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Table of Content

25 June 2012, Volume 33 Issue 12
Processing Technology
Optimization of Ultrasound-Assisted Extraction of Cornus officinalis Seed Oil by Response Surface Methodology and Chemical Composition Analysis
LIU Rui-lin,ZHAN Han-ying,CHEN Tian,MOU Zhao-li,JIA Xiao-meng,ZHANG Zhi-qi
2012, 33(12):  1-7.  doi:10.7506/spkx1002-6630-201212001
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Response surface methdology was employed to optimize the ultrasound-assisted extraction of Cornus officinalis seed oil. Meanwhile, its chemical composition was analyzed by GC-MS. The optimal extraction conditions were determined as 40 ℃ of extracion temperatrure, 40 min of extraction time, and 10:1 of liquid-to-solid raio (mL/g). Under these conditions, the extraction yield of Cornus officinalis seed oil based on the dry weight of Cornus officinalis kernels was 7.90%, accounting for 97.08% of that obtained from Soxhlet extraction. The predominant fatty acids in Cornus officinalis seed oil were oleic acid (61.89%), stearic acid (19.99%), palmitic acid (7.63%), linoleic acids (6.33%), and so on. The percentage of unsaturated fatty acids relative to total fatty acids was 69.45%. In addition, the vitamin E content in Cornus officinalis seed oil, as determined by HPLC, was 76.0 mg/100 g.
Orthogonal Array Optimization of Ultrasonic-Assisted Extraction of Panax notoginseng Saponin Rg1
ZHOU Guo-yan,WANG Chun-xia,SANG Ying-ying,HU Xiao-liang
2012, 33(12):  8-11.  doi:10.7506/spkx1002-6630-201212002
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The ultrasonic-assisted extraction of Panax notoginseng saponin Rg1 was optimized using an L9(34) orthogonal array design based on one-factor-at-a-time experiments. The effects of ethanol concentration, material-to-liquid ratio, ultrasonic frequency and extraction time on extraction efficiency were examined. Ethanol concentration had the highest effect on extraction efficiency, followed by extraction time and material-to-liquid ratio; the effect of ultrasonic frequency was the weakest. The optimal levels of ethanol concentraion, material-to-liquid ratio (g/mL), ultrasonic frequency and extraction time were 70%, 1:12, 59 kHz and 60 min, respectively. Under the optimized extraction conditions, the extraction yield of saponin from Radix Panax notoginseng was 1.85%.
Optimization of Lipase-Catalyzed Synthesis of Ethyl Hexanoate in Solvent Free System by Response Surface Methodology
ZHAO Lei,CHENG Yue,WANG Cheng-tao
2012, 33(12):  12-17.  doi:10.7506/spkx1002-6630-201212003
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Objective: To optimize lipase-catalyzed synthesis of ethyl hexanoate in a solvent-free system. Methods: One-factor-at-a-time experiments were cairred out to identify lipase amount, molar ratio of hexanoic acid to ethanol and reaction time as main variables that influence ethyl hexanoate yield for response surface optimization based on a three-vairable, five-level central composite design. Results: The optimum conditions for lipase-catalyzed synthesis of ethyl hexanoate were determined as 0.5% of enzyme amount, 1:1.3 of molar ratio of hexanoic acid to ethanol, 12.2 h of reaction time and 30 ℃ of reaction temperature, and 150 r/min of rotary speed. Under these conditions, the experimental value of ethyl hexanoate yield was 81.6%, which was close to the predicted value (87.7%). Conclusion: It is feasible to optimize lipase-catalyzed synthesis of ethyl hexanoate in a solvent-free system by response surface methodology.
Enzymatic Synthesis and Physicochemical Properties of MLM-Type Structured Lipids
PAN Li-jun,SHOU Jia-fei,FU Ke-huang,CAO Li-li,JIANG Shao-tong
2012, 33(12):  18-23.  doi:10.7506/spkx1002-6630-201212004
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Monoglycerides were prepared through alcoholysis and used for the synthesis of MLM-type structured lipids through its esterification with caprylic acid under the catalysis of immobilized 1,3-specific lipase. The optimal esterifcation conditions, as determined using orthogonal array design based on one-factor-at-a-time experiments, were 9% of lipozyme RM IM lipase concentration (on the basis of substrate mass), 14 h of reaction time, 40 ℃ of reaction temperature, and 1:6 of molar ratio of MAGs to caprylic acid. Under these conditions, the incorporation rate of caprylic acid was 60.48%, and 92.84% caprylic acid was distributed at the 1or 3 position of glycerol. Purified MLM-type structured lipids were obtained after subsequent two-step molecular distillation with an incorporation rate of 73.34% for caprylic acid. The physicochemical properties could comply with the national standards of Grade 4 rapeseed oil at least.
Extraction of VE from Pumpkin Seed Oil Sediment by Molecular Distillation
LIU Lei,CHEN Xing,WU Qiong,LIU Bo
2012, 33(12):  24-27.  doi:10.7506/spkx1002-6630-201212005
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Response surface methodology was used to optimize VE extraction from pumpkin seed oil sediment. A mathematical model for VE yield as a function of extraction temperature, vacuum degree and scraper speed was built. The optimal extraction conditions were extraction temperature of 220.26 ℃, vacuum degree of 0.11 mbar and scraper speed of 649.3 r/min. Under these extraction conditions, the predicted extraction rate of VE was 83.31%, which was close to the actual yield of 84.25%. Therefore, the regression model revealed excellent fitting degree and could meet the design requirements.
Preparation and Characterization of Sarafloxacin Imprinted Polymer
QUAN Ying,XUE Xing-jie,CHEN Meng-ling,ZHAN Yue-hua,DING Jian-ying,ZHANG Gen-hua
2012, 33(12):  28-31.  doi:10.7506/spkx1002-6630-201212006
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A molecularly imprinted polymer (MIP) was synthesized by bulk polymerization method using propionamide as the template, methylacrylic acid as the functional monomer and ethylene glycol dimethacrylate as the cross-linker. Adsorption experiments were carried out on the MIP with perfect molar ratio of 1:26 between the template and the monomer. The adsorption isothermal curves of MIP and NMIP showed that the adsorption quantity of sarafloxacin in the cavity formed by MIP was higher than that of NMIP. Two kinds of binding sites were observed between the imprinted polymer and the template (sarafloxacin). Their deassiocation constants (Kd) were 0.321 μg/mL and 1.577 μg/mL, and the apparent maximum absorption capacity (Qmax) were 1.249 mg/g and 3.222 mg/g, respectively. The adsorption dynamic curve of MIP displayed that the adsorption of sarafloxacin on MIP could reach equilibrium within 7 h. Therefore, MIP has good adsorption capacity for sarafloxacin.
Quality Improvement of Bitter Buckwheat Tea Based on QFD
GUO Yuan-xin,ZHANG Bing-quan,YE Hua,SHEN De-yan
2012, 33(12):  32-36.  doi:10.7506/spkx1002-6630-201212007
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Based on the application of quality function deployment (QFD) theory, consumer needs for bitter buckwheat tea was converted into the technological parameters for the product design, thus improving the processing requirements during the preparation. Through quality improvement of bitter buckwheat tea, practical and feasible technological parameters were achieved and a novel thought for the development of other new products was proposed.
Optimization of Ultrasonic Extraction of Flavonoids from Wolfberry Bee Pollen Using Response Surface Methdology
RAN Lin-wu,YAN Ya-mei,CAO You-long,ZENG Xiao-xiong,QIN Ken,WEI Zhi-ying
2012, 33(12):  37-40.  doi:10.7506/spkx1002-6630-201212008
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On the basis of one-factor-at-a-time eperiments and central composite rotary design (CCRD) experiments, the ultrasonic extraction of flavonoids from wolfberry bee pollen was optimized and a mathematical regression model was contructed. Eththanol concentration was the most significant parameter that influences extraction efficiency, followed by material-to-liquid ratio; extraction time had the weakest influence. The optimal extraction conditions were ethanol concentration of 75%, extraction time of 95 min and material-to-liquid ratio of 1:40 (g/mL). Under these extraction conditions, the average experimental extraction yield of flavonoids was 3.03% (n = 3), which was consistent with the predicted result.
Optimization of Procyanidins Extraction from Faba Bean Episperm
ZHANG Hong,LIU Zhang-wu
2012, 33(12):  41-45.  doi:10.7506/spkx1002-6630-201212009
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The process conditions for procyanidins extraction from faba bean episperm by microwave pretreatment followed by ethanol extraction were investigated. The effects of microwave pretreatment conditions (microwave power, microwave treatment time, water-to-faba bean episperm powder ratio) and extraction conditions (70% ethanol-to-faba bean episperm powder ratio, temperature and time) on the extraction yield of procyanidins were explored. The results showed that the optimum conditions for microwave pretreatment and ethanol extraction were obtained as follows: faba bean episperm powder was soaked in water at a liquid-to-solid ratio of 2:1 (mL/g) before microwave pretreatment at 140 W for 50 s and subsequent extraction for 72 min with 70% ethanol at a liquid-to-solid ratio of 21:1 (mL/g), 55 ℃. Under these conditions, the extraction recovery of procyanidins was 94.53%.
