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Table of Content

25 February 2012, Volume 33 Issue 4
Processing Technology
Intensified High-Temperature Air-Drying Ripening of Chinese Bacon and Its Effect on Lipid Oxidation and Sensory Quality
WANG Yan,ZHANG Jian-hao,LIU Jia,PENG Jie,SUN Li-shuang
2012, 33(4):  1-7.  doi:10.7506/spkx1002-6630-201204001
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Intensified high-temperature air-drying ripening was used for the production of Chinese bacon from pork bellies and its effect on lipid oxidation and sensory quality in Chinese bacon was investigated. The results showed intensified treatment at 65 ℃ activated lipoxygenase (LOX) significantly (P < 0.05), and resulted in a decrease of 26.1% in the TBARS value and of 45% in the POV value and a 14.0% increase in the sensory evaluation score of Chinese bacon when compared with the control (without high-temperature intensification before air drying), indicating that intensified high-temperature treatment can promote lipid oxidation and the accumulation of flavor substances and reduce oxidation indexes. The optimal levels of intensifying temperature, drying temperature, relative humidity and drying time were respectively 65 ℃, 18-29.5 ℃ (increasing by 1.5 ℃ per day), 72%-68.5% (decreasing by 0.5% per day) and 8 days as demonstrated by regression optimizations based on TBARS value and sensory evaluation score. The dry-cured product obtained under these conditions contained 3.56% of salt and 52.2% of moisture, and the results were in good agreement with sensory analysis.
Process Optimization for Blanching, Enzymatic Treatment and Ultra High Pressure Sterilization of Radish Juice
XU Xia-yang,ZHANG Fu-sheng,CHEN Fang,WU Ji-hong,HU Xiao-song
2012, 33(4):  8-12.  doi:10.7506/spkx1002-6630-201204002
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This study aimed to optimize process parameters for the blanching, enzymatic treatment and ultra high pressure (UHP) sterilization of radish juice. The results showed that myrosinase in radish dices was inactivated completely after blanching for 3 min at 100 ℃. The juice yield reached 81.48% after 60 min of treatment with 40 ℃, pH 5.0,  0.15 g/L pectinase. In addition, UHP treatment had significant sterilization effect on microorganisms, which increased with increasing pressure and treatment time. The results of accelerated tests indicated that treatment at 500 MPa for 1 min was suitable for the sterilization of radish juice.
Response Surface Optimization of Ultrasonic-Assisted Extraction of Total Flavonoids from Flos Buddlejae
GUO Lei,WANG Shu-jun,LIU Wei-wei
2012, 33(4):  13-17.  doi:10.7506/spkx1002-6630-201204003
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This paper reports the optimization of conditions for the ultrasonic-assisted extraction of total flavonoids from Flos Buddlejae. One-factors-at-a-time experiments were carried out to investigate the effects of ethanol concentration, ultrasonic power and extraction temperature on extraction yield of total flavonoids. Further, the process parameters were optimized using a Box-Behnken experimental design coupled with response surface methodology. The optimal extraction conditions were determined as follows: ethanol concentration 62%, ultrasonic power 410 W, extraction temperature 77 ℃, liquid/material ratio (mL/g) 50:1, and extraction time 35 min. Under the optimal conditions, the extraction yield of total flavonoids from Flos Buddlejae was 20.38%.
Optimization by Orthogonal Array Design of Ultrasonic Extraction of Total Flavonoids from Chinese Date Seeds
ZHANG Ji-xiang,OU Lai-liang
2012, 33(4):  18-21.  doi:10.7506/spkx1002-6630-201204004
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Objective: The optimal conditions for ultrasonic extraction of total flavonoids from Chinese date seeds were investigated by orthogonal array design. Methods: The content of total flavonoids was determined spectrometrically using rutin as reference substance. The effects of ultrasonic power, extraction time, material/liquid ratio, ethanol concentration on the content of total flavonoids in extracts were investigated by one-factor-at-a-time method, and the extraction conditions were optimized by orthogonal array design. Results: Ethanol concentration and ultrasonic power were the key factors that affect the extraction of total flavonoids. The optimal extraction conditions were obtained as follows: ultrasonic power 450 W, treatment time 30 min, material/liquid ratio 1:50 and ethanol concentration 50%. Under these conditions, the extraction yield of crude total flavonoids from Chinese date seeds was 7.04% and the content of total flavonoids in crude extracts 1.59%. Conclusion: The optimized process remarkably increases the extraction yield of total flavonoids from Chinese date seeds and has a promising prospect for practical applications.
Effect of Air Puffing Technology on Texture of Walnut Cereal Breakfast
LU Xiao-lian
2012, 33(4):  22-25.  doi:10.7506/spkx1002-6630-201204005
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Walnut meal and rice were used as main raw materials to produce walnut cereal breakfast by means of extrusion and subsequent air puffing. The optimal moisture content in materials and addition level of walnut meal, as determined based on texture properties of walnut cereal breakfast, were respectively 24% and 20%. The results of orthogonal array optimization indicated that the optimal air puffing conditions were air-puffing temperature of 280 ℃, air-puffing time of 45 s, water content of 12% and feeding rate of 1000 g/min.
Optimization of Ultrasonic-Assisted Extraction of Blackberry Seed Oil by Response Surface Methodology
CUI En-hui,FANG Liang,WU Wen-long,LI Wei-lin
2012, 33(4):  26-30.  doi:10.7506/spkx1002-6630-201204006
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In order to improve oil yield and quality, response surface methodology was employed to optimize the ultrasonic-assisted extraction of blackberry seed oil. A mathematical model was constructed describing oil yield as a function of temperature, extraction time, ultrasonic power and liquid (hexane)/material ratio. The optimal extraction conditions were obtained as follows: extraction temperature 42.82 ℃, extraction time 12.20 min, ultrasonic power 53.19 W, and ratio of solid to liquid 1:2.23. Under these conditions, the predicted oil yield was 12.6%, and the experimental value 12.5%.
Extraction and Antioxidant Activity of Polyphenols from Pomegranate Seeds
REN Ya-mei,LI Guang-hui,XU Yong-tao
2012, 33(4):  31-35.  doi:10.7506/spkx1002-6630-201204007
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Orthogonal array design was employed to optimize the extraction of polyphenols from the seeds of pomegranate cultivar   Yushizi,, grown in Huaiyuan of Anhui province. The extraction efficiency of polyphenols was investigated with respect to ethanol concentration, temperature, extraction time, addition level of sodium hexametaphosphate as a chelating agent, pH and material/liquid ratio. The total phenol, total flavonoid, total proanthocyanidin contents of the whole seeds, kernels and husks of pomegranate and the in vitro antioxidant effects of their polyphenol extracts were compared. Better results for the extraction of polyphenols were achieved after 100 min of extraction under the conditions: pH 4.0, 60 ℃, 0.4% sodium hexametaphosphate addition, and 20:1 solid-to-liquid ratio. Pomegranate seeds were rich in proanthocyanidins as the major antioxidant components in it. Polyphenols especially proanthocyanidins were mainly present in the seed kernels of pomegranate.
Optimization of Enzymatic Hydrolysis Parameters for Preparation of Fresh Wax Corn Juice
LIN Mei-juan,SONG Jiang-feng,LI Da-jing,LIU Chun-quan,JIN Bang-quan
2012, 33(4):  36-40.  doi:10.7506/spkx1002-6630-201204008
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The goal of this study was to develop an optimum hydrolysis process for preparing corn juice from fresh wax corn cultivar   Jiangnanhuanuo,,. A series of single factor experiments were carried out to address the effects of mid-temperature α-amylase dosage, neutral protease dosage and neutral protease hydrolysis time on suspension stability. Box-Behnken design coupled with response surface methodology (RSM) was employed to optimize hydrolysis conditions of fresh wax corn juice. The result showed that its suspension stability was significantly influenced by mid-temperature α-amylase dosage, neutral protease dosage as well as neutral protease hydrolysis time. The optimal hydrolysis conditions were achieved as follows: mid-temperature α-amylase dosage 7.5 U/g, neutral protease dosage 83 U/g and neutral protease hydrolysis time 43 min. Under these conditions, the suspension stability of fresh wax corn juice was improved to the greatest extent (OD660 = 1.832, presenting a relative error less than 0.5% when compared with the predicted counterpart). 
