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15 March 2009, Volume 30 Issue 6
Optimization of Extraction Conditions of Total Flavonoids from Lotus Leaves by Plackett-Burman Design and Response Surface Analysis
YANG Ji-yan,HU Lei*,XU Yang
2009, 30(6):  29-33.  doi:10.7506/spkx1002-6630-200906001
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On the basis of single-factor tests, some factors affecting the extraction rate of total flavonoids from lotus leaves were firstly evaluated by Plackett-Burman design, and then the extraction conditions were optimized by response surface analysis. The results showed that the optimal extraction conditions are as follows: ethanol concentration 67%, ratio of ethanol solution to raw material 34∶1 and extraction times 3. Under the above conditions, the predicted value of extraction rate of total flavonoids is 3.19% and its experimental value is 3.17%, which indicated that the combination of Plackett-Burman design and response surface analysis can well optimize the extraction technology of total flavonoids from lotus leaves.

Study on Optimization of Extraction Technology of Resveratrol from Peanut Root by Response Surface Methodology
ZHANG Chu-shu,YU Shan-lin,PAN Li-juan,YANG Qing-li*
2009, 30(6):  34-38.  doi:10.7506/spkx1002-6630-200906002
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To optimize the extraction technology of resveratrol from peanut root, response surface methodology was applied on the basis of single factor tests. The results showed that ethanol concentration, temperature and extraction time significantly affect the resveratrol extraction, and after optimization, they are 65%, 52 ℃ and 39 min, respectively. Under these conditions, the resveratrol yield is 0.012%. In conclusion, the optimization of extraction technology of resveratrol from peanut foot by response surface methodology is feasible, and the extraction technology has practical application value.

Synthesis of Carboxymethyl Chitosan by Phase Transfer Catalytic Method and Its Characterization
XIAO Yu-liang,LI Yu-qin,XIA Cheng-cai,YOU Gui-rong,HAN Jun-fen,DUAN Gui-yun,ZHANG Hai-xia
2009, 30(6):  39-42.  doi:10.7506/spkx1002-6630-200906003
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In this study, preparation of carboxymethyl-chitosan (CMC) with phase transfer catalyst was described. Firstly, the effects of carboxymethylation conditions on the degree of substitution (DS) and solubility of CMC were investigated, and the optimum catalyst, reaction temperature, reaction time, volume ratio of water to alcohol are 6% of triethylbenzylammonium (TEBA), 55 ℃, 4 h and 1:4, respectively. Under these conditions, the DS and the solubility of CMC reach 1.147 and 98.87%, respectively. Then the chemical construction of CMC was characterized by Fourier-transformed infrared (FTIR) and X-ray photoelectron spectroscopy (XPS). The results showed that the carboxymethylation mainly occurs on hydroxy group in C6 site of chitosan.

Effects of Superfine Comminution Technique on Leaching Rates of Quercetin and Kaempferol in Pollen of Brassica campestris
YAO Qiu-ping1,MA Ya-li2,LI Jian2,HUANG Yi-fan2,*
2009, 30(6):  43-45.  doi:10.7506/spkx1002-6630-200906004
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In this study, superfine comminution technique was applied to destroy the spore wall of the pollen of Brassica campestris, and then the leaching rates of quercetin and kaempferol in superfine and common powdered pollens were compared by HPLC. The results showed that the leaching rates of quercetin and kaempferol in superfine pollen are higher 45.16% and 27.86% than those in common powdered pollen, respectively. In conclusion, superfine comminution technique can effectively promote the leaching rates of effective components in the pollen of Brassica campestris.

Study on Alcohol Extraction Technology of Trigonelline from Pumpkin Flesh
XU Ya-qin1,LIU Chun-sheng2,CUI Chong-shi1
2009, 30(6):  46-48.  doi:10.7506/spkx1002-6630-200906005
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In this study, alcohol was used to extract trigonelline from pumpkin flesh. On the basis of single factor tests, the orthogonal test of L9(34) was conducted to optimize the extraction process of trigonelline. The results showed that the optimum extraction process is as follows: extracting pumpkin flesh at 60 ℃ for 8 h with 50% alcohol solution at the material to liquid ratio of 1:20 (g/ml), and under these conditions, the extraction yield of trigonelline is up to 297.4 μg/g.

Study on Determination Methods and Extraction Process of Total Flavonoids in Leaves of Ilex latifolia
KUANG Chun-tao,LI Xiang-zhou,WANG Yu-xia,LIU Shen,WU Bin
2009, 30(6):  49-51.  doi:10.7506/spkx1002-6630-200906006
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The content of total flavonoids in leaves of Ilex latifolia Thunb. were determined using aluminum chloride method and aluminum nitrate-sodium nitrite method. The experimental results showed that the determination results of content of total flavonoids by the two methods are different from each other. The analysis on mechanism of color development of two methods indicated that the aluminum chloride method is suitable for the determination of total flavonoids in leaves of Ilex latifolia Thunb.. The relative standard deviation of precision is 2.2%. The spike recovery rates are from 90.7% to 109.5% and their average value is 97.8%. The extraction process of total flavonoids from leaves of Ilex latifolia Thunb. was optimized by means of orthogonal test design. The results showed that the extraction rate of total flavonoids is 0.68% under the optimal conditions of ratio of extractant to raw material 12:1, taking 60% ethanol as extractant, extraction time 2 h and extraction times 2.

Extraction and Antioxidant Activity of Total Flavonoids from Stem of Wedelia trilobata L.
ZHU Hui1,MA Rui-jun1,WU Shuang-tao2,PANG Qi-yin1
2009, 30(6):  52-56.  doi:10.7506/spkx1002-6630-200906007
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The extraction technology of total flavonoids from stem of Wedelia trilobata L. and its oxidation resistance were investigated. The results showed that the optimum extractant, liquid-solid ratio, temperature, ultrasonic wave power, ultrasonic wave treated time for extraction are 70% ethyl alcohol, 1:25, 50 ℃, 210 W and 20 min, respectively, and the obtained total flavonoids content from stem is 4.1%. Moreover, with three mass concentration gradients, the average maximum clearance rates of the extract to ·OH and O2· are 20.16% and 41.59% respectively, especially its maximum inhibitory rate to H2O2 reaches 55.22%. With the storage time extending, the high concentration extract can more significantly reduce the autoxidation speed of lard. However, there is significant difference of antioxidant activity between common antioxidant BHT and the total flavonoid extract.

Study on Production Technology and Stability of Soft Capsule Shell with Pullulan as Gelatinizer
LIU Mou-quan1,KONG Mei-lan2
2009, 30(6):  57-59.  doi:10.7506/spkx1002-6630-200906008
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Using a vegetal gelatinizer, pullulan as the main material of soft capsule shell, the production technology and stability of soft capsule shell were investigated. The results showed that all conditions of disintegration time, permeability oil, oxidization of soft capsule-contained substance and conglutination of soft capsule shell made from pullulan after storage are better than that made from glutin.