Optimization of Thermal Treatment of Fresh Chinese Prickly Ash (Zanthoxylum schinifolium Sieb.et Zucc)
PU Biao,YAO Jia
2012, 33(12):  46-51.  doi:10.7506/spkx1002-6630-201212010
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In order to extent the storage period of Chinese prickly ash (Zanthoxylum schinifolium Sieb.et Zucc), a high-temperature short-time (HTST) steam treatment method was presented for Chinese prickly ash. A series of one-factor-at-a-time experiments were carried out to investigate the effects of steam pressure, treatment time and material load on volatile oil content and POD activity of Chinese prickly ash from Hanyuan. The best processing conditions, as determined using response surface analysis based on central composite design, were steam pressure 0.33 MPa, treatment time 12.4 s and material load 2696 g/m2. After thermal treatment under these conditions, the predicted volatile oil content was 0.41 mL/20 g.
Formulation Optimization for Clarified Blueberry Juice Beverage by Response Surface Methodology
GE Ying-liang,MA Yan-qiu
2012, 33(12):  52-57.  doi:10.7506/spkx1002-6630-201212011
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This paper reports the optimization of stabilizer formulation by orthogonal array design and the optimization of clarified blueberry juice beverage formulation by response surface methodology. The best stabilizer formulation was composed of xanthan, sodium alginate and β-cyclodextrin at a mass ratio of 1:1:1. The best clarified blueberry juice beverage formulation consisted of blueberry juice 12%, sugar 2%, citric acid 0.15%, and complex stabilizer 0.05%. The resulting beverage showed a mellow blue color, a palatable balance between sweet and tart, and abundant nutrients and had certain healthcare functions.
Pre-treatments of Whey Protein before Ultrafiltration Condensation
LEI Jing,LI Kai-xiong,LU Shi-ling,LIU Jie-jie,XIANG Yan-hong
2012, 33(12):  58-62.  doi:10.7506/spkx1002-6630-201212012
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In order to improve the permeability and ultrafiltration efficiency of whey protein, the flocculation of whey protein with CaCl2 was optimized by one-factor-at-a-time and orthogonal array design methods based on protein content, fat content and transmittance. The optimal flocculation conditions were determined as pH 7.5, 1 mol/L CaCl2 addition at a ratio of 12 mL/L, and gentle stirring on 60 ℃ water bath for 15 min. After these pretreatments, the loss rate of whey protein was only 13.6%, the defatting rate was over 86%. Meanwhile, the transmittance was significantly improved.
Optimization of Extraction Process for Flavonoids from Artemisia anethifolia Web. ex Stechm by Response Surface Methodology and Evaluation of Their Antioxidant Activity
LIU Yu-fen,XIA Hai-tao
2012, 33(12):  63-68.  doi:10.7506/spkx1002-6630-201212013
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Response surface methodology was employed to optimize the extraction of flavonoids from young stems and leaves of Artemisia anethifolia Web. ex Stechm. Meanwhile, the antioxidant activity in vitro was evaluated by hydroxyl radical scavenging assay, superoxide anion radical scavenging assay, total reducing power assay, and anti-lipid peroxidation assay with vitamin C as the reference. The results indicated that the optimal extraction conditions were extraction temperature of 80 ℃, extraction time of 1.75 h, material-to-liquid ratio of 1:27.5, and repeated extraction number of 2. Under these extraction conditions, the predicted and actual values of flavonoids yield were 3.002% and 2.996%, respectively. Artemisia anethifolia Web. ex Stechm flavonoids revealed a relatively weaker scavenging effect on superoxide anion radicals when compared with vitamin C, but revealed better scavenging effect on hydroxyl free radicals, stronger inhibitory activity on lipid peroxidation and higher reducing power. Therefore, Artemisia anethifolia flavonoids are effective natural antioxidants.
Process Design and Optimization for Separation of L-Lactic Acid by Continuous Ion Exchange
JIANG Shao-tong,YU Li-tao,LI Xing-jiang,WU Xue-feng
2012, 33(12):  69-74.  doi:10.7506/spkx1002-6630-201212014
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Over the traditional fixed bed ion exchange, continuous ion exchange has several significant advantages for the separation of L-lactic acid, such as continuous, stable and efficient. Economic, continuous and efficient separation of L-lactic acid was achieved using a continuous ion exchange process designed based on the results of static adsorption and fixed-bed ion exchange. Through static adsorption experiments, 732 type resin was identified as the best resin, which could reach adsorption equilibrium within 1 min with a maximum adsorption quantity of 345.97 mg/g. The best desportion agent was 0.5 mol/L H2SO4. In fixed bed ion exchange experiments, a desorption rate of over 97% was obtained under the conditions: sample loading flow rate 40 mL/min, column height-to-diameter ratio 7.5:1, breakthrough time 21.5 min, and desportion with 0.5 mol/L H2SO4. In continuous ion exchange experiments, the optimal sample loading flow rate at the exchange areas (1#-6#), washing areas after exchange (18#-20#), regeneration areas (12#-17#), washing areas after regeneration (9#-11#), top water areas with product (7#-8#) were 40, 40, 140, 35 mL/min and 20 mL/min, respectively. Each outlet concentration showed a cyclical change.
Treatment of Lychee Juice with Ceramic or Polyether Sulfone Ultrafiltration Membranes: Analysis of Membrane Fouling and Lychee Juice Quality
ZHANG Jing,JIANG Bing,BI Xiu-fang,QIU Dan-dan,HU Xiao-song,LIAO Xiao-jun
2012, 33(12):  75-82.  doi:10.7506/spkx1002-6630-201212015
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The objective of this study was to develop a membrane separation process for the clarification of lychee juice. The effects of trans-membrane pressure (TMP) and axial feed flow rate (Qf) on permeation flux (Qp) under total recycle mode (TRM) during the clarification of lychee juice with ceramic or polyether sulfone membranes were investigated to determine their individual optimal levels. Further, their optimal levels were analyzed when considered concurrently under batch treatment mode. Ceramic membrane was more effective in clarifying lychee juice than polyether sulfone membrane. The optimal operating conditions for clarifying lychee juice with ceramic membrane were determined as 0.3 MPa of TMP and 40 L/min of Qf. Meanwhile, the cause of membrane fouling under batch treatment mode was explored. The R2 obtained from fitting dJ/dt = k(J -Jlim) J2 - n was 0.8812 and 0.8478 for ceramic membrane and 0.9048 for polyether sulfone membrane. Membrane fouling depended on cake filtration (n = 0) for polyether sulfone membrane and dynamic changes between partial pore blocking (n = 1) and cake filtration (n = 0) for ceramic membrane. The dynamic changes of total sugar, total pectin, total protein, antioxidant ability were examined during membrane filtration under batch treatment mode. Ceramic membrane was significantly more effective in maintaining some quality indexes such as total sugar, antioxidant activity and total phenol than polyether sulfone membrane, while no significant difference was observed in other quality indexes.
Optimization of Nucleosides Extraction from Rape Bee Pollen Using Response Surface Methodology
SUN Li-ping,HUANG Lan,XU Xiang,PANG Jie,HE Wei,MU Xue-feng,SHEN Xin-feng
2012, 33(12):  83-88.  doi:10.7506/spkx1002-6630-201212016
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Nucleosides extraction from rape bee pollen was optimized using response surface methodology. The appropriate ranges of extraction time, extraction temperature and material-to-liquid ratio were obtained by one-factor-at-a-time experiments for subsequent optimization using response surface analysis based on a three-variable, three-level central composite design. The optimal ranges of extraction time, extraction temperature and material-to-liquid ratio were 40-60 min, 45-65 ℃ and 1:60-1:80 (g/mL), respectively. The optimized extraction conditions were 53 min, 60 ℃, and 1:70 (g/mL). Under these conditions, the extraction rate of nucleosides from rape bee pollen was (705.2 ±0.006) mg/100 g.
Optimization of Ultra High Pressure Sterilization Conditions for Fish Sausage
LU Hai-xia, HANG Yu-yu, LI Jian-rong,
2012, 33(12):  89-92.  doi:10.7506/spkx1002-6630-201212017
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The effects of pressure, dwell time and temperature on microbial survival in fish sausage after ultra high pressure (UHP) sterilization were studied, and the sterilization conditions were optimized using orthogonal array design. Pressure was the most important affecting factor, followed by temperature; dwell time had the weakest effect. The optimal sterilization conditions were treatment pressure of 400 MPa, pressure-holding time of 5 min and treatment temperature of 30 ℃. Total bacterial count in fish sausage was reduced by 97.25% after UHP sterilization under these conditions, and 100% E. coli, mold and yeast were killed. No pathogenic bacteria were detected before and after UHP sterilization.
Optimization of Lubricant Typye and Amount in Seaweed Polysaccharide-Inulin Effervescent Tablets by Response Surface Methodology
PU Yang,FENG Da-wei,BAO Huan-ling,QIN Song,YI Yue-tao
2012, 33(12):  93-96.  doi:10.7506/spkx1002-6630-201212018
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Effervescent tablets were prepared from organic selenium-enriched seaweed polysaccharides and inulin by absolute alcohol-acid-base two-phase granulation method. Using response surface methodology based on a three-variable, three-level central composite design, the amounts of the added lubricants sodium dodecylsulfate, magnesium stearate, and silica powder in effervescent tablet formulation were optimized to be 0.70%, 2.60% and 0.90%, respectivley. All the quality indexes fhe prepared effervescent tablets complied with the requirements of the Chinese Pharmacopoeia.