Ultrasonic-Assisted Aqueous Two-Phase Extraction and Antioxidant Activity of Total Flavonoids from Porphyra yezoensis
CHEN Li-mei
2012, 33(4):  41-46.  doi:10.7506/spkx1002-6630-201204009
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An ultrasonic-assisted aqueous two phase extraction method was presented for extracting total flavonoids from Porphyra yezoensis and the extraction conditions were optimized by an orthogonal array experimental design. Meanwhile, the hydroxyl free radical scavenging activity of total flavonoids from Porphyra yezoensis was determined. The results indicated that the method allowed effective extraction of total flavonoids. The extraction yield was 0.148%, which was significantly higher than that obtained by ethanol-water reflux extraction. The optimal extraction conditions were obtained as follows: n-propanol-to-water ratio 0.6, ammonium sulphate concentration 0.30 g/mL, ultrasonic treatment time 20 min and material-to-liquid ratio 0.04. P. yezoensis abundantly contained flavonoids and the total flavonoid extract from it had excellent hydroxyl free radical scavenging activity thus providing a good natural free radical scavenger.
Low-Temperature Extraction of Green Tea and Its Effect on Cream Down
CHEN Jie,LIU Zhang-hu,YANG Deng-xiang,GUO Xiao-chuan,LI Hao,NI Xue-wen
2012, 33(4):  47-51.  doi:10.7506/spkx1002-6630-201204010
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The present study was undertaken to provide insight into the effects of low-temperature extraction conditions on the extraction of major biochemical components from green tea. T640 (transmittance at 640 nm) and A420 (absorbance at 420 nm) were determined as measures of the color and turbidity of tea infusion, respectively. The results showed that appropriate amounts of major biochemical components were extracted from green tea by low-temperature extraction and the color of green tea infusion was good. Low-temperature extraction could provide an effective strategy to extract tea for the production of premium tea beverage. The results of orthogonal array optimization indicated that the optimal low-temperature extraction conditions were extraction for 3 h at 20 ℃ and a tea/water ratio of 1:50.
Extraction and Clarification of Golden Jujube Juice
JIAO Hui,XU Huai-de,MI Lin-feng,RUI Ming
2012, 33(4):  52-56.  doi:10.7506/spkx1002-6630-201204011
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This study aimed to optimize the extraction and clarification conditions of golden jujube juice. The results indicated that the highest extraction efficiency was obtained after 200 min of extraction at 50 ℃ and a material/liquid ratio of 1:10 (g/mL). Golden jujube juice obtained after hydrolysis at 45 ℃ for 120 min with a complex enzyme added at a level of 0.015% (V/V) showed the biggest transmittance, a clear and transparent appearance and a strong aroma. The best decolorization results were achieved after 180 min of oscillation at 25 ℃ and 120 r/min in the presence of LX-10C macroporous resin at an addition level of 7.0 g/100 mL.
A New Method for Preparation of Vitamin E Acetate Using SO42-/TiO2 Solid Super Acid and Spectroscopic Characterization
CHENG Hai-tao
2012, 33(4):  57-61.  doi:10.7506/spkx1002-6630-201204012
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The synthesis of vitamin E acetate using SO42-/Tio2 solid super acid as a novel catalyst was investigated with respect to catalyst dose, molar ratio of acetic anhydride to vitamin E, reaction time and reaction temperature. Based on fuzzy mathematical modeling, the optimal synthesis conditions were determined to be temperature 40 ℃, reaction time 3 h, molar ratio of vitamin E to acetic anhydride 1:1.2, and catalyst dose 1.0 g. Under these conditions, the conversion rate of vitamin E was 96.6%. The product obtained was identified as vitamin E acetate by infrared spectrum (IR), elemental analysis and 1H NMR.
Macroporous Resin Adsorption for Purification of Pigments from Wild Plum Skins and Their Stability
LI Zi-wei,OUYANG Yan,LA Ping,ZHANG Xue-rong,MA Xiao-rong
2012, 33(4):  62-65.  doi:10.7506/spkx1002-6630-201204013
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The purification of pigments from wild plum skins was studied by macroporous resin adsorption. Macroporous resin type D101 showed the best adsorption effect on pigments from wild plum skins among the resins tested, and the best elution results were achieved using 80% ethanol solution. Pigments from wild plum skins were stable under acidic conditions (pH ≤4), but unstable when exposed to light and heat. Al3+, Fe3+, Mg2+, Cu2+ and Na+ had obvious hypochromic effect on the pigments.
Enzymatic Preparation of Cello-oligosaccharides from Radix Puerariae Fiber
LIU Sheng-nan,WAN Xiao-chun,DU Xian-feng
2012, 33(4):  66-70.  doi:10.7506/spkx1002-6630-201204014
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An enzymatic method for the preparation of cello-oligosaccharides from Radix Puerariae fiber was developed, and HPLC was employed to determine the sugar composition of cello-oligosaccharide extracts. The effects of enzyme type and dose as well as hydrolysis time on cello-oligosaccharide composition and contents were explored. The results showed that β-glucanase was more suitable for the preparation of cello-oligosaccharides than cellulase. Hydrolysates consisting of mainly glucose, cellobiose and cellotriose were obtained using β-glucanase. The hydrolysate obtained after 2 h of hydrolysis with 3 U/g β-glucanase contained a high proportion of cellobiose and cellotriose and the yield of cello-oligosaccharides was 11.8 g/100 g under these conditions.
Optimization of Hydrolysis Process for Corn Gluten Meal by Response Surface Methodology
ZHENG Ming-yang,WANG Yuan-xiu,ZHANG Gui-xiang,SUN Na-xin
2012, 33(4):  71-76.  doi:10.7506/spkx1002-6630-201204015
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Response surface methodology based on Box-Benhnken experimental design was employed to optimize conditions for the dual-enzymatic hydrolysis of corn gluten meal to obtain the maximum degree of hydrolysis. The optimal hydrolysis conditions were found as follows: pH 11.10, hydrolysis temperature 55.00 ℃, substrate concentration 112 g/L, activity ratio of alkaline protease to neutral protease 5:1, total enzyme dose 48000 U/g, and hydrolysis time 120 min. Under these conditions, the actual degree of hydrolysis was 30.23%, and the predicted value 30.84%. The dual-enzymatic hydrolysis process was simple and provided a high degree of hydrolysis.
Ultrasound-Assisted Enzymatic Extraction and in vitro Antioxidant Activities of Soluble Soybean Polysaccharides
PAN Li-hua,XU Xue-ling,LUO Jian-ping
2012, 33(4):  77-81.  doi:10.7506/spkx1002-6630-201204016
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This paper reports an ultrasound-assisted enzymatic method for the extraction of soluble soybean polysaccharides. On the basis of single factor experiments, four crucial extraction parameters such as material/water ratio, ultrasonic power, extraction temperature and cellulase amount were optimized for maximizing the yield of soluble soybean polysaccharides using a four-variable, five-level quadratic rotation combination experimental design. Subsequently, the in vitro antioxidant activities of soluble polysaccharides extracted from soybean dregs were evaluated by hydroxyl radical, superoxide anion radical and DPPH radical scavenging assays. The maximum extraction yield of soluble polysaccharides from soybean dregs, 9.32%, was obtained after 20-min extraction under the optimal conditions: material-to-liquid ratio 1:25 (g/mL), ultrasound power 700 W, temperature 50 ℃ and cellulase amount 30 U/g. The resulting extract exhibited obvious scavenging activity against hydroxyl, superoxide anion and DPPH free radicals in a concentration-dependent manner.
Optimization of Alkaline Extraction Process for Capsaicin from Chili Pepper
SUN Jing,LI Cun-zhi,PENG Ning,HUANG Xue-song
2012, 33(4):  82-85.  doi:10.7506/spkx1002-6630-201204017
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In order to obtain the maximum extraction yield of capsaicin, extraction parameters such as pH, ethanol concentration, extraction time and temperature were optimized using an L9(34) orthogonal array design. Capsaicin content was determined by GC-MS. The results showed that capsaicin was decomposed at temperatures above 50 ℃. Slightly alkaline pH values were beneficial to the extraction of capsaicin. The extraction parameters could be ranked in decreasing order of importance in their effect on the extraction yield of capsaicin as follows: temperature > ethanol concentration > pH > extraction time. The optimal conditions of pH, ethanol concentration, temperature and extraction time were 8, 70%, 50 ℃ and 3.5 h, respectively. Under these conditions, the average extraction yield of capsaicin were 6.812 mg/g (n = 4).
Optimization of Enzymatic Hydrolysis of Orange Pomace by Response Surface Methodology
LIU Xin,LI Xin-sheng,WU San-qiao,ZHANG Zhi-jian,JIANG Hai,HAN Hao,GAO Yue,XU Yan-ming
2012, 33(4):  86-90.  doi:10.7506/spkx1002-6630-201204018
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Response surface methodology was used to optimize the enzymatic hydrolysis of orange pomace to achieve the maximum juice yield. The combination of pectinase and cellulase at a ratio of 1:2 was more suitable for the enzymatic hydrolysis of orange pomace than each of them. One-factor-at-a-time experiments were conducted to investigate the effects of temperature, pH, enzyme dose and hydrolysis time on juice yield. The optimal conditions for the hydrolysis of orange pomace by both enzymes were enzyme temperature 49.17 ℃, pH 4.23, enzyme addition 0.68 mg/g, and hydrolysis time 3.4 h. Under these conditions, the juice yield from orange pomace was 22.36%.