Study on Microwave Extraction Technology of Water Soluble Dietary Fiber from Banana Pseudo Stem
SONG Wei-chun1,2,XU Yun-sheng2,CAO Yang1,*
2009, 30(6):  60-63.  doi:10.7506/spkx1002-6630-200906009
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In this study, the microwave extraction technology of water soluble dietary fiber from banana pseudo stem was optimized based on several single factor tests and L9(34) orthogonal test. The results showed that the optimal microwave extraction time, power, ratio of liquid to solid and pH value of extractant (water) are 2 min, 900 W, 2 ml/g and pH 4, respectively. Under these conditions, the dry yield of soluble dietary fiber reaches 9.86%, which is higher than that of 7.90% obtained by the direct hot water extraction.

Study on Ultrasonic-assisted Extraction Process of Moringa oleifera Seed Oil
YU Jian-xing1,MA Li-yi2,ZHAO Chun1,DUAN Qiong-fen2,*
2009, 30(6):  64-67.  doi:10.7506/spkx1002-6630-200906010
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In this study, ultrasonic was used in petroleum ether extraction process of Moringa oleifera seed oil. The effects of four primary factors such as petroleum ether l to raw material ratio (V/W), extraction time, extraction times and ultrasonic frequency on the extraction yield of Moringa oleifera seed oil were investigated in single factor test, and then based on the results of single factor test, orthogonal test was designed to optimized the four factors. The results showed that the optimal petroleum ether l to raw material ratio, extraction time, extraction times and ultrasonic frequency are 8:1 (ml/g), 40 min, 2 and 28 kHz, respectively. Under these conditions, the yield of Moringa oleifera seed oil is 35.85%, which accounts for 96% of the total oil content of Moringa oleifera seed.

Study on Preparation and Physicochemical Analysis of Sulphated Scallop (Patinopecten yessoensis) Viscus Polysaccharides
YU Yun-hai,ZHOU Da-yong,SUN Li-ming,YANG Jing-feng,WANG Song,ZHU Bei-wei*
2009, 30(6):  68-71.  doi:10.7506/spkx1002-6630-200906011
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The crude scallop (Patinopecten yessoensis) viscus polysaccharides (SVP) were sulphated with chlorosulfonic acidformamide method, and typical absorption peaks of polysaccharide and sulfate were shown in IR spectra of the sulfated SVP (SSVP). Two polysaccharide compositions SSVP-I and SSVP-II were obtained from the sulfated polysaccharide separated by gel-filtration chromatography with Bio-Gel P-6, and the physicochemical characteristics of SSVP-I was investigated. The results showed that the average molecular weight of SSVP-I is 5900 u, its degree of sulphate group substitution is 0.98, and its monosaccharide composition is Rha, Fuc, Ala, Xyl, Man, Gal and Glu in the molar ratio of 1.0:1.3:2.4:3.0:1.3:4.1:2.5. The anticoagulation experiment in vitro indicated that SSVP-I can prolong activated partial thromboplastin time (APTT), prothrombin time (PT) and thrombin time (TT) of human with a certain dose-effect relationship.

Study on the Extraction Technology and Dynamic Change of Flavonoids in Camellia nitidssima Leaves
HUANG Yong-lin,WEN Yong-xin*,CHEN Yue-yuan,TANG Wen-xiu,LI Dian-peng,LIU Jin-lei,WEI Xiao
2009, 30(6):  72-75.  doi:10.7506/spkx1002-6630-200906012
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Based on the results of single factor, orthogonal test design was adopted to optimize the extraction technology of total flavonoids in Camellia nitidssima leaves. With rutin as reference material, the dynamic change law of content of total flavonoids in Camellia nitidssima leave was analyzed using spectrophotometry. The results showed that the optimal extraction conditions are: using 70% ethanol as extractant, ratio of material to solution 1:50 (W/V), extraction time 2.0 h, extraction temperature 70 ℃. The content of total flavonoids in Camellia nitidssima increases fluctuatingly from January to October, reaching the highest at October.

Study on Microwave-assisted Extraction of Chlorophyll from Silkworm Feces
WANG Kun,HAI Hong*,JIN Wen-ying,WANG Xin-wen
2009, 30(6):  76-79.  doi:10.7506/spkx1002-6630-200906013
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Microwave was used for extraction of chlorophyll from silkworm feces. The extraction conditions were optimized by orthogonal test on the basis of single factor test. The results showed that the optimal extraction conditions are as follows: taking 40% ethanol as extractant, microwave irradiation time 50 s, extraction time 50 min and extraction temperature 70 ℃. Under these conditions, the extraction rate of chlorophyll is 2.684 mg/g, which is increased by 3.4 times compared with traditional organic solvent extraction method. The method has the advantages of high yield, low pollution and low energy consumption.

Optimization of Extraction Technology of Radix stemonae Polysaccharides by Response Surface Methodology
WANG Ming-yan,YANG Fan,LI Yan,MA Wei-xing
2009, 30(6):  80-83.  doi:10.7506/spkx1002-6630-200906014
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On the basis of single-factor tests, extraction temperature, ratio of hot water to crushed raw material, extraction time affecting extraction rate of Radix stemonae polysaccharides (RSP) were optimized using response surface methodology (RSM). The results showed that the optimum temperature, ratio of liquid to solid, time of RSP extraction are 83 ℃, 33:1 and 200 min, respectively. Under these conditions, the extraction rate of RSP is up to 3.74%, which is higher 11.31% than the highest one in single-factor tests.

Study on Extraction Process of Lactic Acid from Fermentation Broth with Anionic Resin
ZHENG Hui-jie1,2,LI Zhi-qiang2,HE Shan2,3,WU Zhao-liang2,ZHAO Xue-ming1
2009, 30(6):  84-88.  doi:10.7506/spkx1002-6630-200906015
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Anionic exchange resins D301G and D311 were chosen to adsorb lactic acid from the fermentation broth, and some factors such as time, fermentation broth concentration, temperature, speed, pH value, flow rate and filling amount of resin were systematically examined. By investigating the single-stage process, the optimum operation conditions were obtained as follows: 3 h, pH 3 and fermentation broth concentration 86.0 g/L. Under the above conditions, the ion exchange capacity can reach 237 mg/g. Moreover, adsorption kinetics and thermodynamics of lactic acid by special resin were also investigated. Results indicated that the adsorption isotherm corresponds with Fiendish equation Qc=KC1/n and its kinetic equation is Qt=Q0+aet/b.

Study on Compound Solvent Extraction Technology of Garlic Oil
HUANG Cheng,YIN Hong,SHEN Wu-cheng,BU Lin-song
2009, 30(6):  89-91.  doi:10.7506/spkx1002-6630-200906016
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The mixture cyclohexane and acetone was used to extract garlic oil in this study. The effects of mass ratio of cyclohexane to acetone, mass ratio of garlic to extraction solven, factors extraction temperature and time on garlic oil extraction rate were investigated. Based on single factor test, orthogonal test was conducted to optimize the above extraction conditions. The results showed that the optimal extraction conditions of garlic oil are as follows: mass ratio of cyclohexane to acetone 7:3, mass ratio of garlic to extraction solvent 1:6, extraction time 6 hours and extraction temperature 55 ℃.