High-Speed Shear Treatment for Cell Wall Disruption of Rape Bee Pollen
LI Li,LIU Ye-wei,ZHAO Jian-xi,PEI Dong,DI Duo-long,WANG Na
2012, 33(12):  97-101.  doi:10.7506/spkx1002-6630-201212019
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A high-speed shear dispersing emulsifier (HSDE) was used to treat rape bee pollen for cell wall disruption. The effects of treatment time, temperature, HSDE speed and ratio of raw material to liquid on disruption rate in aqueous medium were investigated. A predictive polynomial quadratic model was set up by means of central composite design and used to optimize these treatment conditions by response surface methodology. A scanning electron microscope (SEM) was used to characterize pollen morphology, and total flavonoids content was determined by colorimetric method to further explain the effectiveness of HSDE treatment in cell wall disruption. The optimal HSDE treatment conditions were determined as 3 min of treatment time, 22000 r/min of HSDE rotary speed, and 1:3 of material-to-liquid ratio (mL/g), resulting in a disruption rate exceeding 99% and a flavonoid yield of 3.60 mg/g. In conclusion, HSDE treatment is a good pretreatment strategy that can provide a high disruption rate in a short time.
Optimization of Supercritical CO2 Extraction of Tea Flowers by Response Surface Methodology and Chemical Composition Analysis of Tea Flower Extract
YU Rui,WANG Juan,HUANG Hui-hua
2012, 33(12):  102-107.  doi:10.7506/spkx1002-6630-201212020
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This paper reports the optimization of supercritical CO2 extraction of tea flowers by response surface methodology and the chemical composition of tea flower extract. The effects of extraction pressure, temperature, extraction time and entrainer (95% ethanol) amount on extraction efficiency were investigated. The operating parameters were optimized using response surface methodology based on the established regression model for extraction efficiency as a function of them. The highest extraction efficiency was obtained under the conditions: extraction pressure 35 MPa, temperature 48 ℃ and entrainer amount 43%, with theoretical and actual values of 2.882% and (2.785± 0.068)%, respectively. GC-MS analysis showed that 67 components were separated from the extract obtained. Of them, 49 were identified, which accounted for 78.11% of the total extract. The main components were n-hexadecanoic acid (17.81%), acetophenone (2.19%), and alpha-methyl-benzenemethanol (2.76%).
Ultrasonic-Assisted Extraction and Antibacterial Activity of Total Flavonoids from Whole Plants of Saxifraga tangutica Engl.
CUI Wei,LI Yu-lan,YANG Ai-mei
2012, 33(12):  108-113.  doi:10.7506/spkx1002-6630-201212021
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Objective: To investigate the extraction and antioxidant activity of total flavonoids from whole plants of Saxifraga tangutica Engl. Methods: Orthogonal array design was employed to optimize extraction conditions. The antibacterial effect of total flavonoid extract at different concentrations on 6 strains was evaluated by agar diffusion and broth dilution methods. Results: According to the results of analysis of variance, four extraction parameters could be ranked in decreasing order of their effect on extraction efficiency as follows: extraction number > ethanol concentration > ultrasonic treatment time > material-to-liquid ratio. The optimal extraction conditions were ethanol concentration of 80%, material-to-liquid ratio of 1:25 (g:mL), ultrasonic treatment time of 35 min, repeated ultrasonic treatment number of 4, ultrasonic power of 100 W and extraction temperature of 50 ℃. Under these conditions, the extraction efficiency of total flavonoids was 81.73 mg/g. Total flavonoids from whole plants of Saxifraga tangutica Engl. had inhibitory effect on all tested strains. The minimum inhibitory concentrations were 0.156, 0.313 mg/mL and 0.625 mg/mL against Staphyloccus aureus, Bacillus subtilis and Escherichia coli, respectively. The anti-yeast activity was weak. No inhibitory effect on mold was found. Conclusion: This study can provide experimental references for further development and utilization of Saxifraga tangutica Engl.
Spray Drying and Formulation Optimization of Herbal Coffee Powder
GE Yan,GUO Shuang-shuang,CHEN An-jun,PU Biao,CAO Lin
2012, 33(12):  114-118.  doi:10.7506/spkx1002-6630-201212022
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This study aimed to find the best conditions for the extraction, spray drying and formulation of herbal coffee powder. Third repeated extraction at a material/liquid ratio of 1:15 (g/L) for 20 min each time provided a high powder yield. High-quality herbal coffee powder was obtained through spray drying at an inlet temperature of 140 ℃, a feed flow rate of 350 mL/h, and a fan frequency of 55 Hz. The optimal amounts of maltodextrin, β-cyclodextrin, arboxymethylcellulose and arabic gum added to herbal coffee powder, as optimized by one-factor-at-a-time and orthogonal array design methods, were 30%, 4.5%, 0.12% and 1.5%, respectively.
Optimization of Synthesis of Sodium Copper Chlorophyllin by Alkaline Cuprammonium Replacement
YU Wei,JI Ping-xiong
2012, 33(12):  119-122.  doi:10.7506/spkx1002-6630-201212023
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Chlorophyll copper sodium salt as a non-toxic water soluble chlorophyll derivative has excellent stability and colorability and is widely used as a food additive. In the present study, the traditional preparation process for sodium copper chlorophyllin from silkworm excrement chlorophyll was modified to develop a semi-synthesis method based on alkaline cuprammonium replacement. Four reaction conditions such as ethanol concentration, pH, reaction temperature and copper amount were chosen for synthesis process optimization based on orthogonal array design using SAS statistical software. The optimal copper amount, ethanol concentration, reaction temperature and pH were 2.5 times higher than the theoretic value, 75%, 55 ℃, and 11.5, respectively. Under these conditions, the ethanol consumption for copper replacement was reduced by 10%, and the quality of the product obtained was in accordance with the national standard of food additives.
Optimization of Ultrasonic-Assisted Extraction of Alkaloids from Whole Herbs of Urtica angustifolia Using Response Surface Methodology
ZHANG Hai-yue,LI Qian
2012, 33(12):  123-127.  doi:10.7506/spkx1002-6630-201212024
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Response surface methodology was used to optimize the ultrasonic-assisted extraction of alkaloids from whole herbs of Urtica angustifolia. The maximum absorption wavelength of alkaloids was determined by acid dye colorimetry. The optimal extraction conditions were ultrasonic extraction time of 10 min, material/liquid ratio of 1:10 (g/mL), ethanol concentration of 85%, and extraction time of 2 h.
Lipase-Catalyzed Hydrolysis of Linseed Oil
LIN Fei-fan,TAN Zhu-jun
2012, 33(12):  128-131.  doi:10.7506/spkx1002-6630-201212025
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To maximize the degree of lipase-catalyzed hydrolysis of linseed oil, the reaction conditions pH, time, emulsifier amount, enzyme amount and oil-to-water ratio were investigated. A predictive model was established through data fitting with the mathematical software Matlab. A degree of hydrolysis of 62.6% was achieved after 29 h of hydrolysis at pH 5.9, 33 ℃, an oil-to-water ratio of 1:2 (V/V), and an enzyme amount of 13600 U/g.
Optimization of Crispness Preservation Process for Hami Melon Using Response Surface Methodology
JING Si-qun
2012, 33(12):  132-137.  doi:10.7506/spkx1002-6630-201212026
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The preparation of baby Hami melon chili sauce involves material selection, blanching, crushing, frying and seasoning. In this study, the crispness preservation as a key process control point was optimized using response surface methodology based on a three-variable, three-level central composite design. A crispness value of 15.449 mJ was obtained under the optimized conditions: 33% of water content in Hami melon, 0.19 g/100 mL of CaCl2 concentration, 17 min of soaking time. Meanwhile, the optimal sterilization condition was determined to be 1400 W and 2 min.
Extraction and Composition Analysis of Crude Polysaccharide from Young Stems of Oenanthe javanica
ZHOU Yi-feng,TANG Qiao-yu,PENG Hong,WU Lin-zhong
2012, 33(12):  138-142.  doi:10.7506/spkx1002-6630-201212027
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In this study, one-factor-at-a-time and orthogonal array design methods were employed to optimize the hot water bath extraction of crude polysaccharide from young stems of Oenanthe javanica. Crude polysaccharide was deprotenized by Sevag method and sequentianlly precipitated with 1,3-fold and 6-fold volumes of absolute ethanol. All precipited fractions were anlyzed by GC-MS for monosaccharide composition and by atomic absorption spectrometry for partial element composition. The optimal conditons for crude polysaccharide extraction conditions were determined as 100 ℃ of temperature, 1:40 of material-to-liquid ratio (g/mL), and 3 h of extraction time. Under these conditons, the extraction yield of crude polysaccharide was 16.89%. Crude polysaccharide from young stems of Oenanthe javanica consisted of five hexoses such as D-glucose, rhamnose, idose, D-mannose, D-galactose and 7 hexose derivatives such as 1-methyl-α-rhamnoside, methyl-β-D-arab pyran glucoside, methyl-α-1-tallo glucoside, methyl glucoside, α-D-methyl-mannosidase, 1-methyl-α- rham- noside and glycuronic acid. The chactercteristic elements were Zn and Mn. The Zn and Se contents of the precipitate obtained with 1-fold vlome of absolute ethanol were 650.625 μg/g and 4.483 μg/g, respectivley. The Mn content of the precipitate obtaiend with 6-fold volume of absolute ethanol was 725.875 μg/g. In conclusion, crude polysaccharide from young stems of Oenanthe javanica can be developed as Zn and Se supplements.
