged 97% to 115%, and the relative standard deviation (RSD) of 6 repeated detections was 4.1%. The limits of quantitative detection and quantitative detection were 1.5 μg/ml and 5.0 μg/ml, respectively.

Experimental Research on Application of Kinetic Model to Predict Shelf-life of Pampus argenteus
TONG Yi,XIE Jing*
2009, 30(10):  265-268.  doi:10.7506/spkx1002-6630-200910063
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Total viable count (TVC), total volatile base-nitrogen (TVB-N) value, freshness index (K value) and sensory evaluation of Pampus argenteus (pomfret) at different storage temperatures were assessed to investigate the relation between the shelf life and temperature. The Arrhenius models of TVC, TVB-N value and K-value with respect to storage time and temperature were developed. The high regression coefficients(R2 > 0.9)indicated the acceptability of the first order reaction and Arrhenius model for predicting the changes of TVC, TVBN value and K-value of pomfret. The activation energy (EA) and preexponential factor (k0) of TVC, total volatile base-nitrogen value, and K-value prediction models were 47.60 kJ/mol and1.568 × 109, 50.80 kJ/mol and1.490 × 109, and 43.81 kJ/mol and 3.553 × 107 respectively.

Controlling Technology of Peel Browning of “Fengjie” Navel Orange Fruits
GAO Xue1,LI Zheng-guo2
2009, 30(10):  269-272.  doi:10.7506/spkx1002-6630-200910064
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Effects of preharvest calcium spray, bag cover, waxing and postponed harvest on peel browning and qualities of “Fengjie” navel orange (Citrus sinensis Osbeck) were investigated during storage. Results indicated that peel browning was significantly reduced by preharvest calcium spray and bag cover during storage (p < 0.01). Besides, this preharvest calcium treatment also improved skin redness of fruit as well as its quality. However, the peel browning of “Fengjie” navel orange was markedly enhanced by postharvest waxing and postponed harvest. The results suggested that calcium deficiency, waxing, and unsuitable collecting time might be important factors inducing peel browning in navel orange fruits.

Influence of Exogenous Nitric Oxide on Enlargement of Garlic Scape and Membrane Lipid Peroxidation
TU Yin-hua,HUI Wei*,HUANG Liang-ying,LI Cai-xiang,NIU Rui-xue
2009, 30(10):  273-277.  doi:10.7506/spkx1002-6630-200910065
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The diameter of garlic bulbet is seemed as the aging index of postharvest garlic scape and the redistribution of cell contents affects seriously the edible value of garlic scape. In this study, the basal garlic scape was treated with various concentrations(0.1,0.2,0.3,0.4 mmol/L)of sodium nitroprusside (SNP), 0.1 mmol/L sodium nitrite and 0.1 mmol/L potassium ferricyanide for three hours, respectively, dried and then stored at 4 ℃. During the storage of garlic scape, the diameter of garlic bulbet and activities of related antioxidant enzymes were subjected to regular determination. The results showed that compared to control, the diameter enlargement of garlic bulbet and increases of content of hydrogen peroxide, activity of peroxidase (POD) and cell membrane permeability in the basal garlic scape were inhibited by treatment of different concentrations of SNP, but the activities of superoxide dismutase (SOD), catalase (CAT) and ascorbate peroxidase (APX) in garlic scape, and POD in apical garlic scape were increased by treatment of different concentrations of SNP in the storage process. Compared to the control (the garlic scape sample whose basal was soaked in distilled water for 3 h), different concentrations of SNP could effectively restrain the diameter enlargement of garlic bulbet and the content increase of hydrogen peroxide. 0.1 mmol/L SNP treatment presented the most remarkable effect (p < 0.05). No significant difference was found in diameter of garlic bulbet and activities of related antioxidant enzymes between 0.1 mmol/ L sodium nitrite or 0.1 mmol/L potassium ferricyanide-treated garlic scape and the control. Based on these, we concluded that exogenous nitric oxide can inhibit the diameter enlargement of garlic bulbet, and this effect may be related to inhibiting the content increase of hydrogen peroxide in the basal of garlic scape.

Preservation Effects of 1-Methylcyclopropene on Fresh-cut Hami Melon
XIE Shao-zhong,WU Bin,ZHONG Mei,XIAO Li-mei,WANG Ji-de*
2009, 30(10):  278-281.  doi:10.7506/spkx1002-6630-200910066
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This study aimed to investigate effects of 1-methylcyclopropene (1-MCP) on postharvest physiology, quality and safety of fresh-cut Hami melon (Cucumis melo L. var. inodorus Jacq 8601) during storage at 5 ℃. The results indicated that the 1.0 μl/L 1-MCP treatment significantly inhibited the ethylene production, transparency rate and microbial quantity, reduced the lipid peroxidation level of cell membrane, maintained the fruit firmness, soluble solid content (SSC), vitamin C content of and good sensory quality, and prolonged the shelf life of fresh-cut Hami melon.

Study on Processing Technology of Carrot Juice Concentrate
HUANG Cheng1,ZHOU Chang-chun2,3,YIN Hong1
2009, 30(10):  282-285.  doi:10.7506/spkx1002-6630-200910067
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In the processing technology of carrot juice concentrate, pectinase dose affecting carrot juice yield and working parameters of triple effect vacuum flasher for concentrating carrot juice were optimized. The results showed that the carrot juice yield could be increased by 20% when treating crushed carrot pulp with 150 mg/kg of pectinase for 50 min at 50 ℃. The optimal working parameters of triple effect vacuum flasher were determined by orthogonal test as follows: concentration temperature 50 to 55 ℃, vacuum degree 9.33×104 to 10.0×104 Pa, steam pressure 7.5 ×104 to 8.0×104 MPa, and carrot juice flux 6.0× 103 to 6.5×103 L/h. When stored at not higher than -18 ℃, the pH value, and total acid and β-carotene contents of concentrated carrot juice had little changes.

Development of Compound Beverage of Sweet Potato, Milk and Orange
GU Ren-yong,YAO Mao-jun,YIN Yong-zhong
2009, 30(10 ):  286-289.  doi:10.7506/spkx1002-6630-200910068
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Taking sweet potato, orange and milk as main raw materials, a new compound beverage was developed in this study. In the processing technology, color protection method for sweet potato, ratio of sweet potato juice to milk to orange juice, ratio of compound stabilizers (carrageenan and glutin), and compound beverage formula were optimized. The results showed the color of sweet potato could be better protected when it was firstly blanched in hot water at 95 to 100 ℃ for 2 to 3 min, and then soaked in the solution containing NaCl (2.0%) and citric acid (0.2%) for 30 min. The optimal ratio of carrageenan to glutin was 1:2, the optimal ratio of sweet potato juice to milk to orange juice was 20:5:3, and the optimal formula of compound beverage was as follows (in 1 L of compound juice): citric acid 1.0 g, sucrose 40.0 g, honey 8.0 g, and compound stabilizers 2.5 g.