Optimization of Inhibitory Conditions against Yacon (Smallanthus sonchifolius) Juice Browning
HU Yun-feng,HU Ming,XING Ya-ge,LIU Xiao-yuan,YANG Zhen
2009, 30(6):  92-96.  doi:10.7506/spkx1002-6630-200906017
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In single factor tests, the inhibitory effects of vitamin C (VC), DL- malic acid and L-cysteine (L-Cys) amounts and temperature on yacon juice browning were investigated. Based on the results of single factor tests, the optimization tests of the four factors were designed according to Box-Behnken central combination design principle, and the test results were analyzed by response surface regression. The results showed that optimal inhibitory conditions against yacon juice browning are as follows: VC amount 0.31%, DL- malic acid amount 0.30%, L-Cys amount 0.30% and temperature 89 ℃, and under these conditions the change rate of browning is 20.88%.

Optimization of Extraction Technology of Flavonoids from Peanut Hull
SUN Lan-ping,MA Long,ZHANG Bin,ZHAO Da-qing,XU Hui
2009, 30(6):  97-101.  doi:10.7506/spkx1002-6630-200906018
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This study aimed to optimize the extraction technology of flavonoids from peanut hull with ethanol as extraction solvent. By means of combination design of quadratic regression orthogonal rotation, the effects of time, temperature, ethanol concentration, ratio of liquid to solid on the extraction rate of peanut hull flavonoids were analyzed on the basis of single-factor tests. A quadric regression model on extraction conditions of flavonoids was established, and the optimum conditions were obtained. The results indicated that the extraction rate of peanut hull flavonoids is affected in turn by time, ratio of liquid to solid, ethanol concentration and temperature, and the optimum extraction time, temperature, ethanol concentration, ratio of liquid to solid are 2 h, 53 ℃, 73% and 27 ml/g, respectively. Under the above conditions, the extraction rate of flavonoids from peanut hull is up to 4.04%.

Study on Preparation of O/W MCFA Micro-emulsion and Its Characteristics
LIU Wei-lin,LIU Cheng-mei*,LIU Wei,CHEN Hong-lan,LIU Jian-hua
2009, 30(6):  102-105.  doi:10.7506/spkx1002-6630-200906019
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In this study, self-emulsification method (HLB method) was taken to prepare O/W medium-chain fatty acid (MCFA) micro-emulsions. By means of titration method, it indicated that the titration of the compound of MCFA, surfactant and cosurfactant with distilled water is the best. Through comparison of emulsification efficiency and micro-emulsion area in pseudoternary phase diagram, it was found that the optimal HLB, surfactant, Km value and co-surfactant are 15, single Tween-80, 2:1 and iso-amyl alcohol, respectively. According to the estimation of characteristics of micro-emulsion samples, the formula was optimized as MCFA, Tween-80, iso-amyl alcohol and distilled water in the mass ratios of 3:2:1:0.68. The surface tension, viscidity, conductance, particle size and zeta potential of the obtained micro-emulsion are 26.7142 mN/cm, 65.22 cP, 1.87 μs/cm, 17.3 nm and -7.14 mV, respectively, and its stability is good.

Study on Ultrasonic-assisted Extraction Technique of Polysaccharides from Different Parts of Tamarix karelinii Bge.
LI Jia,LI Guo-qing,SULTAN Ababakery*
2009, 30(6):  106-108.  doi:10.7506/spkx1002-6630-200906020
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In this study, ultrasonic is used to extract polysaccharides from different parts of Tamarix karelinii Bge..The effects of raw material to hot water ratio, soaking time in hot water, ultrasonic treatment time and power on extraction rates of polysaccharides from flowers, young leaves and stem of Tamarix karelinii Bge. were investigated. Based on the results of single factor test, orthogonal test was designed to optimize these factors. The results showed that the contents of polysaccharides in the extracts of flowers, young leaves and stem of Tamarix karelinii Bge. are 53.06, 164.90 mg/g and 48.01 mg/g, respectively when the raw materials of Tamarix karelinii Bge. were soaked in hot water at the proportion of 1:60 (W/V) for 1 hour and then extracted for 20 minutes at the ultrasonic power of 300 W. The average spike recovery in content determination of Tamarix karelinii Bge. polysaccharides is 98.25%.

Study on Extraction Process of Leaf Protein Concentrate (LPC) from Stellaria media
ZHOU Jian-jian,SHAN Yu,ZHENG Yu-hong,GUAN Fu-qin,XIA Bing*
2009, 30(6):  109-112.  doi:10.7506/spkx1002-6630-200906021
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The acid-heating extraction conditions of LPC from fresh leaves of Stellaria media were optimized in this study. The effects of solid-liquid ratio, layer number of filter cloth, temperature and time on extraction rate of LPC were investigated. Based on the results of single factor tests, orthogonal test was designed to optimize the extraction conditions of LPC. The results showed that the optimal extraction conditions are as follows: solid-liquid ratio 1:5, layer number of filter cloth 5 and heating temperature 75 ℃ and heating time 11 min. Under these conditions, the extraction rate of LPC reaches 52.08% and the yield rate is 27.17%.

Study on Separation Process and Physicochemical Characteristics of Water Insoluble Dietary Fiber from Citrus Peel
HAO Rui-juan1,WANG Zhou-feng2,LUO Hai-zhou1
2009, 30(6):  113-116.  doi:10.7506/spkx1002-6630-200906022
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In this study, alcohol was used to decolorize citrus peel powder, and then neutral water was used to separate water insoluble dietary fiber from the decolorized citrus peel powder. The separation process was optimized through orthogonal test design and the physical and chemical characteristics of obtained water insoluble dietary fiber (IDF) were investigated. The results showed that optimal separation conditions of IDF are as follows: material to water ratio (g/ml) 1:30, extraction temperature 70 ℃ and extraction time 90 min. The water holding capacity and expansion capability of IDF increase with temperature rising, but decrease with concentrations of sodium chloride solution and glucose solution declining. In neutral medium, water holding capacity and expansion capability of IDF exist, weak acidic or alkaline condition results in their increase, whereas they decrease with acidity or alkalinity increasing.

Study on Extraction Conditions of Water Soluble Polysaccharide from Citrus Skin
WANG Li-yan,JING Rui-yong,RUAN Hong-sheng,WANG Bei-yan,FANG Shu-mei,YIN Kui-de*
2009, 30(6):  117-119.  doi:10.7506/spkx1002-6630-200906023
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Based on single factor test and orthogonal test design, the effects of solid-liquid ratio, temperature and time on the extraction rate of water soluble polysaccharides from citrus skin were investigated. The results showed that temperature is the key factor affecting the extraction rate, and the optimal extraction temperature, time and solid-liquid ratio are 95 ℃, 2 h and 1:20, respectively. Under these conditions, the extraction rate is 4.99%.