Analysis & Detection
Fluorescence Enhancement Mechanism of Aflatoxin G1 by β-Cyclodextrin and Its Derivatives
MA Liang,ZHANG Min,ZHANG Yu-hao,HU Yuan-yuan,ZHOU Yao
2012, 33(12):  143-148.  doi:10.7506/spkx1002-6630-201212028
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The fluorescence response signals of supramolecular inclusion complexes of AFG1 with β-cyclodextrin or its derivatives were studied. The fluorescence response signal of AFG1-HE-β-CD reaction system was significantly enhanced compared with AFG1, which reached maximum level after 3 min reation in 2% methanol solution HE-β-CD at the HE-β-CD cocnentration of 0.05 mol/L. According to the Benesi-Hidebrand equation, an inclusion complex was formed from AFG1 and HE-β-CD at a ratio of 1:1. UV spectroscopic, infrared spectroscopic and thermodynamic analyses and KI quenching experiments showed that AFG1 entered the cavity of HE-β-CD so that its fluorescence intensity was protected. An excellent linear relationship with fluorescence intensity was observed in the AFG1 concentration of 2-40 μg/kg (r = 0.9998). The detection limit was 0.079 μg/L. Therefore, the application of HE-β-CD can permit the accurate and precise analysis of AFG1 in peanut samples.
Solid Phase Microextraction and GC-MS Analysis of the Effect of Cumin Powder on Volatile Compounds in Low Sugar Cookies with Stevioside
ZHONG Jing,WU Chao,ABDEL-SAMIE Mohamed ABDEL-SHAFI,WANG Feng,HUANG Wei-ning,ZHENG Jian-xian
2012, 33(12):  149-153.  doi:10.7506/spkx1002-6630-201212029
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In order to explore the effect of cumin power on volatile flavor compounds in low sugar cookies with stevioside, solid phase micro-extraction and gas chromatography-mass spectrometry were used to characterize the categories and contents of volatile flavor compounds in different cookie food systems, including normal cookies (control), low sugar cookies with 45% (m/m) sugar replaced by stevioside (S) and low sugar cookies with 10% (m/m) cumin powder (S+C). A total of 97 components were identified, and 16 of them were detected in all three samples, while 34 components were detected in low sugar cookies with stevioside (S) but not in the control. Meanwhile, only 25 components were observed in S+C. Aldehydes, ketones and esters were the major volatile compounds in the control samples, and heterocyclic compounds were significantly increased in S cookie samples with the addition of stevioside. The addition of cumin powder resulted in an obvious increase in the contents of aldehydes and alkenes in low-sugar cookies, which reached 48% and 26.51% (accounting for the total flavor compounds), respectively. The main aldehydes were cuminaldehyde (27.45%), 2-caren-10-al (15.01%) and phellandral (3.08%), and the main alkenes were α-pinene (8.08%), γ-terpinene (8.07%), limonene (1.91%) and β-myrcene (1.67%).
Feasibility Study of Identifying Melamine-Formaldehyde Resin in Cow Feed by Near Infrared Spectroscopy
LIU Xing,SHAN Yang,,ZHANG Xin,YANG Gui-sen
2012, 33(12):  154-158.  doi:10.7506/spkx1002-6630-201212030
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Thirty-three samples of typical cow feed concentrate supplement without melamine-formaldehyde resin (MFR) and 99 ones adulterated with different concentrations of MFR were subjected to full wavelength near-infrared transmission and reflectance spectroscopic scanning. A discrimination model was established by BP (back propagation) neural network or PLS-LDA (partial least squares-linear discriminant analysis). The BP neural network model showed 100% accurate prediction. The minimum cross validation error rate of the PLS-LDA model was 0.0778, misclassification rate 0.0667, and prediction error rate 0.1429. Therefore, it is feasible to establish a predictive model for detecting MFR adulteration in cow feed by means of near-infrared transmission and reflectance spectroscopy.
Multiplex PCR Detection of Transgenic Components of Genetically Modified Rice
WEI Shuang,CHEN Zhen,LU Chun-bin,MA Jun,BAI Wei-bin,WU Xi-yang
2012, 33(12):  159-162.  doi:10.7506/spkx1002-6630-201212031
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In order to detect transgenic components in genetically modified rice, endogenous gene sps, exogenous insect resistant gene Cry1Ab/Ac, exogenous insect resistant gene Cry1Ab, exogenous insect resistant gene Btc, reporter gene gus, nos terminator and CaMV35S promoter were evaluated by multiplex polymerase chain reaction. Seven pairs of primers were designed, and primer concentration and annealing temperature were optimized to establish a multiplex PCR system. The results showed that the developed seven-plex PCR system could allow the detection of transgenic components in genetically modified rice and other crops including soybean, corn, cottonseeds and rapeseed meal with high efficiency and good stability.
Determination of 30 Fatty Acids in Scallop by Ultrasonic Extraction Gas Chromatography
PENG Quan-cai,SONG Jin-ming,LI Jun,YU Ying
2012, 33(12):  163-168.  doi:10.7506/spkx1002-6630-201212032
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An analytical method for the simultaneous determination of 30 fatty acids (including saturated and unsaturated fatty acids) in scallop was developed. Samples were lyophilized, extracted under ultrasonic assistance, and methyl esterified with sulfuric acid and methanol before GC analysis. The fatty acids in scallop were quantified by internal standard method. The optimal conditions for fatty acid extraction from scallop samples, as determined using orthogonal array design, were a mixture of methanol and dichloromethane (1:3, V/V) as the extraction solvent at a material-to-liquid ratio of 1:140 (mg/mL) and three replicate extractions for 15 min each time. Both extraction number and material-to-liquid ratio had a significant effect on fatty acid extraction (P< 0.05). A good linear relationship was found for all 30 fatty acids in the concentration range of 5.0-80.0 μg/mL with a correlation coefficient exceeding 0.999. The average recovery rates of 30 fatty acids at low and high spike levels were 1.3%-3.5% and 0.9%-3.1%, respectively (n = 5). The detection limits of the method varied in the range of 1.94-2.57 mg/kg (RSN = 3). This method was simple, rapid, sensitive and accurate and could meet the requirements for the determination of fatty acids in scallop and similar organisms.
Comparative Analysis of Flavor Components in Pork from Different Breeds by SPME with Different Fiber Coatings and GC-MS
PAN Jian,YANG Jun-jie,ZOU Ying-zi
2012, 33(12):  169-172.  doi:10.7506/spkx1002-6630-201212033
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The flavor components of cooked tenderloin from Dingyuan Black pig and lean-type pig were comparatively analyzed by SPME with different fiber coatings and gas chromatography-mass spectrometry (GC-MS). The results indicated that a significant difference in six aldehydes, three alcohols, four ketones and six carboxylic acids was observed between both breeds of pork. The contents of aldehydes, alcohols and ketones in Dingyuan black pig tenderloin were higher than those in lean-type pig tenderloin. Meanwhile, these compounds had very low threshold value so that they offered more contributions to the flavor difference between the two breeds of pork. The contents of six aldehydes in lean-type pig tenderloin were low, but relatively higher compared to Dingyuan Black pig tenderloin, and they had little effect on the flavor difference due to their high threshold values. Therefore, the differences in the contents of aldehydes, alcohols and ketones are the major causes of the flavor difference between the two breeds of pork.
Analysis of Lovastatin-Producing Ability of Fungi in Pu-erh Tea
ZHAO Zhen-jun,TONG Hua-rong,ZHOU Li,LIU Qin-jin
2012, 33(12):  173-176.  doi:10.7506/spkx1002-6630-201212034
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The pure strains of Aspergillus, Penicillium and Trichoderma isolated from Pu-erh tea were cultured individually to analyze their ability to produce lovastatin by HPLC. The results showed that only one strain of A. tubingensis, one strain of A. wenti and one strain of A. fumigatus among the genera of Aspergillus had the ability to synthesize lovastatin with the content of 9.59, 2.33 ng/g and 2.77 ng/g, respectively, after culture in the Czapek Yeast Agar (CYA) medium. On the CYA medium, only P. chrysogenum revealed the ability to secrete lovastatin with the content of 3.36 ng/g. Two strains of Trichoderma (T. asperellum and T. citrinoviride) from Pu-erh tea samples had the ability to produce lovastatin with the content of 4.8 ng/g and 1.47 ng/g on the CYA medium, respectively.