Optimization of Microencasuplation of Black Raspberry Juice by Response Surface Methodology
QU Xiao-yuan,HU Ping
2012, 33(4):  91-95.  doi:10.7506/spkx1002-6630-201204019
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Black raspberry juice was microencapsulated using sodium alginate and chitosan as wall materials by piercing-solidifying incuber method. Box-Behnken experimental design coupled with response surface was used to optimize key process conditions including wall/core material ratio, sodium alginate concentration and chitosan concentration. A polynomial regression model describing the effects of the process conditions on microencasuplation efficiency of black raspberry juice was established. The results showed that the best microencapsulation results were obtained under the conditions: wall/core material ratio 4.05, sodium alginate concentration 2.27%, and chitosan concentration 1.28%. The microencasuplation efficiency was up to 87.15%.
Influence of Different Production Lines on Quality of Orange Juice
XU Qin,CAO Yu-jiao,PAN Si-yi
2012, 33(4):  96-99.  doi:10.7506/spkx1002-6630-201204020
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This paper compares the quality of orange juice from three cultivars, Beipei 447, Zhongyu 7 and Wuhexuegan produced by two different concentrated orange juice production lines, FMC medium and lab-simulated production lines with the aim of selecting the better of the production lines. The results showed that the Beipei 447, Zhongyu 7 and Wuhexuegan concentration orange juices produced by the industrial production line exhibited 4.78-, 3.81-, and 3.39-fold increases in limonin content when compared with the corresponding fresh juices. By contrast, 2.78-, 2.48-, and 2.32-fold increases in limonin content were observed for Beipei 447, Zhongyu 7 and Wuhexuegan concentration orange juices produced by the lab-simulated production line. Squeezing and homogenization in the production lines had little effect on the quality of concentrated orange juice. The sterilization and concentration modes used in the lab-simulated production line were more conducive to increasing the quality of concentrated orange juice.
Optimization of Ultrasonic/Microwave-Assisted Extraction of Polysaccharides from Green Tea by Response Surface Methodology
CHEN Yi-yong,DOU Xiang-long,HUANG You-ru,ZHU Dong-xing,YU Da
2012, 33(4):  100-103.  doi:10.7506/spkx1002-6630-201204021
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Response surface methodology was used to optimize the ultrasonic/microwave-assisted extraction of water-soluble polysaccharides from crude green tea. The traditional water extraction and ultrasonic/microwave-assisted extraction methods were compared for their effect on extraction efficiency, purity and structure of polysaccharides. The optimal ultrasonic-assisted extraction conditions were extraction time of 23 min, material-to-liquid ratio of 1:30 (g/mL) and microwave power of 90 W. The ultrasonic/microwave-assisted extraction method required shorter time and increased polysaccharide yield from 2.95% to 4.19% and polysaccharide purity from 70.15% to 86.08% compared with the traditional water extraction method. Polysaccharides extracted by the methods had basically the same groups.
Ultrasound-Assisted Extraction and Heat Stability of Capsaicinoids from Doubanjiang (Bean Paste)
JIA Hong-feng,PENG De-chuan,LIANG Ai-hua,HE Jiang-hong,CHEN Zu-ming,HE Zhi-fei
2012, 33(4):  104-108.  doi:10.7506/spkx1002-6630-201204022
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A fast method has been developed for the extraction of capsaicinoids from Doubanjiang employing ultrasound-assisted extraction (UAE). The effects of operating parameters such as solvent type, temperature, extraction time and number of repeated extractions on the extraction rates of capaicin, dihydrocapsaicin and capsaicinoids were investigated. The optimum extraction conditions were ultrasound power of 200 W, ultrasound frequency of 40 kHz, Doubanjiang/methanol ratio of 2.5:10 (g/mL), temperature of 70 ℃, and twice-repeated extractions for 5 min each time. The results of thermal stability experiments indicated that capsaicinoid contents in Doubanjiang began to gradually decrease as the temperature increased from 130 ℃ and exhibited a distinct decrease when the temperature was over 200 ℃.
Response Surface Methodology for Optimization of Extraction Process of Soluble Dietary Fiber from Navel Orange Residue
WU Xiao-chen,WANG Ke-jun,ZHONG Jin-lian,LUO Xu-zhong
2012, 33(4):  109-114.  doi:10.7506/spkx1002-6630-201204023
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Navel orange residue was treated with cellulase to extract soluble dietary fiber. Extraction parameters including extraction temperature, cellulase dose and length of extraction time were optimized using Box-Behnken design and response surface methodology based on single factor investigations for achieving maximum yield of soluble dietary fiber. A regression equation reflecting the relationship between the yield of soluble dietary fiber and the extraction parameters was set up. The optimal extraction parameters were found as follows: extraction temperature, 48 ℃; cellulase dose, 1.25%; length of extraction time, 5 h. Under the optimized conditions, the actual yield of soluble dietary fiber was 13.11%, close to the predicted value of 13.14%.
Optimal Process Points and Methods for Fouling Control in Alcohol Production from Sugarcane Molasses
MAO Rui-feng,FANG Yan,WANG Shuang-fei,GUO Li-dong,LU Hai-qin,ZHAO Ri-xin
2012, 33(4):  115-121.  doi:10.7506/spkx1002-6630-201204024
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This paper describes the selection of multiple process points before the distillation stage in alcohol production from sugarcane molasses, use of gravity separation methods (diluted molasses standing settlement, fouling removal at the bottom of the fermentation tank, mechanical centrifugationl) and gravity separation methods with the addition of chemical additives to perform antifouling processing on materials in alcohol production from sugarcane molasses. Physical and chemical parameters such as apparent fouling, total calcium magnesium and total sulfate were measured on materials and fouling to assess fouling removal effectiveness and characteristics. Based on apparent fouling removal rate by various control methods at various process points, optimal process points and methods for fouling removal were analyzed and technical protocols for fouling control and removal in alcohol production from sugarcane molasses were proposed.
Optimization of Microwave Inactivation of Myrosinase Activity in Maca by Response Surface Methodology
TU Xing-hao,ZHANG Hong,ZHENG Hua,GAN Jin,XU Long-feng,LI Kun
2012, 33(4):  122-127.  doi:10.7506/spkx1002-6630-201204025
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The purpose of the present study was to explore the application of microwave to inactivate myrosinase in maca. One-factor-at-a-time experiments were carried out to investigate the effects of microwave intensity, treatment time and material-to-liquid ratio on the residual activity of myrosinase and glucosinolate content. Response surface methodology was employed to optimize the operating parameters based on the residual activity of myrosinase. A regression model that describes the residual activity of myrosinase as a function of the operating parameters was established. The results showed that myrosinase in maca almost lost all of its activity under the conditions: microwave intensity 14 W/g, material-to-liquid ratio 2:1, and treatment tine 60 s. In addition to effectively inactivating myrosinase, the microwave treatment resulted in a decrease of 28% and 21% in glucosinolate and VC contents, respectively compared with the traditional hot water blanching time, but had little effect on protein content.
Extraction of Red Pigment from Sunflower Seed Shells
XIE Jiao,WANG Hua,TAN An-qun,REN Ting-yuan,ZHANG Yin,LI Yuan-hu
2012, 33(4):  128-133.  doi:10.7506/spkx1002-6630-201204026
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With the aim of demonstrating the feasibility of extracting red pigment from sunflower seed shells and its utilization potential, the extraction, purification and stability of red pigment from sunflower seed shells was studied. Sunflower seed shells were extracted with 50% ethanol solution (pH 1-2) under ultrasonic assistance. Employing orthogonal array design, the optimal extraction conditions were determined as follows: temperature 55 ℃, material/liquid ratio 1:16, and extraction time 10 min. Under these conditions, the extraction yield of red pigment was 8.2%. The results from stability experiments indicated that the OD value and color of the pigment changed little when exposed to hydrogen peroxide, sodium sulfite, food additives or light, indicating good stability. However, poor stability was observed at temperatures higher than 80 ℃ or pH ≥ 3 as a result of notable changes in the color and OD. The purification yield of red pigment from crude extract was 6.30%.