Study on Effect of Addition Amount of Starter on Quality of Semi-hard Cheese
HE Jia-liang1,2,LI Kai-xiong2,*,HOU Yu-ze1,LI Xing-ke2
2009, 30(6):  120-122.  doi:10.7506/spkx1002-6630-200906024
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In production process of semi-hard cheese, starter was added at the volume ratios of 1%, 2%, 3%, 4% and 5%. And then the physicochemical indexes and sensory indexes of ripened cheese were analyzed to make clear the effect of addition amount of starter on quality of semi-hard cheese. The results showed that with the addition of starter rising, the sensory evaluation score increases firstly, and then decreases gradually, the hardness and pH value of cheese decrease gradually, but the total acidity, content of pH 4.6 soluble nitrogen, total content of free amino acid and moisture content increase gradually. With the sensory evaluation score as main index combined with other quality indexes, the optimal addition amount of starter is determined to be 2% to 3%.

Study on Enzymatic Synthesis of Ethyl Caproate in Organic Medium
ZENG Jia-yu1,2,ZHOU Xing-hui1,ZHANG Ji1,2,TANG Gong1,GAO Ya-juan1
2009, 30(6):  123-127.  doi:10.7506/spkx1002-6630-200906025
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The synthesis of ethyl caproate catalyzed by candida rugosa lipase (CRL) in organic solvents was investigated, and the effects of reaction time, organic solvent, substrate concentration, and the molar ratio of acid to alcohol on ethyl caproate synthesis were examined systematically. Moreover, the structure, purity and molecular weight of the synthesized product were also characterized by IR, GC and GC-MS. The experimental results showed that the synthesized product is ethyl caproate, its molecular weight is 144, and its purity reaches 96.91%. When the esterification is carried out with the molar ratio of acid to ethanol of 1:1.3 at 38 ℃ for 24 h by using n-heptane as reaction medium, the yield of the esterification reaches 94.6%.

Separation of ATP from Waste Beer Yeast Hydrolysate by SD3 Ion Exchange Resin
QIAO De-yang,GAN Dan
2009, 30(6 ):  128-131.  doi:10.7506/spkx1002-6630-200906026
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The dynamic adsorption and desorption of SD3 ion exchange resin to ATP were studied. The results showed that the optimum adsorption conditions of ATP are as follows: pH of waste beer yeast hydrolysate 2.0, its concentration 1.0 mg/ml, its flow rate 8.25 g/L and diameter to height ratio of column 10 (80 g of wet resin filled into the column). The optimum eluent for removing impurity is HCl solution at pH 1.5 containing 0.05 mol/L NaCl. And the optimum elution conditions of ATP are as follows: taking NaOH solution at pH 12.0 containing 0.1 mol/L NaCl as eluent and its flow rate 0.5 ml/min.

Study on Removal of Inorganic Impurities and Saccharides in Phospholipid Concentrate by Extraction Method
YU Dian-yu1,LI Hong-ling1,JIN Min2,GUO Xi-feng1,2,FENG Xiao1,*
2009, 30(6 ):  132-134.  doi:10.7506/spkx1002-6630-200906027
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In this study, phospholipid concentrate was extracted with n-hexane and ethanol to remove inorganic impurities and saccharides. The n-hexane extraction conditions are n-hexane amount 1.5 ml/g and standing time 1.5 h. The optimized ethanol extraction process through orthogonal test is adding phospholipid concentrate into absolute ethanol at the addition amount of 1 ml/g, and then stirring the mixed system by the speed of 100 r/min at 25 ℃ for 4 min. The saccharide content, yield, inorganic impurity, acetone insoluble substance content and moisture plus volatile substance of the obtained phospholipid concentrate product under the above conditions are 1.15%, 90%, 0.05%, 62.06% and 1.0%, respectively, and its appearance is clear and transparent.

Study on Rapid Determination of Adulterated Components in Milk by Charger-coupled Device Shortwave Near-infrared Spectrometer
WANG You-jun1,ZHU Da-zhou2,TU Zhen-hua1,QING Zhao-shen1,JI Bao-ping1,*
2009, 30(6 ):  135-138.  doi:10.7506/spkx1002-6630-200906028
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In this study, 25 normal milk samples without any adulterated components were collected, and then 3 groups (50 samples/group) of adulterated milk samples were prepared by addition of different concentrations of hydrolyzed vegetable proteins (HVP, 0.3 to 50 g/kg), whey powder (0.03 to 30 g/kg), and non-dairy creamer (0.03 to 30 g/kg), respectively. A chargercoupled device (CCD) near-infrared (NIR) spectrometer (600 to 1100 nm) was applied to scan the permeable reflection spectrum, the possibility of rapid detection of adulterated components in milk was investigated, and the quantitative model between NIR spectra and contents of adulterated components was constructed by partial least squares (PLS). The results showed that the correlation coefficient for HVP detection is 0.969 and its standard error of prediction (SEP) is 0.456 g/kg, thus the precision of quantitative prediction for HVP may meet the practical measurement requirement. However, when the concentrations of adulterated components are lower than 1‰, the detection of NIR is limited and the contents of whey powder and nondairy creamer cannot be accurately predicted.

Denaturing High-Performance Liquid Chromatography Coupled with Polymerase Chain Reaction for Detecting seudomonas aeruginosa in Dairy and Cosmetic Products
CAO Ji-juan1,ZENG Qiu-yue1,2,SUN Zhe-ping1,WANG Qiu-yan1,PEI Yi-jun1,ZHAO Xin1
2009, 30(6):  139-142.  doi:10.7506/spkx1002-6630-200906029
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Objective: To rapidly identify Pseudomonas aeruginosa using denaturing high-performance liquid chromatography DHPLC) coupled with polymerase chain reaction (PCR). Methods: The primers and probes for specific PCR amplification ere designed based on the reported sequence of exotoxin type A (ETA)gene of P.aeruginosa, and then the specificity, sensitivity nd stability of this method were analyzed. Results: In analysis of Pseudomonas aeruginosa and other species of Pseudomonas y this method, only P.aeruginosa can be detected, and the sensitivity is 100 CFU/ml. Conclusion: The PCR-DHPLC method s rapid, specific, sensitive and relatively simple for the identification of P.aeruginosa.