Analysis of Volatile Flavor Compounds from Enteromorpha intestinalis
SONG Shao-hua,QIU Di-hong
2012, 33(12):  177-180.  doi:10.7506/spkx1002-6630-201212035
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Headspace solid phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometer (GC-MS) was used to determine the volatile flavor compounds of the green macroalga Enteromorpha intestinalis. A comparative sensory evaluation of the main flavor substances was also done. The results showed that the main characteristic volatile flavor compound of Enteromorpha intestinalis were (Z)-3-heptadecene, with a content as high as 59.43% in fresh samples. The other volatile flavors were hexadecanal, (E,E)-2,4-heptadienal, beta-ionone, nonanal, (E)-2-hexenal, 2,4 - pentadienal, (E,E)-2,4-decadienal, and so on.
Determination of Eight Water-Soluble Vitamins in Fruit Vinegar by RP-HPLC
SONG Ping-ping,CAO Jiang-ping,LIU Shu-hui,
2012, 33(12):  181-184.  doi:10.7506/spkx1002-6630-201212036
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A RP-HPLC gradient elution method was developed for the simultaneous determination of eight water-soluble vitamins, including ascorbic acid, thiamine, riboflavin, nicotinic acid, pyridoxine, cyanocobalamin, folic acid and nicotinamide in fruit vinegar. The effects of temperature, buffer solution concentration, pH value and gradient elution procedure on chromatographic separation were studied. The mobile phase was a mixture of 0.1 mol/L sodium acetate solution (pH 4.25) and methanol at a flow rate of 1.00 mL/min. The column temperature was set as 30 ℃. Baseline separation was achieved for 8 water-soluble vitamins within 14.2 min. The detection was carried out at 266 nm and 280 nm. The method offered excellent linearity over a range of 0.05-12.5 μg/mL for riboflavin and folic acid, 0.1-25 μg/mL for ascorbic acid, thiamine, nicotinic acid and nicotinamide, 0.15-37.5 μg/mL for pyridoxine and cyanocobalamin, with correlation coefficients (r>0.999). The detection limits were in the range of 0.47-3.46 ng/mL This method has been successfully applied to assay vitamins in fruit vinegar. The average spike recovery varied from 92.4% to 105.2% with RSD in the range of 0.08%-1.54% (n =3).
Analysis of Aroma Components of Xinyang Maojian Tea by SPME-GC-MS
KONG Wei-ting,LIU Jian-jun,SI Hui-qing
2012, 33(12):  185-189.  doi:10.7506/spkx1002-6630-201212037
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Solid-phase microextraction (SPME) time and temperature were investigated for the analysis of aroma components in Xinyang Maojian tea by GC-MS. The optimal SPME extraction time and temperature were 50 min and 70 ℃, respectively. A total of 99 aroma components were identified including 32 alcohols (47.83%), 20 hydrocarbons (10.97%), 15 ketones (20.43%), 11 esters (7.24%), 8 phenols (3.4%), 7 aldehydes (7.73%), 3 mixed oxide compounds (1.01%), and 3 nitrogen-containing compounds (1.39%). The characteristic aroma components of Xinyang maojian were linalool, nerol, 6-methyl-5-heptene-2-ketone, amyl alcohol, β-ionone, toluene, 5,6-epoxy-β-ionone, phenethyl alcohol, Z-jasmone, heptaldehyde, 2,2,6 - trimethyl cyclohexanone, benzyl alcohol, 2-ethylhexyl alcohol, nerolidol, and so on.
Rapid Simultaneous Determination of Eight Quinolone Residues in Eel by Syncore Analyst-Ultra Performance Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry
ZHANG Xian-chen,HUA Hong-bo,ZHANG Peng-jie,WANG Yong,YANG Fang,LI Rong,HU Yi-guang, LU Jun-wen
2012, 33(12):  190-195.  doi:10.7506/spkx1002-6630-201212038
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A method for the simultaneous determination of eight quinolone residues in eel was developed by syncore analyst-ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry (SA-UPLC-MS/MS). Deuterium substituted reagents were added as internal standards before sample extraction with acidified acetonitrile, followed by concentration using a Syncore Analyst and clean-up with hexane. Eight quinolone residues were analyzed by UPLC-MS/MS under positive ion mode. The limit of detection of the method for eight quinolones was 0.5μg/kg, and the limit of quantification was 1.0μg/kg. The calibration curves showed good linearity over the concentration range of 2.5-200 ng/mL (r > 0.99). The average recovery rates were 81.4%-11.1% across three spike levels (n = 6). This method was simple, rapid, stable, reliable, sensitive and suitable for the determination of bulk aquatic products.
Rapid Determination of Crude Protein in Vigna minima Seeds by Microwave Programmed Digestion-Conductivity Micro-titration
GAO Xiang-yang,WANG Hui-rong,REN Ting-ting
2012, 33(12):  196-199.  doi:10.7506/spkx1002-6630-201212039
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A new analytical method to rapidly determine protein content in Vigna minima seeds was established in the present study. Samples were digested with a sulfuric acid-hydrogen peroxide solution by microwave programmed digestion to convert crude protein to NH4+. The NH4+ generated in the solution were further converted to H+ ions for conductivity micro-titration with standard NaOH solution. The results showed that the average content of protein in wild Vigna minima seeds from Zhengzhou was determined to be 23.41% with relative standard deviation (RSD) of 1.5% (n = 5). Compared with the classic standard determination method, the conductivity micro-titration did not exhibit significant difference as analyzed by F-test and t-test at 95% confidence level. This method has the advantages of convenient operation, high sensitivity, quick determination, accurate results and no requirements for indicators.
Identification of Unknown Pigment in Inferior Black Sesame Paste
DING Hua,DONG Li-na,CHEN Jian-biao,YANG Jie,XIA Hong,PENG Mao-min,WANG Qing-qing,HU Ding-jin,ZHOU You-xiang
2012, 33(12):  200-204.  doi:10.7506/spkx1002-6630-201212040
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An unknown blue pigment was extracted from an inferior black sesame paste on the market. The maximum absorption wavelength of the pigment was determined by UV-visible spectroscopy. It was analyzed qualitatively by HPLC-MS and analyzed quantitatively by HPLC. The pigment had a high solubility in methanol. It could be effectively separated on Inertsil ODS-3 column using a mobile phase composed of 20 mmol/L ammonium acetate solution and acetonitrile (V/V = 70:30). It was identified as brilliant blue through ion-trap MS analysis. The results of quantitative analysis by HPLC with diode-array detection indicated that the content of brilliant blue in the inferior black sesame paste was 1.73 mg/kg.
Determination of Aroma Components in Distilled Fermented Apple Pomace Wine by Head Space Solid Phase Microextraction (HS-SPME) and GC-MS
WANG Yang,WANG Jie,LIU Ya-qiong,LIU Zheng,FAN Jing-fang
2012, 33(12):  205-209.  doi:10.7506/spkx1002-6630-201212041
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The volatile aroma components of distilled fermented apple pomace wine and distilled alcohol-immersed apple pomace wine were analyzed by HS-SPME and GC-MS. A total of 57 volatile compounds were found in distilled wine fermented from apple pomace, including 30 esters, 5 carboxylic acids, 6 alcohols, 1 ketone, 14 hydrocarbons and 1 unknown compound, of which the relative contents were 50.604%, 6.322%, 22.207%, 0.254%, 20.542% and 0.013%, respectively; 37 volatile compounds were found in distilled alcohol-immersed apple pomace wine, including 22 esters, 3 carboxylic acids, 2 alcohols, 9 hydrocarbons and 1 unknown compounds, of which the relative contents were 64.272%, 2.538%, 14.885%, 17.437% and 0.911%, respectively. These results show that distilled wine fermented from apple pomace contains much more volatile compounds compared to distilled alcohol-immersed apple pomace wine. Moreover, it was found that the former presented a more even distribution of volatile compounds, a more mellow and natural taste, and a better sense of hierarchy. The nutrients and unique aroma of apple pomace were retained in the fermented wine. This study demonstrates that fermentation of apple pomace to produce distilled wine is a better approach for comprehensive utilization of apple pomace.
Determination of Pefloxacin Residue in Urine and Serum by Flow Injection Chemiluminescence
REN Nai-lin,LI Hong
2012, 33(12):  215-218.  doi:10.7506/spkx1002-6630-201212043
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An analytical method to determine pefloxacin (PEFX) residue in urine and serum was established based on the fact that the presence of Tb3+ enhances the luminous intensity of Ce(Ⅳ)-SO32-- PEFX system. There was a good linear relationship between the luminous intensity of the system and PEFX concentration over the range of 2 × 10-9-6 × 10-7 g/mL. The limit of detection for PEFX was 8.8 × 10-10 g/mL. The relative standard deviation for 11 parallel determination of PEFX at 1 × 10-7 g/mL was 3.1%. The average spike recoveries of PEFX from human urine and duck serum ranged from 98.5% to 102.5%.
Simultaneous Determination of Bromate, Chlorite, Chlorate and Common Inorganic Anions in Drinking Water by Ion Chromatography
YANG Min,XIE Jing,YANG Shu-ke,CHEN Hai-yun,WANG Hong-bin
2012, 33(12):  219-222.  doi:10.7506/spkx1002-6630-201212044
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An analytical method for the simultaneous determination of bromate, chlorite, chlorate and common inorganic anions in drinking water was developed using large-volume direct injection and chemically suppressed ion chromatography (IC). An IonPac AS9-HC separation column and an IonPac AG9-HC protection column were used. The mobile phase was 12 mmol/L Na2CO3 at a flow rate of 1.0 mL/min. The injection volume was 100μL. Ten anions could be detected by the method within 18 min with average spike recovery of 93.0%~103.1% (n = 5). The correlation coefficients of calibration curve were 0.9993~0.9999. This method was sensitive, accurate and rapid. It has been applied to determine Kunming tap water and a variety of commercial drinking water with satisfying results.