Ultrasound-Assisted Extraction of Total Flavonoids from Stems and Leaves of Gynura divaricata (L.) DC. and Its Inhibitory Activity on α-Glucosidase
LIU Xu,LIU Wei-wei,CAO Xue-li
2012, 33(4):  134-139.  doi:10.7506/spkx1002-6630-201204027
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On the basis of single-factor experiments, three key process parameters including ethanol concentration, solid/liquid ratio and extraction number for the ultrasound-assisted extraction of total flavonoids from the stems and leaves of Gynura divaricata (L.) DC. were optimized by Box-Behnken experimental design coupled with response surface methodology. The inhibitory effects of crude total flavonoid extract and its different solvent fractions on α-glucosidase were investigated. The results showed that the optimal ultrasound-assisted extraction conditions were 55% ethanol as extraction solvent at a material/liquid ratio of 1:35 (g/mL) for 4 repeated extractions. Under these conditions, the actual extraction yield of total flavonoids was 3.071%, which was basically consistent with the predicted value, 3.095%. HPLC analysis revealed that the major components in crude extract had the absorption characteristics of flavonoids.
Analysis & Detection
A Chemometrics-Assisted Potentiometric Method for Simultaneous Determination of Cinnamic Acid and L-Phenylalanine
HE Yang-chun,FANG Sheng
2012, 33(4):  140-143.  doi:10.7506/spkx1002-6630-201204028
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In this work, we proposed a new method for the simultaneous determination of cinnamic acid, L-phenylalanine and amonium sulfate in solution using combined potentiometric titration and chemometrics. The partial least squares (PLS) algorithm was applied and 25 standard mixtures of the compounds were prepared according to orthogonal experimental design for calibration set. The commonly used leave-one-out cross-validiation method was used to select the optimum number of factors in the PLS model. An independent set of synthetic raw mixtures was employed to evaluate the prediction performance of the resulting models. The results showed that the recovery values ranged from 92.9% to 104.4% for cinnamic acid, 94.9% to 101.5% for L-phenylalanine, and 96.6% to 105.1% for amonium sulfate respectively. The study proves the feasibility of simultaneous spectrometric determination of cinnamic acid, L-phenylalanine and ammonium salts in raw mixtures without preliminary separation steps.
Simultaneous Determination of Malachite Green, Methylene Blue, Crystal Violet as well as Their Metabolites in Aquatic Products by High Performance Liquid Chromatography
GONG Xiang-hong,XU Ying-jiang,REN Chuan-bo,LIU Hui-hui,TIAN Xiu-hui,ZHANG Shi-juan
2012, 33(4):  144-147.  doi:10.7506/spkx1002-6630-201204029
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A solid-phase extraction coupled with high performance liquid chromatography (SPE-HPLC) was presented for the simultaneous determination of malachite green, methylene blue, crystal violet as well as their metabolites (leucomalachite green for malachite green, azure A, azure B, azure C for methylene blue, and leucocrystal violet for crystal violet). Samples were extracted with a mixture of ammonium acetate buffer and acetonitrile, cleaned up with dichloromethane, purified on an MCAX solid phase extraction cartridge using a mobile phased made up of acetonitrile and 0.125 mol/L ammonium acetate buffer, and detected by a UV detector. The limits of quantification (LOQ) of the method were 20 μg/kg for malachite green, leucomalachite green, crystal violet, leucocrystal violet and azure B and 0.5 μg/kg for methylene blue, azure A and azure C, respectively. An average spike recovery above 70% was found for malachite green, leucomalachite green, leucocrystal violet, crystal violet and azure B at spike levels ranging from 2 to 40 μg/kg and for methylene blue, azure A and azure C at spike levels between 5μg/kg and 80 μg/kg, with a relative standard derivation (RSD) less than 15%.
Determination of Multiple Pesticide Residues in Coix Seed
LI Jun,WANG Zhen,PANG Hong-yu,GUO Xiao-guan,REN Yu-juan,WU Xu-gang
2012, 33(4):  148-152.  doi:10.7506/spkx1002-6630-201204030
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A method to simultaneously determine 43 pesticide residues in coix seed is described in this paper. Samples were extracted by accelerated solvent extraction (ASE), cleaned up by either solid phase extraction (SPE) or gel permeation chromatography (GPC), and analyzed by gas chromatography-mass spectrometry (GC-MS). The spike recoveries obtained by SPE and GPC were 72.45%-111.74% and 74.70%-106.49%, and the RSDs 1.47%-5.06% and 1.58%-5.08%, respectively.  Correlation coefficients between 1.47% and 5.06% were found for the established calibration curves. The limits of detection (LOD) of the method varied from 0.002 to 0.02 mg/kg, and the limits of quantification (LOQ) from 0.005 to 0.05 mg/kg. The method was efficient, accurate, sensitive and applicable for the simultaneous determination of multiple pesticide residues in coix seed.
Determination of Thiocyanate in Milk and Milk Powder by Gas Chromatography-Mass Spectrometry
ZHOU Zheng-xiang
2012, 33(4):  153-156.  doi:10.7506/spkx1002-6630-201204031
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Gas chromatography-mass spectrometry was used to determine thiocyanate residues in dairy products (mainly liquid milk and milk powder). Samples were extracted by shaking before derivatization based on the replacement reaction of pentafluorobenzyl bromide with thiocyanate. The derivatization products were separated using a high-speed refrigerated centrifuge and scanned in the selected ion monitoring mode. Thiocyanate was qualified based on retention time and ion abundance ratio and quantified by external standard method. High recovery, sensitivity, accuracy and reproducibility were found in the quantitative range of 0.02-50.0 mg/kg. The method was characterized by simple pretreatment, easy operation, low cost and time saving, and applicable for the rapid determination of thiocyanate residues in dairy products.
Analysis of Key Aroma-Active Components of Propolis and Poplar Tree Gum
YAN Sha,ZHANG Hong-cheng,DONG Jie
2012, 33(4):  157-161.  doi:10.7506/spkx1002-6630-201204032
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The volatile composition of propolis and poplar tree gum was analyzed by headspace solid phase micro-extraction followed by GC-MS coupled to olfactometry. A total of 48 aroma-active compounds were identified, including esters, aldehydes, alcohols, ketones and acids. In propolis, there were many compounds responsible for the floral and fruity aroma and providing it with delicate and mellow aroma characteristics.
Determination of Lactose, Glucose and Galactose Contents in Fermented Milk by HPLC
LI Qi,ZHANG Lan-wei,ZHANG Ying-chun,YI Hua-xi,DU Ming,HAN Xue, GUO Chun-feng,LI Jing-yan,XUE Chao-hui
2012, 33(4):  162-166.  doi:10.7506/spkx1002-6630-201204033
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An HPLC method for the determination of lactose, glucose and galactose in fermented milk was established. Proteins from samples were precipitated with Carrez reagent. The chromatographic separation was achieved on an Aminex HPX 87H column using 5 mmol/L H2SO4  as mobile phase at a flow rate of 0.6 mL/min. Good separation was obtained for the analytes. The calibration curves established showed good linearity over the concentration range of 0.5 to 12 mg/mL, with a correlation coefficient of 0.9986 to 0.9999 (n=5). The mean spike recoveries for the sugars in fermented skim milk prepared in our lab varied from 96.45% to 101.78% with a RSD between 0.62% and 4.21% (n=5). The reproducibility RSDs ranged from 1.86% to 3.44%. The method was rapid, accurate and reliable.
Analysis and Evaluation of Trace Elements in Edible Parts of Coelomactra antiquata
MENG Xue-ping,HAO Jue, LIANG Meng,SHEN Xin,ZHAO Na-na, CHENG Han-liang,YAN Bin-lun,TIAN Mei
2012, 33(4):  167-172.  doi:10.7506/spkx1002-6630-201204034
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In order to evaluate the nutrition value and heavy metal pollution of the edible parts of Coelomactra antiquata, the adductor muscle, mantle, foot, gill and visceral mass of Coelomactra antiquate from the Yellow Sea near Rizhao, the East Sea near Zhangzhou and a certain Vietnamese sea area of the Beibu Gulf (adjacent to the sea off the coast of Beihai in Guangxi) were analyzed for Ag, As, Cd, Cr, Co, Cu, Fe, Mn, Pb, Se, Sn and Zn contents by inductively coupled plasma atomic emission spectrometry (ICP-AES) after digestion with mixed HNO3-HClO4  acid. The average spike recovery rates for the metal elements varied from 78.3% to 112.1% with relative standard deviations between 0.16% and 7.64%. Coelomactra antiquate was rich in essential trace elements such as Fe, Zn, Mn, Cu, and Se and a small amount of Ag and Sn. The majority of the elements under investigation showed a significant difference in their contents in the different parts of Coelomactra antiquate from the same sea area (P<0.05). The mantle and visceral mass of Coelomactra antiquate from the sea near Rizhao contained significantly more Fe than other tissues and all tissues of Coelomactra antiquate from other two sea areas. The contents of As and Cd in Coelomactra antiquata exceeded the limits stipulated by the national hygiene standards, while Cd content was below the limits stipulated by the World Health Organization, Australia and Hong Kong. 