Determination of Tertiary Butyhydroquinone in Edible Oils by Ultra Performance Liquid Chromatography-Tantem ass Spectrometry
ZHANG Peng-jie,ZHANG Xian-chen,ZHANG Jing,WANG Yong*
2009, 30(6):  143-145.  doi:10.7506/spkx1002-6630-200906030
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Objective: To develop a stable and reliable method of ultra performance liquid chromatography-tantem mass pectrometry (UPLC-TMS) for determining tertiary butyhydroquinone (TBHQ) content in edible oils. Methods: TBHQ in amples was extracted with acetonitrile, eluted by the mobile phase of acetonitrile-water with reserved C18 column as the separation olumn, scanned by negative ion detection mode with electrospray ionization as joint, detected by selected reaction monitoring SRM) mode and calibrated by external standard. Result: The detection limit of TBHQ is 0.10 mg/kg, the correlation coefficient f linear calibration curve is over 0.999 in the range of 0.05 to 2.5 μg/ml, and the recovery rate is 83% to 115%. Conclusion: The ethod is of high sensitivity, low detection limit, good determination capacity and short analysis time, and can be used to ccurately determine TBHQ content in edible oil.

Extraction and Spectrophotometry Determination of Sterol in Apple Seed Oil
LIU Hai-xia1,WANG Feng1,ZHAO Yan-wu1,2, QIU Nong-xue1,*
2009, 30(6):  146-150.  doi:10.7506/spkx1002-6630-200906031
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In this study, the extraction technology of sterol from apple seed oil was confirmed by orthogonal test and quantitatively analyzed by thin layer chromatography-spectrophotometry. The results showed the optimal conditions extraction of sterol are as following: solid-liquid ratio 1:4, alkaline concentration 0.5 mol/L, saponification at 85 ℃ for 120 min, and the optimum developer solvent and color reagent for thin layer chromatography are aether: petroleum aether (3:7, V/V) and 0.02% alcoholic solution of butylrhodamin 6B, respectively. Sterol from apple seed oil represents purple band under ultraviolet lamp after TLC, and forms stabile green matter, which has the maximum absorbance at the wavelength of 660 nm, via reaction with H3PO4- H2SO4-FeCl3 color reagent. Moreover, the optimum color conditions of spectrophotometry are ethanol volume 2 ml, H3PO4- H2SO4-FeCl3 color reagent volume 2 ml, color reaction time 15 min and temperature 50 ℃. This method is easy and rapid with high precision and excellent reproducibility.

Determination of Total Alkaloids in Emilia sonchifolia Collected at Different Harvesting Time in Guangxi
ZHOU Wu-ping,LI Jun-sheng,WEI Yuan-yuan,YAN Liu-juan,LIANG Yan
2009, 30(6):  151-154.  doi:10.7506/spkx1002-6630-200906032
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Objective: To establish a method for determing total alkaloids content in Emilia sonchifolia and then determine its best harvesting time. Methods: The optimum extraction conditions were confirmed by single factor tests, and with matrine as standard, total alkaloids content was determined at the wavelength of 414 nm by UV-visible spectrophotometry. Results: The calibration curve shows good linearity in the range of 0.0021 to 0.0294 mg/ml (R2=0.9997), and the average spike recovery is 97.6% with the RSD of 0.447% (n=6). The contents of total alkaloids in chloroform extract samples of Emilia sonchifolia collected at different harvesting time are 4.31 to 13.99 mg/g, and August is considered as the best harvesting time of Emilia sonchifolia with the highest otal alkaloids content. Conclusion: The method is simple and accurate with high repeatability, and can be used for quality analysis of Emilia sonchifolia.

Determination of Galactose, Glucose, Mannose and Fructose from Tea Polysaccharides by High Performance Anion Exchange Chromatography Coupled with Pulsed Amperometric Detection
LIU Ting,ZHOU Guang-ming*,LUO Zhen-ya,XU Jin
2009, 30(6):  155-159.  doi:10.7506/spkx1002-6630-200906033
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In this study, a method of high performance anion exchange chromatography coupled with pulsed amperometric detection (HPAEC-PAD) was established for determination of galactose, glucose, mannose and fructose from hydrolyzed tea polysaccharides. METROSEP CARB 1 (150×4.0 mm)anion exchange column was used as separation column. The 4 kinds of monosaccharides were eluted by 6.0 mmol/L NaOH at 1.0 ml/min of flow rate for 45 min. Under the optimized conditions, their detection limits are 0.125 mg/L to 2.0 mg/L (injection volume 20 μl, peak height taken as quantitative analysis index). The RSDs of peak height and retention time are 5.82% to 14.19% and 2.03% to 2.26%, respectively for 7 continuous determinations of mixed solution of 20 mg/L galactose, glucose, mannose and 30 mg/L fructose. The spike recovery rates of galactose, glucose, mannose and fructose from hydrolyzed polysaccharides of green tea, Pu'er tea, oolong tea and black tea are 91.8% to 99.3%.

Direct Determination of Trace Arsenic in Flour by Suspension-sampling Hydride-generation Atomic Absorption Spectrometry
SUN Han-wen,LIU Xiao-li
2009, 30(6):  160-162.  doi:10.7506/spkx1002-6630-200906034
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A novel suspension-sampling hydride-generation atomic absorption spectrometry was proposed for direct determination of trace arsenic in flour. The experimental conditions of suspension and hydride generation affecting the intensity of arsenic signal were investigated and optimized. The satisfactory result was obtained by using 0.3% agar as a stabilizing agent, 1% citric acid as a sensitizing agent, and n-octanol as an defoaming agent. The interferences of coexisting ions were also examined. Furthermore, the reliability of the procedure was to be proved by analyzing three varieties of Chinese certified reference flours, and the results showed no significant difference (p=0.05) between the certified and determined values. The method was applied to the determination of arsenic in 5 flour samples (e.g. wheat, rice)with the detection limit of 0.239 μg/L, recovery of 95.5% to 108%, and relative standard deviation (n=3) of 0.86% to 3.02%. The proposed method in this study has the advantages of simple operation, high speed and high sensitivity.

Determination of Diphenylamine Residue in Food by HPLC
LUO Xiao-yan
2009, 30(6):  163-166.  doi:10.7506/spkx1002-6630-200906035
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Objective: An analytic method with SPE-HPLC was developed to determine diphenylamine residue in food. Method: Food was extracted with CH3OH and purified by SPE,then determined by HPLC. The chromatographic column was AQ-C18 (250 mm×4.6 mm, 5 μm), the mobile phase was methanol-0.02 mol/L NH4Ac (72:28, V/V) with the flow rate of 1.0 ml/min, and the DAD detection wavelength was 285 nm. Results: The linear range of this method is 0.050 to 10.0 μg/ml. The standard curve is well linear, and the regression equation is y=136.39x-0.13, r = 0.9999. The limit of detection is 0.10 mg/kg, the recovery is 88.0% to 100% and the relative standard deviation is less than 7.0%. Conclusion: The method is satisfying in precision, accuracy and sensitivity of determining residue of diphenylamine in food.