Analysis of Aroma Constituents in Gardenia jasminoides at Different Flowering Stages
TAN Yi-tan,XUE Shan,TANG Hui-zhou
2012, 33(12):  223-227.  doi:10.7506/spkx1002-6630-201212045
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In order to under the aroma composition and release regularity of Gardenia jasminoides during the flowering period, the aroma-active components of Gardenia jasminoides at the early, full and late flowering stages were determined by solid phase microextraction (SPME) and gas chromatograph-mass spectrophotometry (GC-MS). A total of 36 aroma-active components were detected throughout the whole flowering stages, which were mainly esters, terpenoids and hydrocarbons and together accounted for 85.25%, 85.29% and 94.37% of total volatile compounds at the early, full and late flowering stages, respectively. The relative contents of esters and hydrocarbons were low at the early flowering stage and then increased as the flowering period proceeded; however, the relative content of terpenoids showed a trend of decreasing initially and then increasing. The main compounds responsible for the aroma of Gardenia jasminoides flowers were ocimene, α-farnesene, benzoic acid methyl ester, isopropyl cyclohexane and 3,7-dimethyl 1,6-octadiene-3-alcohol propionate.
Amino Acid Compositions of Silkworm Pupa Protein and Its Hydrolysates
LU..Wen-jun,ZHAO Zhong-xing,LIAO Dan-kui,SUN Jian-hua,HUANG Ke-lin,SUN Guo-song,WU Zhi-hong,TONG Zhang-fa
2012, 33(12):  228-232.  doi:10.7506/spkx1002-6630-201212046
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The amino acid compositions of silkworm pupa protein and its hydrolysates prepared with neutral protease were determined by reversed-phase high performance liquid chromatography (RP-HPLC) with precolumn derivatization. Meanwhile, their ACE inhibitory activity was also tested. The results indicated that the content of hydrophobic amino acids in the hydrolysate ultrafiltration fraction SN2 (< 10 kD) was 49.15% compared to 40.55% for the hydrolysate ultrafiltration fraction SN1 (>10 kD) and 45.21% for silkworm pupa protein. The contents of proline and aromatic amino acids (Trp, Phe and Tyr), which had great effect on ACE inhibitory activity, were 7.42% and 15.81%, respectively. Moreover, the ACE inhibitory rate of SN2 was 47.6%, which was remarkably higher than that of SN1 and silkworm pupa protein, suggesting that the change trends of hydrophobic amino acid composition and ACE inhibitory activity are the same and that the ACE inhibitory activity is mostly concentrated on SN2.
Determination of Total and Individual Phenolics in Potato Flesh and Skin from Different Growing Areas
CAI Li-chuang,LUO Cheng-yao,LUO Xiao-yan,RUAN Zheng,WEN Hong-yan
2012, 33(12):  233-237.  doi:10.7506/spkx1002-6630-201212047
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The contents of total and individual phenolics in potato flesh and skin from different growing areas in Xinjiang, Jiangxi, Fujian and Beijing were comparatively determined by both HPLC and Folin-Ciocalteu colorimetry. The gradient elution of phenolics was carried out on YMC-C18 column (250 mm × 4.6 mm, 5 μm) using methanol (mobile phase A) and .5% phosphoric acid (mobile phase B). Baseline separation was observed for chlorogenic acid, caffeic acid, p-coumaric acid, ferulic acid and rutin. All of them showed good linear relationship over a wide concentration range. The average spike recoveries for them from a known sample were 91.36%-102.23% (n = 3). The total phenolic contents in all samples under investigation were 0.238-1.190 mg/g. Chlorogenic acid accounted for 80.59%-89.06% of the total phenolics in potato flesh compared to 65.54%-80.00% in potato skin. The HPLC method was quick, accurate, reliable and repeatable. The Folin-Ciocalteu colorimetry method was more suitable for the determination of total phenolics in potato.
Analysis of Aroma-Active Compounds in Canned Stewed Beef
XU Qian-qian,LIN Mei-li,LIU Xue-ni,SONG Huan-lu,CHEN Bin,QU Wei-li
2012, 33(12):  238-241.  doi:10.7506/spkx1002-6630-201212048
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The aroma-active compounds of canned stewed beef braised in brown sauce were qualitatively and quantitatively analyzed by dynamic headspace sampling, thermal desorption injection and GC-O/GC-MS. A total of 73 volatile compounds were identified. Among them were 23 aroma-active compounds, mainly consisting of 4 ketones, 3 aldehydes, 2 alcohols, 2 esters, 2 furans, 2 pyrazine, 2 thiazole, 2 terpenes, 1 alkene, and 1 pyridine. The important aroma-active compounds were 2-butanone (fruity) , 2-pentanone (fruity and sweet) , camphene (woody and minty) , ethyl butyrate (sweet and fruity), pyridine(soul and fishy), 2,5-dimethyl-pyrazine(nut and roast), benzaldehyde (sweet and fruity), and 2-acetylthiazole (nut and roast peanut).
Analysis of Aroma-active Components in Purple Potato Wine during Fermentation
YANG Ya-li,SHEN Hai-liang,KAN Jian-quan
2012, 33(12):  242-246.  doi:10.7506/spkx1002-6630-201212049
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The aroma-active components of purple potato wine were extracted by solid-phase microextraction (SPME) and identified by gas chromatography-mass spectrometry (GC-MS) and computer retrieval. Moreover, the changes of alcohol degree, anthocyanins, chromatic aberration, pH, soluble solid content were tracked during the whole fermentation of purple potato wine. Fifty-seven aroma-active components were identified from purple potato wine, accounting for 97.13% of the total peak area. The major aroma-active compounds were isobutanol, isoamylol, octylic acid ethyl ester, and phenyl ethanol. Alcohol degree and volatile acid content exhibited a gradually increasing trend, while anthocyanins, soluble solid content and chromatic aberration tended to gradually decrease. Little change in pH was observed during the entire fermentation process.
Determination of Iodine in Eggs by Indirect Atomic Absorption Spectrometry
CHEN Li-juan,FENG Ling,LUO Di,LIU Sha,YAO Cheng-wei,HUANG Bao-mei
2012, 33(12):  247-249.  doi:10.7506/spkx1002-6630-201212050
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A new method to determine iodine in eggs by indirect atomic absorption spectrometry (AAS) was established. Based on the reduction of Cu2+ by ascorbic acid to Cu+ for precipitation between Cu+ and I-, Cu residue in the supernatant was determined and calculated to obtain iodine content in eggs. The reaction was carried out using 0.8 mL of 1000 μg/mL ascorbic acid solution in pH 4.0 potassium hydrogen phthalate buffer at 30 ℃, and the centrifugation time was 10 min. This method was simple and rapid and had a wide linear range. The detection limit was 1.0 μg/mL. Satisfying results were obtained in the determination of iodine in actual samples by this method.
Analysis of Fatty Acids in Chinese Star Anise (Illicium verum Hook.f.) by GC-MS
ZHAO Li-juan
2012, 33(12):  250-253.  doi:10.7506/spkx1002-6630-201212051
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The fatty acids in Illicium verum Hook.f. grown in Zhumadian and Yulin were extracted by ultrasonic-assisted extraction or Soxhlet extraction, methyl esterificated and then analyzed by GC-MS. The extraction yields of fatty acids from Chinese star anise grown in Zhumadian and Yulin were 26.65% and 34.30% by ultrasonic-assisted extraction and 15.45% and 20.55% by Soxhlet extraction, respectively. The fatty acid composition of Chinese star anise varied little with geographic area and extraction method. The dominant fatty acids were hexadecanoic acid, heptadecanoic acid, octadecanoic acid, linoleic acid and oleic acid.
Headspace Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometric Analysis of Volatile Composition Changes of Steamed Bread during Processing
YAN Wen,ZHANG Zheng-mao,LIU La-ping
2012, 33(12):  254-258.  doi:10.7506/spkx1002-6630-201212052
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To study the volatile composition changes of steamed bread during processing, the volatile components in wheat flours, fermented doughs and steamed breads from three representative wheat cultivars with different gluten strength, Pubing 143, Jinmai 47 and Xinong 9817, were extracted by headspace solid-phase microextraction (HSPME) and analyzed by GC-MS. A total 23 volatile compounds (mainly naphthalene, 1-methyl-naphthalene, (Z)-2-Butenedioic acid dimethyl ester, 1,7-dimethyl-naphthalene and 2-methyl-naphthalene) were found to be common to wheat flours from all investigated cultivars, accounting for 84.01%, 77.82% and 82.28% of the total volatile compounds in Pubing 143, Jinmai 47 and Xinong 9817, respectively. Eighteen volatile compounds (mainly ethanol, naphthalene, 1-methyl-naphthalene, butanedioic acid ethyl methyl ester and phenylethyl alcohol) were common to fermented doughs made with wheat flours from all investigated cultivars, accounting for 80.99%, 71.65% and 70.44% of the total volatile compounds in Pubing 143, Jinmai 47 and Xinong 9817, respectively. Twenty-six volatile compounds (mainly naphthalene, 1-methyl-naphthalene, 2-pentyl-furan, ethanol and nonanal) were common to steamed breads made with wheat flours from all investigated cultivars, accounting for 80.26%, 75.99% and 80.43% of the total compounds in Pubing 143, Jinmai 47 and Xinong 9817, respectively. The results obtained demonstrate that wheat flour, fermented dough and steamed bread vary in volatile composition among wheat cultivars with different gluten strength despite no difference in most of the main volatile components. During the processing of steamed bread from wheat flour; the relative content of hydrocarbons significantly decreases, whereas both the kinds and relative contents of alcohols increase, suggesting a significant change in the volatile composition.