Direct Separation and Determination of Synthetic Pigments in Jelly by Capillary Electrophoresis
DU Jian-zhong,XIE Wei-wei,CAI Quan-lin,JIN Bei
2012, 33(4):  173-177.  doi:10.7506/spkx1002-6630-201204035
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A method was developed for the direct determination of brilliant blue, ponceau 4R and tartrazine in jelly by capillary electrophoresis. The effects of several factors, such as pH value, type and concentration of running buffer, separation voltage on the separation of the synthetic pigments were investigated to find optimum conditions. The best separation among brilliant blue, ponceau 4R and tartrazine was achieved within 6 min under the following conditions: a mixture of 5 mmol/L Na2HPO4 and 5 mmol/L Na2B4O7 (pH=8.5) as running buffer, separation voltage 18 kV, and detection wavelength 255 nm. The method has been used to determine some commercial jellies with satisfying results and recovery rates between 85% and 110%.
Comparison of Several Determination Methods for Sulfur Dioxide in Wine
LIANG Hong,LIN Yan-kui,WANG Bing-tao,WANG Yao-yu,YAN Zhi,WANG Lou-ming,SHEN Yan
2012, 33(4):  178-181.  doi:10.7506/spkx1002-6630-201204036
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To make a detailed comparison among the four national standard methods oxidation, distillation, iodine titration, hydrochloric pararosaniline and flow injection method, the factors the affect the determination of sulfur dioxide in imported wines by each of them and their repeatability were investigated. Significant differences existed among the results obtained using the different methods. The results obtained using the methods of oxidation, distillation and flow injection showed a small difference (P > 0.05), but differed greatly from those obtained using the other two methods (P < 0.01). Since the methods differ in suitability, the appropriate method should be carefully selected according to the specific details of samples and the requirements for the determination of sulfur dioxide to reduce determination errors.
Uncertainty Evaluation of Calcium Determination in Fruits by Microwave Digestion-Flame Atomic Absorption Spectrometry
WU Yong-long,NIE Ji-yun,LI Jing,LI Hai-fei,XU Guo-feng,QIN Xing,LI Zhi-xia
2012, 33(4):  182-185.  doi:10.7506/spkx1002-6630-201204037
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A mathematic model for evaluating the uncertainty in the determination procedure for calcium content in fruits by microwave digestion-flame atomic absorption spectrometry (FAAS) was established. The uncertainty sources for each parameter in the model were analyzed. The uncertainties of type A (based on the calculation of the statistical distribution of the determination results) type B (based on the estimation by experience and the probability distribution of other information) were evaluated. According to JJF 1059-1999, the component uncertainties were synthesized and extended. An expanded uncertainty of 1.18 mg/kg was obtained at the confidence probability of 95% and coverage factor of  k=2. Based on the analysis of uncertainty, the preparation of standard solutions and the fitting of standard curves were the major sources of uncertainty, while sample weighing and the preparation of digestion solution revealed little effect on the final uncertainty. Meanwhile, some strategies for improving quality control were proposed.
Determination of Sodium Cyclamate in Pickles by Liquid Chromatography-Mass Spectrometry
XU Qin,MU Zhi-chun,HAO Jie,LIU Lin,CAI Xue,LIN Hong
2012, 33(4):  186-188.  doi:10.7506/spkx1002-6630-201204038
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A liquid chromatography-mass spectrometry (LC-MS) method was developed for determining sodium cyclamate in pickles. Pickle samples were extracted directly by water and the separation was performed on a ZORBAX SB-C18 column (4.6 mm × 250 mm, 5 μm) in an isocratic elution mode using a mobile phase consisting of acetonitrile and 0.1% formic acid (25:75, V/V) at a flow rate of 0.6 mL/min. Sodium cyclamate was monitored by ESI MS in the SIM negative ion mode on the basis of [M-Na]-  ion m/z 178.1 and quantified using the external standard method. Key experimental conditions were optimized. The calibration curve of the method revealed an excellent linear relationship in the concentration range of 0.1-5.0 mg/kg (R2 =0.99987), and the limit of quantification (LOQ) was 0.1 mg/kg. The recovery rates across three spike levels were higher than 82.0% with RSD of 2.59%-4.82% (n = 6). The method was simple, accurate and suitable for the determination of sodium cyclamate in pickles.
Extraction and Determination of Lutein in Formulated Foods for Infant and Young Children
SHAN Yi,JIANG Yu-jun,CHEN Yi,WANG Xiang-xin,E Lai-ming
2012, 33(4):  189-192.  doi:10.7506/spkx1002-6630-201204039
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Three methods for extracting lutein from formulated foods for infant and young children such as potassium hydroxide saponification, acetone extraction and n-hexane extraction were compared, and the n-hexane extraction method was found to be the best of them. An HPLC method for the determination of lutein was developed based on the selected extraction method. The chromatographic separation was performed on a YMC Carotenoid (4.6 mm × 250 mm, 5μm) using a mobile phased composed of methanol and methyl tertiary butyl ether under a gradient elution mode at a flow rate of 1 mL/min. Lutein was detected at the wavelength of 445 nm. The method was characterized by easy operation and high extraction efficiency (95.4% average recovery), and good reproducibility (0.93% RSD). The detection limit was 2μg/100 g. It allowed accurate determination of lutein in formulated foods for infant and young children.
Direct Determination of Arsenic and Lead in Fruit Juice by Inductively Coupled Plasma Mass Spectrometry
HE Tao,SUN Meng-yin,JIANG Jie,WU Ying,ZHU Lei,WANG Zhen
2012, 33(4):  193-195.  doi:10.7506/spkx1002-6630-201204040
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Inductively coupled plasma mass spectrometry (ICP-MS) with dynamic reaction cell (DRC) was applied for the direct determination of arsenic (As) and lead (Pb) in fruit juice via microinjection and online addition of 115In as internal standard. The limits of detection for As and Pb were both less than 2.000μg/L. The results showed that the spiked recovery rates were in the range of 95.69%-105.45% for As and 100.98%-105.14% for Pb. This method was validated by juice reference material. The analytical value (0.0875 μg/g) was consistent with the recommended value (0.085 μg/g) with RSDs of 2.50% and 2.94% for As and Pb, respectively. The results obtained using microwave digestion followed by ICP-MS and the method showed no significant difference. The method was simple, rapid, accurate and completely met the requirements for the determination of arsenic and lead in fruit juice.
Comparative GC-MS Analysis of Volatile Oil Composition of Dehydrated and Freeze Dried Green Pepper (Piper nigrum L.)
DING Cheng-cui ,XU Zhi,ZHANG Cheng-hui,NIU Lei
2012, 33(4):  196-199.  doi:10.7506/spkx1002-6630-201204041
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In this study, the volatile oil composition of dehydrated and freeze dried green pepper (Piper nigrum L.) was extracted by steam distillation and analyzed by gas chromatography-mass spectrometry (GC-MS). The results demonstrated that the yields of volatile oil from dehydrated and freeze dried green peppers were 2.25% and 2.56%, respectively. Meanwhile, a total of 42 chemical components were identified in the volatile oils of green pepper subjected to the different treatments, including 35 found in dehydrated green pepper and 38 in freeze dried green pepper. Thirty-one components were presented in both of them. 