Determination of Dimethylamine in Sea Food by Gas Chromatography Coupled with Hydrogen Flame Ionization Detector (GC-FID)
JIA Jia,ZHU Jun-li,LI Jian-rong*
2009, 30(6):  167-170.  doi:10.7506/spkx1002-6630-200906036
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An GC-FID method for determination of dimethylamine (DMA) in sea food was developed in this study. The sea food samples were extracted with 7.5% TCA. The supernatant reacted with p-touluenesulfonyl chloride for 1 hour at 60 ℃, and the product of derivatization reaction was analyzed using GC method. The results showed that the correlation coefficient between peak area and DMA concentration in the range of 0.001 mg/ml to 2 mg/ml is 0.9998. The intra-day and inter-day precision RSDs are 2.8% and 5.0%, respectively. The limit of detection and the limit of quantification of DMA are 0.38μg/ml and 0.71μg/ml, respectively. The spike recoveries are in the range of 91.21% to 103.24%. This method has high sensitivity, and is easy-operation.

Nondestructive Determination of Total Sugar Content in Tomatoes by Near Infrared Spectroscopy
MA Lan,XIA Jun-fang*,ZHANG Zhan-feng,WANG Zhi-shan
2009, 30(6):  171-174.  doi:10.7506/spkx1002-6630-200906037
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Based on the precision of quantitative analysis models established by application of partial least squares (PLS), the effects of average and original spectra as well as 10 spectral data preprocessing methods on near infrared spectroscopy (NIRS) nondestructive determination of total sugar (TS) content in tomatoes were analyzed. The results suggested that PLS correction model based on averaged spectrum is obviously superior than that based on original spectrum, and the constant offset elimination (COE) is the best data preprocessing for NIRS nondestructive determination of tomato TS content. In 11998.9 to 7497.9 cm-1 and 4601.3 to 4256.5 cm-1 spectral region, the correlation coefficient (R) between prediction and actual values of PLS model is 0.917, the standard error of calibration (RMSEC) is 0.263%, and the standard error of prediction (RMSEP) is 0.236%. In conclusion, the average spectra and the optimized spectral data preprocessing method can effectively increase the precision of NIRS nondestructive determination of tomato TS content.

Study on Determination of Vibrio mimicus in Food by Polymerase Chain Reaction Coupled with Denaturing High Performance Liquid Chromatography (PCR-DHPLC)
ZHENG Qiu-yue1,2,CAO Ji-juan1,JIANG Dan1,LIU Shu-yan1,ZHAO Xin1,FU Jun-fan2
2009, 30(6):  175-177.  doi:10.7506/spkx1002-6630-200906038
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PCR-DHPLC was adopted as a sensitive, specific, rapid and high flux approach for the detection of food-borne pathogenic bacteria, Vibrio mimicus in this study. DHPLC was used for separating double-stranded DNA under non-degeneration temperature and for detecting the specific PCR products. Under the optimum conditions, the clustering analysis diagram of elution peaks of samples were analyzed, and the spectrum with characteristic peak of Vibrio mimicus was obtained. The results showed that PCR-DHPLC has excellent specificity and accuracy of 100% compared with the traditional technology, therefore it has extensive application value in food safety assessment.

HPLC Determination of Formononetin in Corn Silk
ZHANG Yan-qing,LU Xiao-xiang*,DONG Cai-xia
2009, 30(6):  178-179.  doi:10.7506/spkx1002-6630-200906039
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Objective: To develop an HPLC method for the determination of formononetin in corn silk. Method: Analysis was carried out by using Hypersil C18 (4. 6 mm ×250 mm, 5 μm) column with CH3OH-0.1% H3PO4 (55:45, V/V) as the mobile phase. The flow rate was 0.8 ml/min and the UV detection wavelength was set at 254 nm. Results: There is good linear relationship between integral value (Y) of peak area and formononetin reference substance concentration (X) in the range of 2.3 to 23μg/ml (r = 0.9991). The average recovery of formononetin is 96.93% with the RSD of 1.30%. Conclusion: The method is convenient and accurate, and can be used for the quality determination of corn silk.

Determination of Inosinic Acid in Animal Muscles by High Performance Capillary Electrophoresis
MA Wang1,CAI Hai-ying1,*,TAN Hua-rong2,WANG Yan-hong2
2009, 30(6):  180-183.  doi:10.7506/spkx1002-6630-200906040
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The aim of this study was to set up a capillary electrophoresis method for determining inosinic acid in animal muscles. P/ACETM MDQ high performance capillary electriphoresis (HPCE) instrument was adopted. The buffer, pH value, temperature, oltage and UV detection wavelength of HPCE were 20 mmol/L K2HPO4-NaB4O7·10H2O, 6.5, 25 ℃, 22 kV and 248 nm, espectively. The results showed that the relative standard deviation of inosinic acid in animal muscle is 1.72% and its recoveries f retro-plus and pro-plus standard preparations are 80.91% to 84.14% and 79.03% to 82.41%. This new method is convenient, apid and accurate for assaying inosinic acid in muscle flavor substance and deserved to be spread.

Rapid Analysis of Chloramphenicol Residue in Milk by Near Infrared Spectrometry
WANG Cai-yun1,XIANG Bing-ren1,*,ZHANG Wei1,WANG Zheng-wu2,CHEN Chang-yun3
2009, 30(6):  184-187.  doi:10.7506/spkx1002-6630-200906041
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In this study, a rapid determination method of chloramphenicol residue in milk was developed using near infrared NIR) transmission spectrophotometry and partial least squares (PLS). The correlation coefficient between true and predicted alues of chloramphenicol residue is 0.9893. The average recovery of prediction sets is 99.77%. This method can be used for the apid determination of chloramphenicol residue in milk.

High Performance Liquid Chromatography Analysis of Surfactin Content in Fermentation Broth of acillus amyloliquefaciens ES-2
AI Jia,LU Zhao-xin*,BIE Xiao-mei,LU Feng-xia,YUAN Yong-jun,HUANG Xian-qing
2009, 30(6):  188-190.  doi:10.7506/spkx1002-6630-200906042
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A new analysis method of surfactin content in fermentation broth of Bacillus amyloliquefaciens ES-2 by high erformance liquid chromatography (HPLC) was established. The detection of surfactin was finished in 20 minutes at 210 nm n COSMOSIL 5C18-AR-Ⅱcolumn (4.6×250 mm) using acetonitrile (containing 0.1% triflouroacetic acid)-water (containing .1% triflouroacetic acid) (60:40, V/V) as mobile phase at the flow rate of 0.84 ml/min by gradient elution. The correlation oefficient between integral peak area and concentration is 0.9998 in the range of 1 to 100 mg/L. The precision, detection limit nd spike recovery of this method is 1.5%, 1 mg/L and 91.36%, respectively.