Fast Extraction of Fat and Fatty Acid Analysis of Hot Pepper Seeds
YU Cai-yun,WANG Shu-bin,LIU Jin-bing,PAN Bao-gui,DIAO Wei-ping,GE Wei
2012, 33(12):  259-263.  doi:10.7506/spkx1002-6630-201212053
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A method for fast fat extraction from hot pepper seeds was proposed based on ultrasonic-assisted Soxhlet extraction. The effects of seed particle size, ultrasonic power, ultrasonic treatment time, and extraction temperature on extraction rate were explored. Using one-factor-at-a-time and orthogonal array design methods, the optimal extraction conditions were determined to be particle size of 80 mesh, ultrasonic power of 70 W, ultrasonic treatment time of 30 min and extraction temperature of 25 ℃. The extraction rate of fat from 19 hot pepper varieties was in the range of 13.37%-28.81% with an average of 18.92% under the optimal extraction conditions. The main fatty acids in hot pepper seeds were linoleic acid, palmitic acid, oleic acid, stearic acid, linolenic acid, behenic acid, arachidic acid and myristic acid as determined by GC-MS analysis. Differences in fatty acid composition and content were observed among 19 hot pepper varieties.
Rapid Determination of Chlorine Ion in Pickles by Direct Reading Method
WANG Shan,WEI Jiang-mian,GAO Xiang-yang
2012, 33(12):  264-267.  doi:10.7506/spkx1002-6630-201212054
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A new analytical method was presented, allowing the rapid and simple determination of chlorine ion in pickles through direct reading. Pickle samples were pretreated by means of ultrasonic. The determination was performed using a chloride ion-selective electrode. The relative standard deviations (RSD) for five replicate determinations of chlorine ion using a total ionic strength adjustment buffer (TISAB) at pH 5.50 containing 0.20 g/L trisodium citrate and 0.80 mol/L potassium nitrate were 1.9%~2.9%. The spike recovery rates of chlorine ion from four types of pickle samples were 94.1%~105.6%. The limit of detection was 1.20 × 10-5 mol/L. There was no significant difference between this method and the national standard method as demonstrated by F test and t test analysis. This method was economic, simple, fast and suitable for rapid on-site determination of chlorine ion.
Analysis of Volatile Components in Yellowfin Tuna by Electronic Nose and GC-MS
WANG Xia,HUANG Jian,HOU Yun-dan,WANG Qiu-juan,CHEN Yi-fang,XIA Jing-bo,SU Xiu-rong
2012, 33(12):  268-272.  doi:10.7506/spkx1002-6630-201212055
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Purpose: To discover the effect of processing temperature on the volatile composition of yellowfin tuna. Methods: An electronic nose was used to detect raw and thermally processed (70, 80, 90, 100, 120 ℃ and 150 ℃) yellowfin tuna samples. The data obtained were analyzed by principal component analysis (PCA). Moreover, raw, 95 ℃ processed and 150 ℃ processed yellowfin tuna samples were analyzed by headspace solid-phase micro-extraction and GC-MS. Results: The electronic nose signals of different samples showed a strong cluster property. A total of 52, 50 and 53 volatile compounds were identified in aw, 95 ℃ processed and 150 ℃ processed yellowfin tuna samples, respectively. Among these compounds, the predominant ones were aldehydes, hydrocarbons, alcohols, kotones and furans, which synergistically contributed to the characteristic flavor of yellowfin tuna. Conclusions: Raw yellowfin tuna contains a large amount of the off-flavor compounds 1-penten-3-ol and 1,5-octadien-3-ol. Thermal processing can result in a significant decrease in their relative contents but a significant increase in the contents of the aroma-active compounds long-chain aldehydes and furans. 2-Ethyl-furan and 2-pentyl-furan are responsible for the characteristic aroma of roast yellowfin tuna.
Analysis of Total Mercury in Aquatic Vegetables Cultivated in Suzhou and Aquatic Products in Taihu Lake
FAN Li-li,FU Chun-ling,DING Wei-wei
2012, 33(12):  273-275.  doi:10.7506/spkx1002-6630-201212056
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Total mercury content in aquatic vegetables cultivated in Suzhou and aquatic products in Taihu Lake was determined by microwave digestion and cold atomic fluorescent spectrometry (AFS). The highest total mercury content was found in crab among six species of aquatic production from Taihu Lake, which was as high as 0.470 mg/kg in male crab paste. Total mercury content was relatively lower in other aquatic products such as white fish, white shrimp, Margarya, and so on. Except Zizania caduciflora, all other aquatic vegetables from Suzhou under investigation were polluted by mercury to different extent with a content exceeding the national standard limit. Total mercury content was higher in floating leaf vegetable than emerged vegetable, in naked vegetable than wrapped vegetable.
Shelf-Life Prediction and Pathogenic Bacterial Detection of Low-Sodium Salt Pork Sausages by Polymerase Chain Reaction
HUANG Mei-xiang,WANG Hai-bin,LI Rui,WANG Hong-xun,CONG Hao
2012, 33(12):  276-280.  doi:10.7506/spkx1002-6630-201212057
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The shelf-life of low-sodium pork sausages was predicted with accelerated shelf-life test model and pathogenic bacteria were detected by polymerase chain reaction (PCR) in this study. Meanwhile, the change trends of texture (tenderness) were also explored during storage. The results showed that the shelf-life of four kinds of pork sausages with the addition of 3% common iodine salt and 0.3% sodium tripolyphosphate (control group), the addition of 2.5% low-sodium salt and 0.35% TG, the addition of 2.0% low-sodium salt and 0.3% sodium tripolyphosphate, and the addition of 3% multi-component salt substitute (consisting of 40% NaCl, 35% KCl, 15% CaCl2, and 10% aminoacetic acid) and 0.35% TG were 17.5, 17.6, 16.9 days and 15.7 days at room temperature (25 ℃), and 189, 208, 142 days and 146 days at 4 ℃, respectively. No pathogenic bacteria were detected after 1 month of storage at 4 ℃. The tenderness of all groups exhibited an initial increase and final decrease during 90 days storage at 4 ℃. Moreover, pork sausages with the addition of 2.5% low-sodium salt and 0.35% TG had the best storage stability.
Packaging & Storage
Effect of 1-MCP and Its Structural Analogue on Hanfu Apple Quality during Storage at Ambient Temperature
WEI Bao-dong,LENG Jun-ying,CHENG Shun-chang,REN Xiao-lin,FENG Xu-qiao
2012, 33(12):  281-284.  doi:10.7506/spkx1002-6630-201212058
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In this study, the effects of 1-MCP and its structural analogues (1-PentCP and 1-OCP) on the quality of Hanfu apple during storage at ambient temperature were comparatively studied. The results showed that 1-MCP and its structural analogues could inhibit the respiration intensity and ethylene production rate, decrease the loss of fruit firmness, delay the reduction speed of acidity and inhibit the activities of cellulase and polygalacturonase related to fruit softening. Moreover, no significant difference was found between 1-MCP and its structural analogues.
Effect of Storage Temperature on Quality of Luncheon Sausages
FU Jun-jie,HE Zhi-fei,LI Hong-jun,YUAN Xian-qun,QUAN Tuo,LI Yan-li,YAO Yan-ling,JIANG Li-shi
2012, 33(12):  285-289.  doi:10.7506/spkx1002-6630-201212059
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In order to explore the quality change of luncheon sausages during the shelf life period and provide a theoretical guidance for good manufacture practice, the sensory quality, physiochemical index and microbiological index of three different types of luncheon sausages stored at mimic supermarket storage temperature 0-4 ℃ or 7-11℃ were determined at intervals of 10 days. The results indicated that total bacterial count of luncheon sausages stored at 0-4℃ was obviously lower than that of luncheon sausages stored at 7-11 ℃, suggesting that the low temperature can inhibit the growth of bacteria. Meanwhile, E. coli was not detected during storage at 0-4 ℃. Moreover, the samples stored at 7-11 ℃ revealed a larger fluctuation in pH, water-holding capacity and color when compared to the samples stored at 0-4 ℃. Therefore, a low temperature environment is better for the maintenance and stability of sausage quality.