Qualitative Analysis of Edible Oil Oxidation by Near Infrared Transmission Spectroscopy
ZHANG Jing-ya,ZHANG Jian-xin,YU Xiu-zhu,DU Shuang-kui
2012, 33(4):  200-203.  doi:10.7506/spkx1002-6630-201204042
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To establish a quick method for identifying of edible oil oxidation, the qualitative discrimination between oxidized and unoxidized oils as categorized according to the limits of acid value and peroxide value stipulated by the Chinese national standards was modeled based on near infrared transmission spectroscopy (NITS) and distance-discrimination analysis. The results indicated that recognition rates of the calibration and external validation models reached up to 99% and 97.8% in the wave number range from 5450 cm-1 to 4650 cm-1 after multiple scattering correction, first derivative and Norris derivative smoothing. Therefore, good prediction results were achieved. In conclusion, it is feasible to apply NITS to qualitatively analyze edible oil oxidation
Rapid Analysis and Evaluation of Freshness of Chilled Pork Based on Color Difference
CHEN Xiao-liang,WANG Shi-ping,LIU Huan
2012, 33(4):  204-208.  doi:10.7506/spkx1002-6630-201204043
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The variability during storage under 4 ℃ and 20 ℃ of chilled pork (longissimus dorsi muscle) was studied in globulin precipitation, sensory evaluation, pH, water content and the color and color parameters of pork surface and extract. The results indicated that the variations of globulin precipitation and pH in chilled had a significant difference. The color changes such as L* of pork surface under 20 ℃ and L*, b*, C and ΔE* of pork extract differ significantly (P<0.05). The relationship between color changes and pH or storage time of chilled pork during storage was established. The CIE a* under 20 ℃, b* and C under 4 ℃ of pork surface as well as the L*, b*, C, and ΔE*  of pork extract under 20 ℃ and L* under 4 ℃ were positively correlated with storage time. Moreover, the L* of pork surface under 4 ℃, the L*, b*, C and ΔE*  of pork extract under both temperatures and a* under 4 ℃ were correlated positively with pH; when L* >48.73, a* >4.72 and b* >9.18, chilled pork could be identified as fresh meat in cold chain.
Simultaneous Determination of Carbamate Insecticides and Metabolite Residues in Animal Muscle by High Performance Liquid Chromatography-Tandem Mass Spectrometry
DENG Long,GUO Xin-dong,HE Qiang,YANG Qun-hua,SHEN Yu-dong,WANG Hong
2012, 33(4):  209-213.  doi:10.7506/spkx1002-6630-201204044
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A high performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (HPLC-ESI/MS/MS) method for rapid determination of 16 residual analytes including carbamate insecticides and their metabolites in animal muscles was established. Samples were extracted with acetonitrile, and the extract was then condensed, cleaned up, analyzed by reversed phase HPLC-ESI/MS/MS, and quantified by internal standard method. The calibration curves for the analytes exhibited a good linear relationship in the range of 1.0-100 μg/L with correlation coefficient higher than 0.9959. The limits of quantification (LOQ) ranged from 0.5 to 2.5 μg/kg. The recovery rates of the analytes from animal muscle sample across the spike levels of 5.0, 10.0μg/kg and 20 μg/kg were in the range of 71.4%-105.5% with relative standard deviation (RSD) varying from 3.2% to 13.7%. The method was accurate, sensitive, simple and suitable for the simultaneous analysis of  carbamate insecticides and their metabolite residues in animal muscle.
Preparation of Electrochemical Sensor Modified by Molecularly Imprinted Nano-porous Film for Melamine Determination
ZHAO Chang,YU Bo,CHEN Zhen-xing,JIN Guan-ping
2012, 33(4):  214-218.  doi:10.7506/spkx1002-6630-201204045
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A molecularly imprinted nano-porous film for melamine adsorption was electrochemically generated in situ on a paraffin-impregnated graphite electrode with a melamine/chitosan/nano-silver/polyquercetin complex. The film displayed a 3D network structure as characterized using field emission scanning electron microscopy, X-ray photoelectron spectroscopy, infrared spectroscopy and electrochemical techniques. The modified electrode exhibited a highly selective enrichment for melamine. Oxidation peak current and melamine concentration in the range of 1 × 10-7 -1 × 10-5 mol/L showed an excellent linear relationship. The detection limit of the method was 1 × 10-8 mol/L (3σ). The modified electrode had excellent anti-interference performance and allowed the determination of melamine in milk.
Determination and Safety Evaluation of Inorganic Arsenic in Shellfish by Hydride Generation-Atomic Fluorescence Spectrometry
HAO Yun-bin,SONG Hong-qiang,WU Yi-chun,LUO Hai-jun,ZHU Shi-jun,SUN Ya-qin
2012, 33(4):  219-222.  doi:10.7506/spkx1002-6630-201204046
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This paper describes the application of hydride generation-atomic fluorescence spectrometry (CF-HGAFS) for the determination of inorganic arsenic in four main commercial shellfish species in Zhoushan city, Zhejiang province. Besides, their food safety was assessed. Inorganic arsenic contents in the edible parts of clam, razor clam, oyster and mussel found to be in the range of 138-0.191, 0.112-0.171, 0.067-0.163, 0.070-0.168 mg/kg respectively, were consistent with the national food hygiene standards and inorganic arsenic intakes from them were below the WHO/FAO JECFA recommended acceptable daily intake (ADI) of 129 μg per person per day.
Comparative Analysis of Fatty Acid Composition of Eel Liver and Bone
LIU Jin-hai,HUANG Shi-yu,HUANG Yu-ying,SUN-Min,GUAN Rui-zhang
2012, 33(4):  223-226.  doi:10.7506/spkx1002-6630-201204047
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Oils from eel liver and bone were extracted by organic solvent extraction and comparatively analyzed for differences in sensory performance, physicochemical properties and fatty acid composition. The results showed that the sensory performance of eel liver oil was better than that of eel bon oil, although both oils could reach the requirements of first-class refined fish oil stipulated in the standard SC/T 3502-2000. The content of saturated fatty acids in eel liver oil decreased compared with eel bone oil (respectively 24.3% and 34.9%). The content of monounsaturated fatty acids was similar in both oils (respectively 48.0% and 49.6%). The content of polyunsaturated fatty acids was higher in eel liver oil (12.1%) than in eel bone oil (3.3%), especially EPA (1.90% versus 0.6%) and DHA (9.0% versus 1.6%). The content of unknown fatty acids found in eel liver oil (15.7%) exhibited a slight increase compared with eel bone oil (12.1%). In conclusion, eel liver oil has higher nutritional value and better quality than eel bone oil in terms of the varieties and amount of fatty acids.
Determination of Hexaconazole in Fruits and Vegetables by Gas Chramtography Tandem Mass Spectrometry
FU Xiao-fang,LI Jing,WANG Peng,ZHAO Xiao-ya,SHANG Yin-zhu,SUN Ming-ju,YE Cheng
2012, 33(4):  227-229.  doi:10.7506/spkx1002-6630-201204048
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A gas chromatography-tandem mass spectrometric (GC-MS/MS) method was established for the determination of hexaconazole in fruits and vegetables. Samples were extracted with acetonitrile, and cleaned up on a GCB/NH2 SPE column using a mixture of petroleum ether and acetone at ratio of 15:85 (V/V). The chromatographic separation was carried out on a DB-5 ms column. The limit of detection for hexaconazole was 0.02 mg/kg. The precision RSDs and spike recoveries of the method were separately 3.03%-9.34% and 92.24%-106.13%. The method was highly linear, repeatable and accurate and thus could offer a suitable method for the accurate determination of hexaconazole residue in fruits and vegetables.
Simultaneous Determination of 14 Sulfonamide Residues in Fishery Products by High Performance Liquid Chromatography with online Postcolumn Derivatization and Fluorescence Detection
ZHENG Bin,YU Hai-xia,YANG Hui-cheng,LIAO Miao-fei,FU Guang-ming,ZHANG Xiao-jun
2012, 33(4):  230-233.  doi:10.7506/spkx1002-6630-201204049
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A new method for the determination of 14 sulfonamide (sulfanilamide, sulfadiazine, sulfathiazole, sulfamerazine, sulfameter, sulfamethazine, sulfamethoxypyridazine, sulfachlorpyridazine, sulfamonomethoxine, sulfamethoxazole, sulfadoxine, sulfafurazole, sulfadimethoxine, and sulfaquinoxaline) residues in fishery products using high performance liquid chromatography (HPLC) equipped with fluorescence detector was established. Homogenized samples were extracted with ethylacetate, reverse-extracted into hydrochloric acid, defatted with hexane, separated by reversed-phase column chromatography, treated by on-line post-column derivatization, detected using a fluorescence detector, and quantified using the internal standard method. The linear range of the method for detecting the sulfonamides was from 2.5 to 800 μg/L, and the relative coefficients were all above 0.9934. The mean recoveries across spike levels varying from 2.5 to 200μg/kg were between 88.9% and 98.6% with RSDs less than 6.96%. The limits of quantification for the sulfonamides were 2.5-20μg/kg. The method exhibited good repeatability, high sensitivity, little interference and was widely suitable for the determination of sulfonamide residues in aquatic products.