Optimization of Separation Conditions of Theaflavins by High-speed Countercurrent Chromatography
WANG Kun-bo1,2,LIU Zhong-hua1,2,*,HUANG Jian-an1,2,LIU Fang1,2,GONG Yu-shun1,2,PAN Yu1,2,HUANG Hao1,2
2009, 30(6):  191-195.  doi:10.7506/spkx1002-6630-200906043
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In this study, high-speed countercurrent chromatography (HSCCC) was used to separate theaflavins. The optimized wo-phase solvent system, flow rate, revolution speed and injection amount of HSCCC were hexane-ethyl acetate- methanolwater- cetic acid (1:5:1:5:0.25, V/V), 2 ml/min, 700 r/min and 30 mg, respectively. The upper phase was used as the stationary hase, while the lower phase was the mobile phase of HSCCC. Under these conditions, four theaflavins including theaflavin TF1), theaflavin 3-gallate (TF2A), theaflavin 3'-gallate (TF2B) and theaflavin 3, 3'-digallate (TF3) were separated out from rude extract. Especially, two kinds of ester theaflavins, TF2A and TF2B were better separated.

Improved Flinders Technology Associates (FTA) Filter Paper-based DNA Extraction with Polymerase Chain eaction (PCR) for Rapid Detection of Listeria monocytogenes
LI Hui,ZHANG Hui-yan,MA Xiao-yan,LIU Yi,HE Yi,ZHANG Wei*
2009, 30(6):  196-198.  doi:10.7506/spkx1002-6630-200906044
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Objective: To set up a detection approach of Listeria monocytogenes based on PCR. Methods: A pair of primers ere designed with hlyA gene of Listeria monocytogenes as target sequence for its detection by improved FTA-PCR method. esults: A 136-bp DNA fragment was amplified from the primers. The sensitivity of the improved FTA-PCR method was up o 1.1 × 102 CFU/ml. Conclusion: This method is rapid, sensitive and accurate, with high specificity, which can shorten the etection time from 7 to 14 days to 1 to 1.5 days.

Catalytic Kinetic Spectrophotometric Determination of Trace Formaldehyde in Beverage
FANG Xia,HUANG Yu-gai,LI Ling-ling,CAO Lian-yun
2009, 30(6):  199-202.  doi:10.7506/spkx1002-6630-200906045
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A kinetic spectrophotometric method for determination of trace formaldehyde in beverage was proposed based on the catalytic effect of formadehyde on the discoloration reaction of azure I oxidized by potassium bromate in hydrochloric acid. The linear range is 0. 20 to 6.00 μg/ml. The method has been used to determine the formaldehyde in saled carbonated beverage and in pond water from river samples with satisfying results.

Study on Capillary Electrophoresis Determination of Citrinin in Mouldy Food
DU Jian-zhong,CHEN Hai-li,WU Jin-mei,JIANG Yang-hua
2009, 30(6):  203-207.  doi:10.7506/spkx1002-6630-200906046
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A method was set up for determination of citrinin using capillary electrophoresis. The effects of some important factors, such as running buffer type, concentration and pH value, running voltage and ethanol concentration on citrinin separation were investigated. The citrinin in extract of mouldy steamed bread sample was completely separated in 9 minutes with 10 mmol/L NaH2PO3-10 mmol/L Na2B4O7 at pH 7.0 as running buffer and 10% (V/ V) ethanol as extractant at running voltage of 15 kV. The relative standard deviations (RSDs) were more than 0.13% and 1.6% for citrinin migration time and peak area, respectively. There was good linear relationship between concentration and peak area (The correlation coefficient is 0.9969). The method is simple and accurate, and has less reagent consumption and good separation effect.

GC-MS Determination of Cuminal Content in Volatile Oil of Cuminum cyminum L.
YANG Wen-ju1, YANG Tao1, LIU Long2,YU Bo2,TIAN Shu-ge2,JING Si-qun3
2009, 30(6):  208-212.  doi:10.7506/spkx1002-6630-200906047
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In this study, the volatile oil of Cuminum cyminum L. was extracted by steam distillation method and the cuminal content in the volatile oil was analyzed using GC-MS. The Shimazu Column DB-5 (30 m×0.32 mm, 0.25 μm) was used. The injection temperature was 220 ℃, and the initial temperature of 40 ℃ was increased to 220 ℃ at the rising rate of 8 ℃/min. The helium flow rate, split ratio and injection volume were 1.2 ml/min, 100:1 and 0.5 μl, respectively. The results showed that there is good linear relationship between integral value (Y) of peak area and cuminal content (X) in the range of 7.75 to 69.75 mg/ ml, and the linear equation is Y = 3.34 × 108X - 3.373 × 106 (r =0.9989). The RSDs in precision, repeatability and stability experiments are 1.40%, 2.3% and 1.2%. The average spike recovery is 96.5% with the RSD of 1.8% (n=5). The method is simple and accurate with good reproducibility, therefore it can be used for quality control of Cuminum cyminum L..

HPLC Determination of Vitamin E Content in Highland Barley from Tibetan Plateau
ZHANG Chun-hong1,2,XU Chuan-mei1,2,DONG Qi1,HU Feng-zu1,*
2009, 30(6):  213-215.  doi:10.7506/spkx1002-6630-200906048
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In order to provide scientific basis for the quantity control and comprehensive utilization of highland barley, δ-vitamin E, γ- vitamin E , α- vitamin E contents in 16 cultivars of highland barley from Qinghai and highland barley samples from different 10 areas of Tibet were determined by HPLC. The chromatographic column, mobile phase, column temperature, flow rate and detection wavelength were Symmetry C18 column (4.6 mm × 250 mm, 5 μm), methanol-water at the volume ratio of 98: 2, 25 ℃, 1 ml/min and 295 nm, respectively. The results indicated that all the collected highland barley in Tibetan plateau contain vitamin E,and the total content is between 0.3 mg/100g and 0.8 mg/100 g, especially the average content of total vitamin E in highland barley from Tibet is higher about 10% than that from Qinghai.

Dual-wavelength Spectrophotometric Determination of Calcium in Food
WANG Yu-bao,CHEN Yu-jing*,HOU Fa-ju
2009, 30(6):  216-218.  doi:10.7506/spkx1002-6630-200906049
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In the presence of peregal, calcium reacts with arsenazo Ⅰ to form a stable purple complex in NH3-NH4Cl buffer solution (pH 9.5), and then with the measuring and reference wavelengths of 570 nm and 480 nm respectively, a new dual-wavelength dual-peak spectrophotometric method for the determination of calcium content was developed in this study. The results showed that the dual-wavelength spectrophotometer is more sensitive than the single-wavelength spectrophotometer, ε0 = 6.16×104 L/mol·cm, and the calcium content accords with Bill’s law in the range of 0 to1.3 μg/ml. The method was applied in the etermination of calcium in milk powder and glucose samples. The obtained results are satisfying.