Optimization of Alginate-Based Coating Formulation for Chicken Breast during Storage at 4 ℃
MA Qing-qing,BAI Yun,XU Xing-lian,ZHOU Guang-hong
2012, 33(12):  290-293.  doi:10.7506/spkx1002-6630-201212060
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Orthogonal array design method was used to optimize the formulation of sodium alginate and calcium chloride based coatings for chicken breast based on water loss rate and MDA content. The results showed that soaking in 2 g/100 mL alginate and then calcification with 2 g/100 mL calcium chloride for 2 min exhibited the best fresh-keeping effect on chicken breast.
Fresh-Keeping Effect of 1-MCP Combined with Na2S2O5 on Muskmelon (Cucumis melo)
WANG Liang-yan,ZHANG You-lin,ZHANG Run-guang,YIN Meng-ting
2012, 33(12):  294-298.  doi:10.7506/spkx1002-6630-201212061
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The postharvest physiology and storage characteristics of Cucumis melo L. treated by 1-methylcyclopropene (1-MCP), sodium metabisulfite (Na2S2O5) and their combination were studied. The results demonstrated that 1-MCP combined with Na2S2O5 could delay the maturation of fruits, inhibit the increase of soluble solids, significantly reduce decay rate and also inhibit the increase of phenylanlanine ammonialyase (PAL) and peroxidase (POD) activities, thus maintaining catalase (CAT) and superoxide dismutase (SOD) activities at a high level. After 80 days of storage the decay rate and the commodity rate were 0.37 and 80%, respectively. Therefore, 1-MCP combined with Na2S2O5 can maintain high storage quality of Cucumis melo L.
Fresh-Keeping Effect of High Electrostatic Field on Fresh-Cut Broccoli
JIANG Yao-ting,CHANG Xiu-lian,LI Lei
2012, 33(12):  299-302.  doi:10.7506/spkx1002-6630-201212062
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In this study, the effect of high electrostatic field on total bacterial count, protein content and vitamin C content, respiration intensity and sensory quality of fresh-cut broccoli was investigated. The results indicated that high electrostatic field with various voltage: 176.8, 278.8 kV and 443.4 kV had a prominent eliminating effect on bacteria on the surface of fresh-cut broccoli. Ozone generated in a corona discharge delayed the metabolism of the fresh-cut cauliflower so that the loss of its protein and vitamin C as well as respiration intensity could be controlled effectively. The fresh-keeping effect of electrostatic field was better than the control group. The optimal voltage and treatment time were 278.8 kV and 20 min, respectively. Based on the above results, the conclusion can be drawn that high electrostatic field treatment is an effective method for the preservation of fresh-cut broccoli.
Effect of Low-Temperature Treatment on Chilling Injury in Cherry Fruits
ZHANG Ping,ZHANG Peng,LIU Hui,CHEN Shao-hui,ZHANG Xiu-min,LI Jiang-kuo
2012, 33(12):  303-308.  doi:10.7506/spkx1002-6630-201212063
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In order to prevent cherry fruit loss caused by chilling injury during storage, the effect of low-temperature storage on chilling injury in cherry fruits was explored to determine the optimal storage temperature. Four cherry varieties including Juhong, Summit, Lapins and Rainier were measured for their chilling injury index, sensory quality and physiological index during storage at -0.5, -1.0, -1.5 or -2.0 ℃. The results showed that the chilling injury increased with decreasing temperature. Moreover, all four types of cherry fruits stored at -2.0 ℃ revealed obvious chilling injury with a decay rate of 100%, and lost the edible value completely. However, the cherry fruits stored at -0.5 ℃ had the minimal chilling injury. Meanwhile, the activities of SOD and POD and the content of total phenols in Juhong at the storage condition of -0.5 ℃ were higher than those of other three varieties. In contrast, its PPO activity, MDA content and ethanol content were lower than other varieties although its sensory quality and physiological index were better than those of other varieties.
Effect of Regulated Superchilling on Quality Characteristics of Common Carp during Storage
HE Xue-ying,KONG Bao-hua,LIU Qian,LI Pei-jun
2012, 33(12):  309-312.  doi:10.7506/spkx1002-6630-201212064
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The effects of different storage conditions (-1, -3 or -3 ℃ coupled with freezing point modulator, and -18 ℃) on quality characteristics of common carp during storage were investigated. Under different storage conditions, the changes in total bacterial count, thiobarbituric acid value (TBARS) and brightness were determined. When the freezing temperature of -1 ℃ was adjusted to -3 ℃ by adding freezing point modulator, total bacterial count, brightness, TRBAS value and volatile basic nitrogen content revealed a slow increase up to a level that exhibited a significant decrease when compared to storage at -1 and -3 ℃ (P < 0.05). Therefore, the freezing point of common carp can be regulated by the modulator, and microbial growth can be inhibited during regulated freezing storage thus prolonging the shelf life.
Orthogonal Array Design for Optimization of Konjac-Glucomannan Blend Film Formulation and Its Preservative Effect on Bell Pepper (Capsicum annum L.) Fruits
ZHANG Yan-mei,WANG Hui,QIN Wen
2012, 33(12):  313-317.  doi:10.7506/spkx1002-6630-201212065
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A five-variable, two-level orthogonal array design was employed to optimize the formulation of edible blend films based on konjac glucomannan (KGM) for bell pepper fruits. Besides, the effect of KGM-based edible blend films on aging index, malondialdehyde (MDA) content, vitamin C content and chlorophyll content was investigated during storage of bell pepper fruits at (9 ± 1 )℃. The results showed that the formula for KGM-based edible blend films was 8 g/L KGM, 0.35% glycerol, 1.0 g/L kojic acid, 0.4 g/L EDTA and 0.1 g/L vitamin C. After 30 d storage, the aging index, MDA content, vitamin C content and chlorophyll content of bell pepper fruits treated with KGM-based edible blend films were 0.32, 0.87 nmol/g, 25.0 mg/100 g and 0.08 mg/g, respectively, indicating that KGM-based edible blend films are better for preserving bell pepper fruits compared to control samples.
Multivariate Analysis of Fruit Quality of Angeleno , Plum Fumigated with Four Volatile Compounds
WANG You-sheng,GUO Xiao-min,WANG Zhi-yuan,LI Li-ping,YANG Hong-wei
2012, 33(12):  318-323.  doi:10.7506/spkx1002-6630-201212066
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TThe influence of four postharvest fumigation treatments on fruit quality and antioxidant properties of Angeleno, plum were analyzed using multivariate analysis. The results of one-way analysis of variance showed that chlorine dioxide significantly reduced fruit decay rate as well as total phenols, total flavonoids, antioxidant ability and scavenging capacities against superoxide and hydroxyl radical after 18 days of storage at 20 ℃. In contrast, 1-methylcyclopropene (1-MCP) promoted the total phenol, flavonoid and anthocyanin contents of plum fruit, whereas the pulp a* value, hue angle, and color ratio increased significantly in fruit treated with both thymol and ethanol as compared with the control. The correlation analysis indicated that both total phenol and total flavonoid contents of plum were highly correlated (P<0.01) with antioxidant parameters including total antioxidant activity and scavenging capacities against superoxide, DPPH radical and hydroxyl radical. The results of PLSR and path coefficient analysis showed that decay rate of plums was positively correlated with a* value, whereas hue angle of fruit pulp was positively correlated with hydroxyl radical scavenging capacity.
Technology Application
Optimization of Quick-Frozen Sweet and Sour Spareribs Recipe
REN Hong-tao,SHAO Jian-feng,CHENG Li-ying,YANG Lian-zhi
2012, 33(12):  324-329.  doi:10.7506/spkx1002-6630-201212067
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Orthogonal array design method was used to optimize the industrial formulation of quick-frozen sweet and sour spareribs and to investigate the effects of various processing conditions on sensory quality. Meanwhile, the formulation of seasoning sauce was optimized by uniform experimental design and quadratic polynomial regression analysis. The optimal quick-frozen sweet and sour sparerib formula was 500 g of meat, 50 g of sugar, 10 g of soy sauce, 70 g of vinegar, and 40 g of cooking wine. The optimal processing conditions were 10 min precooking, 10 min curing, 3 min deep frying, 15 min high fire cooking. The optimal seasoning sauce was composed of 50 g of meat, 35 g of oil, 15 g of sugar, 5.98 g of soy sauce, 10.71 g of cooking wine, 30.77 g of vinegar, 71.93 g of water, and 0.45 g of salt.
Process Optimization for Development of Jam from Fresh Jujubes
JIAO Wen-yue,LU Zhou-min,ZHAO Jia-qi,ZHAO Nan,HUA Zhi-xiu
2012, 33(12):  330-333.  doi:10.7506/spkx1002-6630-201212068
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Fresh jujubes were softened, beaten into pulp and cooked with the addition of white sugar and citric acid to prepare fruit jam. Various softening parameters were investigated. White sugar and citric acid amounts and cooking time were optimized by orthogonal array design. The results indicated that steam softening could maintain most nutrients of jujubes. Cooking time had the highest effect on jam quality, followed by white sugar amount; the effect of citric acid amount was the weakest. Fruit jam with high sensory and nutritional quality was obtained through beating jujubes in the presence of water at a mass ratio of 1:1 into pulp followed by 15 min cooking with the addition of 140 g of white sugar and 0.8 g of citric acid.