Determination of Methylmercury in Aquatic Products by HPLC-AFS
CHEN Xue-chang,MEI Guang-ming,ZHANG Xiao-jun,ZHU Jing-ping, GUO Yuan-ming,GU Jie,ZHENG Bin
2012, 33(4):  234-237.  doi:10.7506/spkx1002-6630-201204050
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A high performance liquid chromatography-atomic fluorescence spectrometry (HPLC-AFS) method was developed for the determination of methylmercury in aquatic products. Samples were extracted with a mixture of vitriol, potassium chloride and hydrochloric acid. Then the extract was cleaned up on an SPE column, diluted with the HPLC mobile phase and filtrated through a 0.45 μm pore size membrane prior to HPLC-AFS analysis. The quantification of methylmercury was carried out using the external standard method. Good linearity between chromatographic peak area and methylmercury concentration ranging from 2 to 50μg/L was found (R2=0.9995). Average recoveries for methylmercury in different blank aquatic products spiked at 20, 200 ,1000μg/kg were 80.2%-87.1% with relative standard deviations (RSD) between 3.4% and 6.8%. The method exhibited a detection limit of 20μg/kg. The method had the advantages of simplicity and little matrix interference, and meanwhile its precision and accuracy could meet the requirements for the analysis of methylmercury in aquatic products.
Packaging & Storage
Influence of 1-MCP on Dielectric Properties of Kiwifruit at Different Maturities
TANG Yan,DU Guang-yuan,ZHANG Ji-shu
2012, 33(4):  238-242.  doi:10.7506/spkx1002-6630-201204051
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In this study,  Hayward, kiwifruit at the appropriate harvest (maturity I, with a TSS of 6.2%) and late harvest (maturityⅡ, with a TSS of 8.8%) was used to investigate the effect of 0.5μL/L 1-methylcyclopropene (1-MCP) on postharvest electric properties of fruits at room temperature (20 ℃). Kiwifruits at maturity I revealed a remarkable increased in impedance (Z) at the frequency of 1 MHz when compared with those at maturity Ⅱ and a significant difference in Z value began appearing on storage day 7 (P <0.05). The same results were observed for capacitance in the parallel equivalent circuit mode (Cp) at 10 kHz. 1-MCP inhibited the decrease of Z value in kiwifruit with prolonged storage period at 0.1 kHz or 1 MHz. 1-MCP-treated kiwifruit presented a significantly higher Cp at 10 MHz than the control. However, inductance in parallel equivalent circuit mode (Lp) and impedance phase angle (θ) had insensitive response to fruit maturity and 1-MCP, and consequently was not a measure of maturity and 1 MHz treatment or not.
Analysis of Spoilage Ability of Dominant Spoilage Bacteria from Stored Chilled Cyprinus carpio and Oreochromis niloticus
XU Zhen-wei,LI Xue-ying,YANG Xian-shi,GUO Quan-you,JIANG Chao-jun
2012, 33(4):  243-246.  doi:10.7506/spkx1002-6630-201204052
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Sensory quality, the growth kinetic parameters of spoilage bacteria and the yield factor of metabolic products, YTVBN/CFU, were assayed on sterile Cyprinus carpio and Oreochromis niloticus tissue blocks inoculated with spoilage bacteria during chilled storage. The spoilage ability of two dominant spoilage bacteria, Pseudomonas spp. and Shewanella putrefaciens, were analyzed on Cyprinus carpio and Oreochromis niloticus stored aerobically under chilled conditions. The post-inoculation shelf-lives of sterile Cyprinus carpio tissue blocks inoculated with Shewanella putrefaciens and Pseudomonas putida were 132  h and 162 h, respectively, the TVBNs 27.12 mg/100 g and 22.51 mg/100 g, the bacterial counts 8.96 lg(CFU/g) and 9.07 lg(CFU/g) and the YTVBN/CFU values 9.28 × 10-9 mg TVBN/CFU and 1.81 × 10-8  mg TVBN/CFU. The post-inoculation shelf-lives of sterile Oreochromis niloticus tissue blocks inoculated with Pseudomonas fluorescens and Shewanella putrefaciens were 132 h and 144 h, respectively, the TVBNs 23.46 mg/100 g and 24.30 mg/100 g, the bacterial counts 8.83 lg(CFU/g) and 9.12 lg(CFU/g) and the YTVBN/CFU values 1.67 × 10-8 mg TVBN/CFU and 9.10 × 10-9 mg TVBN/CFU. Based on the microflora changes and the role of the spoilage bacteria during chilled storage of the two species of cultured fish, it can be preliminarily concluded that the special spoilage organisms of stored chilled Oreochromis niloticus and Cyprinus carpio was Pseudomonas spp and that the spoilage ability of Pseudomonas spp and Shewanella putrefaciens is strong.
Effects of Microwave Blanching Conditions on POD Activity of Pleurotus eryngii
YAN Qi-mei,NIU Li-ying,TANG Ming-xia,WANG Jian-hua,LI Da-jing,JIN Bang-quan,LIU Chun-quan
2012, 33(4):  247-251.  doi:10.7506/spkx1002-6630-201204053
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The effects of microwave treatment on the peroxidase (POD) activity of Pleurotus eryngii were investigated and compared with those of normal blanching method, boiling water blanching and steam blanching. In order to obtain optimal microwave treatment conditions for blanching Pleurotus eryngii, response surface methodology was employed to construct a quadratic regression model describing the effects of microwave power and treatment time on the residual activity of POD in Pleurotus eryngii. The optimal conditions for inactivating POD were microwave treatment for 59 s at a 570 W power. Under these conditions, a small amount of free amino acids was lost, and the sensory quality of Pleurotus eryngii remained good.
Effect of Modified Atmosphere on Browning and Bioavailability of in vitro Digests of Pleurotus nebrodensis
LI Xi-hong,XUE Ting,LI Yuan-yuan,TANG Yao
2012, 33(4):  252-256.  doi:10.7506/spkx1002-6630-201204054
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In order to gain insight into the effect of positive modified atmosphere on the browning and polysaccharide bioavailability of Pleurotus nebrodensis, such physiological and biochemical indexes as oxygen and carbon dioxide concentrations, color difference, polyphenol oxidase (PPO) activity and polysaccharide bioavailability were measured on Pleurotus nebrodensis modified atmospheric packaged with PVC or PE films of different thickness (0.03 or 0.05 mm)or microporous film (0.015 mm) at regular time intervals during 28 days of storage at 4 ℃ and 95% relative humidity. A low-oxygen, high-carbon dioxide stable environment composed of 0.3%-2.1% O2 and 6%-10.3% CO2 was formed by 0.05 mm thick film on storage day 7 and could keep for 21 days. The environment could delay the occurrence of the PPO activity peak, inhibit the increase of PPO activity, and maintain polysaccharide bioavailability during the early part of the storage period. Different packages had no significant difference in their effect on the color of Pleurotus nebrodensis. Consequently, modified atmosphere packaging with 0.05 mm thick film could inhibit the browning of Pleurotus nebrodensis well, reduce the loss of nutrients and extend the storage life of Pleurotus nebrodensis.
Processing Technologies for Ready-to-Eat Litopenaeus vannamei and Changes in Its Properties during Storage
CUI Hong-bo,XUE Yong,SU Wei,XUE Chang-hu
2012, 33(4):  257-261.  doi:10.7506/spkx1002-6630-201204055
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Key processing techniques for producing long lasting ready-to-eat Litopenaeus vannamei products were investigated. #br# In addition, the changes in texture properties, the contents of protein, free amino acids and astaxanthin, TBA, and microstructure of ready-to-eat Litopenaeus vannamei were measured during storage. The storage life of ready-to-eat Litopenaeus vannamei produced by steaming, curing and high pressure steam sterilization at 115 ℃ was up to more than 30 days at 40 ℃. The texture of Litopenaeus vannamei deteriorated obviously during storage and the changes were associated with the decomposition of proteins and structural damage of muscle fibers. Moreover, lipid oxidation could cause the decomposition of astaxanthin and changes in the color of Litopenaeus vannamei.
Screening of Optimal Ethanol Extracts of Chinese Herbal Medicines for Preserving Strawberry and Effectiveness Evaluation
LI Hai-yan,LI Hui
2012, 33(4):  262-266.  doi:10.7506/spkx1002-6630-201204056
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The optimal single and combined ethanol extracts of Chinese herbal medicines inhibiting the main postharvest pathogens of strawberry were screened and the optimal concentrations of three selected ethanol extracts when used combinatorially were determined using orthogonal array design to be 1 g/L for both Flos Caryophylli and Fructus Cnidii and 1.5 g/L for Fructus Psoralea. The fresh-keeping effects of Flos Caryophylli ethanol extract, carbendazim as a chemical preservative and the best combination of three selected ethanol extracts on strawberry were compared. The results showed that various preservative groups could the weight loss rate and decay rate of strawberry and reduce the decrease of soluble solid and vitamin C contents. Moreover, the combination of Flos Caryophylli, Fructus Cnidii and Fructus Psoralea was superior to Flos Caryophylli and carbendazim in terms of physicochemical properties of treated strawberry. 
Partial Biochemical Properties of Scallop (Patinopecten yessoensis) Mince during Frozen Storage
WANG Xiao-li,ZHU Bei-wei,DONG Xiu-ping,ZHENG Jie,CHEN Zhao,LIU Gui-yang
2012, 33(4):  267-270.  doi:10.7506/spkx1002-6630-201204057
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The changes of biochemical properties, including the salt extractable protein content, Ca2+-ATPase activity, Ca2+-Mg2+-ATPase activity and the contents of total and active sulfhydryl groups, of scallop (Patinopecten yessoensis) mince during frozen storage (-18 or -35 ℃) were investigated. The results showed that the protein denaturation was very serious after 5 months of storage at -18 ℃. The solubility in salt solutions, Ca2+-ATPase and Ca2+-Mg2+-ATPase activity, total and sulfhydryl group contents of actomyosin decreased to 11.28%, 20.31%, 30.36%, 68.49% and 83.67% of their original values after 5 months of storage at -18 ℃ and to 60.01%, 45.25%, 48.17%, 82.80% and 88.71% after 10 months of storage at -35 ℃, respectively. Under each temperature condition, all the parameters showed a downward trend with prolonged storage period and decreased less at -35 ℃ than at -18 ℃. Therefore, -35 ℃ was more suitable for storing scallop mince than -18 ℃.
Correlations between Browning Degree and PPO or POD Activity of Dajiao Banana (Musa paradisiaca ABB cv. Dajiao) and Preliminary Identification of Browning Substrates during Postharvest Ripening
BAI Yong-liang,YU Ming,YUAN Gen-liang,DU Bing,LU Wang-wang,HUANG Shou-yao,YANG Gong-ming
2012, 33(4):  271-275.  doi:10.7506/spkx1002-6630-201204058
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The variation regularity of browning degree (BD), polyphenol oxidase (PPO) and peroxidase (POD) of Dajiao banana (Musa paradisiaca ABB cv. Dajiao) was observed and compared with other two banana varieties, Fenjiao and Cavendish. Meanwhile, the role of total and free phenol contents in the browning of Dajiao banana was investigated. BD indicated a progressively increasing trend in the three varieties of banana during postharvest ripening, and Fenjiao and Cavendish browned significantly faster than Dajian after the 13th day of storage, suggesting that Dajiao was more suitable for deep processing. In addition, Dajiao exhibited low PPO and POD activities and low free phenol content but high total phenol content and consequently browned slowly, demonstrating an association between the BD and PPO or POD activities and a negative correlation between the browning rate and free phenol content of Dajiao. The correlation coefficients between BD and PPO or POD activities were 0.8789 and 0.9240, respectively. Thus, there is a close correlation between the browning potential and PPO or POD activities of Dajiao. The main browning substrates in Dajiao were gallic acid and epicatechin as preliminarily identified using UV-VIS absorption spectroscopy and HPLC.
Effect of Low Temperature Conditioning on Chilling Injury and Energy Status in Cold-Stored Peach Fruit
ZHAO Ying-ying,CHEN Jing-jing,JIN Peng,YUAN Ruo-xi,LI Hui-hui,ZHENG Yong-hua
2012, 33(4):  276-281.  doi:10.7506/spkx1002-6630-201204059
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The effects of low temperature conditioning (LTC) on chilling injury and energy status in peach fruit were investigated. Peach fruit were pre-conditioned at 12 ℃ for 6 d and then stored at 0 ℃ for 30 d. Fruit browning index, firmness, extractable juice rate, the activities of mitochondria respiratory metabolism-related enzymes H+-ATPase, Ca2+-ATPase, succinic dehydrogenase (SDH) and cytochrome C oxidase (CCO), ATP, ADP and AMP contents, and energy charge were determined during storage at five-day intervals. The results indicated that LTC treatment effectively inhibited the decrease of H+-ATPase and Ca2+-ATPase activities, maintained higher activities of SDH and CCO and higher contents of ATP and ADP and energy charge, retarded the accumulation of malonaldehyde (MDA) and the increase in membrane permeability, delayed the decrease of extractable juice rate, and inhibited the increase of browning index. These results suggest that LTC treatment may maintain high energy status by regulating the activities of mitochondria respiratory metabolism-related enzymes, thereby delaying membrane lipid peroxidation and preventing the development of chilling injury of cold-stored peach fruit.
Technology Application
Preparation of Acetylcholinesterase Biosensor Based on Functionalized Multi-walled Carbon Nanotubes for Pesticides Detection
SUN Xia,ZHAO Wen-ping,LIU Zhong-he,WANG Xiang-you
2012, 33(4):  282-286.  doi:10.7506/spkx1002-6630-201204060
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This paper describes the use of functionalized multiwalled carbon nanotubes (FCNTs) based conductive polymer for designing acetylcholinesterase (AChE) biosensor. Transducers were obtained by directly dropping the sol-gel solution formed from FCNTs, chitosan (CHIT) and glutaraldehyde (GTA) on the surface of glassy carbon electrode (GCE). Acetylcholinesterase (AChE) as bio-recognizer was immobilized onto a CHIT membrane to recognize pesticides selectively. Before the detection, the CHIT enzyme membrane was quickly fixed on the surface of FCNTs-CHIT-GTA/GCE with O-ring, and thus a sensitive, fast and stable amperometric sensor for quantitative determination of organophosphates (OP) was developed. The electrochemical behavior of AChE-FCNTs-CHIT-GTA/GCE was studied and the results showed the FCNTs-CHIT-GTA promoted electron-transfer reactions at a low potential and catalyzed the electro-oxidation of thiocholine, thus increasing detection sensitivity. Based on the inhibition of OP on AChE activity, using dichlorvos as a model pesticide, the biosensor had good linearity in the concentration range 25-50 ng/L and 50-100 μg/L with a correlation coefficient of 0.9995 and 0.9991, respectively. The detection limit was 20 ng/L. The biosensor exhibited high sensitivity and good reproducibility and stability, and it was suitable for trace detection of OP pesticide residue.
Process Optimization for Production of Nutritional Seasoning Juice from Leftover Pickle Juice from Making Low
LEI Lan-lan,WU Zu-fang,WENG Pei-fang
2012, 33(4):  287-291.  doi:10.7506/spkx1002-6630-201204061
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In order to avoid the problem of environmental pollution caused by the salty wastewater left over from the production of pickled mustard tuber, a novel nutritional seasoning juice was developed based on its membrane separation, vacuum concentration and pasteurization. The results showed that the optimum operating conditions were determined as follows: ultrafiltration separation using a 0.22 μm membrane, vacuum concentration at 65 ℃ and 0.090 MPa and water-bath sterilization at 90 ℃ for 10 min. The nutritional seasoning juice obtained was clear and bright in color and had a strong aroma of pickled mustard tuber with a light sauce fragrance and a good sweet/salty balance of flavor, thus providing an excellent seasoning for cold dishes and noodles.
Development and Nutritional Evaluation of Compound Rice Bran Protein Powder
LIU Ying,TIAN Wen-juan
2012, 33(4):  292-295.  doi:10.7506/spkx1002-6630-201204062
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A kind of compound rice bran protein powder has been developed from rice bran protein powder and milk powder according to protein complementarity principles, and its nutritional values was assessed by rat feeding and metabolism experiments. The results showed the nutritional value of rice bran protein was improved greatly. The correction PER, true digestibility (TD), biological value (BV) and net protein utilization (NPU) of the compound protein power were 2.45, (89.12 ± 1.43)%, 79.34 ± 1.36, (67.53 ± 1.24)% respectively, which were much higher than neat milk protein and very similar to casein protein . The compound rice bran protein powder can offer high protein nutritional products with a nice blend of proteins of plant and animal origin.
Development of Functional Jelly Using Tibetan Hulless Barley β-glucan as Main Matrix Material
YANG Wen-yu,JIANG Chun-yan,YAN Dong,YANG Xin-yu
2012, 33(4):  296-300.  doi:10.7506/spkx1002-6630-201204063
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The product formulation and preparation process for a jelly with lipid-lowering function using Tibetan hulless barley β-glucan (THBG) as main matrix material were investigated in this study. THBG, gelatin and glycerin was found to be the optimal jelly matrix components among 12 formulations in terms of sensory and texture properties, and the optimal jelly matrix composition was 5% THBG, 0.5% gelatin and 5% glycerin in terms of gel strength, viscosity and water-holding capacity as determined using orthogonal array design. Additives such as hawthorn extract, licorice extract and sugar were added to the matrix at concentrations of 1.5%, 0.5%-2.5% and 8.0%, respectively. The jelly obtained was a safe functional product with characteristics of good taste, no choking hazard and good meltability in the mouth.