Determination of Zn in Food by Nanometer TiO2 Separation and Concentration -Atomic Absorption Spectroscopy
LIU Hui,YANG Chun
2009, 30(6):  219-221.  doi:10.7506/spkx1002-6630-200906050
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In this study, the adsorption and desorption behaviors of nanometer TiO2 to Zn were investigated. It was found hat nanometer TiO2 has good and rapid adsorption capacity to Zn in the range of pH 9 to 11. Under the optimized experimental onditions, the static adsorption capacity of nanometer TiO2 is 15.9 mg/g. 95% Zn can be desorbed by 0.5 mol/L HNO3, and the oncentration multiple of Zn is 75. The detection limit (3σ) of Zn by atomic absorption spectroscopy is 20.15 ng/L, and the RSD f this method is 3.5% (n=10) at 10 μg/ml of Zn. The spike recoveries of Zn in tap water, pork, crucian meat, burdock and tomato re in the range of 92.5% to 105.0%.

Determination of Quinolone Residues in Royal Jelly by High-Performance Liquid Chromatography Coupled with luorescence Detector
ZHOU Ping1,HU Fu-liang2,*,XU Quan-hua1,SHAO Qiao-yun1
2009, 30(6):  222-225.  doi:10.7506/spkx1002-6630-200906051
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Quinolones (QNs) is one kind of antibiotics, and in recent years its residue exceeding limits has been found frequently n animal-origin exportation food such as bee products. In this study, liquid-liquid extraction was used to pre-treat royal jelly ample, and then five QNs residues in royal jelly sample were determined by high-performance liquid chromatography coupled ith fluorescence detector. The results showed that the detection limits of ofloxacin, enrofloxacin, ciprofloxacin, norfloxacin and anofloxacin are 5 μg/kg, 2.5 μg/kg, 2.5 μg/kg, 2.5 μg/kg and 1 μg/kg, respectively, which meet the detection demand of allowable imits of QNs in royal jelly. The proposed method is simple, rapid, accurate and low-reagent consumption and cost.

Determination of Five Rare Earth Elements in Tea by Inductive Coupling Plasma-Optical Emission Spectrometry
HUO Jiang-lian1,LIU Meng-gang2,LOU Guo-zhu1
2009, 30(6):  226-228.  doi:10.7506/spkx1002-6630-200906052
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ICP-OES was sused to establish a analysis method of five rare earth elements, such as La, Ce, Pr, Nd and Sm in tea. nder the optimum conditions, the limits of detection and the spike recoveries of the five rare earth elements at the concentration f 0.4 mg/kg and 2.0 mg/kg are excellent, which are 1.1μg/kg to 5.1μg/kg and 80.3% to 98.7% respectively. The accuracy of this ethod was evaluated using the tea standard reference material GBW10016. The determination results are in the range of certified value.

Determination of Saccharide Components and Contents in Blueberry Juice by HPLC
ZHANG Ying-chun,DONG Ai-jun,YANG Xin*,ZHANG Hua,MA Ying
2009, 30(6):  229-231.  doi:10.7506/spkx1002-6630-200906053
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Objective: To set up an examination method for determining saccharides in blueberry juice by HPLC. Method: Saccharides were extracted from samples with water using ultrasonic, and then their components and contents were determined by HPLC. Agilent Zorbax carbohydrate (4.6 × 250 mm, 5 μm) column was adopted, mobile phase was acetonitrile-water (75:25, V:V), and the flow rate was 1 ml/min. Results: The calibration curve of saccharide concentrations is well linear in the range of 0.5 to 10 mg/ml, the correlation coefficient is over 0.9989 (n=5), the RSD is 0.36% to 2.18% (n=5) in precision experiment, and the average recovery rate is 91.36% to 101.34%. Conclusion: This method is convenient, rapid and effective for separation and quantitative analysis of saccharides in blueberry juice.

Analysis of Essential oil Composition of Allium tuberosum Seed
HU Guo-hua1,CHEN Hao2,MA Zheng-zhi1
2009, 30(6):  232-234.  doi:10.7506/spkx1002-6630-200906054
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The essential oil compositions of seeds of Chinese chive (Allium tuberosum Rottl. Ex Spreng) “791”, “Pingfeng o.6” and “Pingfeng No.1”were analyzed using gas chromatography-mass spectrometry (GC-MS). The results showed hat 27 common components are identified, accounting for 92.79%, 93.00% and 92.01% of the total essential oil, respectively. Hexanal (17.74%), 10-nonadecanen-2-one (10.39%) and 2-pentyl furan (6.50%) are the main constituents of essential oil of Chinese chive“ 791” seed, which include 7 disulfide compounds, 1 tetrasulfide compound, 3 aldehyde compounds, 2 ketone compounds and 3 alcohol compounds. The total content of disulfide compounds is 32.43%.

Analysis of Nucleosides in Mycelia of Paecilomyces tenuipes
CHEN An-hui1,SHAO Ying1,FAN Mei-zhen2,WU Hai-lian
2009, 30(6):  235-237.  doi:10.7506/spkx1002-6630-200906055
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The nucleoside compositions in Cordyceps sinensis and fermentation mycelia of Paecilomyces tenuipes RCEF0441 were determined by high performance liquid chromatography (HPLC). The results showed that the nucleosides in mycelia of Paecilomyces tenuipes RCEF0441 include mainly adenosine, uridine, guanosine, inosine, cytidine and thymidine. The contents of cytidine, inosine and guanosine are about 3, 7 and 9 times of those in Cordyceps sinensis, respectively. Moreover, the contents of adenosine and uridine are obviously higher than those in Cordyceps sinensis.

Study on Quantitative Detection of Glyphosate-resistant Genetically Modified Soybean Powder by Real-time Fluorescence PCR Method
BAI Wei-bin1,2,SUN Jian-xia1,2,TRINH Quoc-linh1,LUO Yun-bo1,JIANG Gui-chuan2,HUANG Ya-dong3,*
2009, 30(6):  238-242.  doi:10.7506/spkx1002-6630-200906056
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A real-time fluorescence PCR method was developed for quantitative detection glyphosate-resistant genetically modified soybean powder. The detection results showed that the genetically modified (GM) contents of soybean powder from USA, Argentina, Brazil and China are 5.37%, 3.96%, 2.26% and 0, respectively. The sensitivity of established detection method is 0.001% and its stability is fairly good.

Limulus Amoebocyte Lysate (LAL) Assay Coupled with Gram Negative Bacteria (GNB) Count for Detecting γ-Ray-irradiated Chicken
HU Qun,ZOU Chun-ying,GUO Li-ping
2009, 30(6):  243-245.  doi:10.7506/spkx1002-6630-200906057
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Objective: To explore the availability of LAL/GNB method for screening irradiated chicken. Methods: Every 50 g of saled diced chicken was packaged into a sample and then every 12 chicken samples were irradiated byγ-ray of 0, 2 and 6 kGy, respectively. The viable GNB number in chicken sample was estimated by GNB count method, and the total number of GNB was estimated according to bacterial endotoxin concentration. The difference in the two numebers was used to judge if chicken sample had been irradiated or not. Results: In the 6 kGy-dose group, all 12 samples were detected to be irradiated. In the 4 kGydose group, 8 samples were detected to be irradiated, except 4 samples. In the control group, all 12 samples were detected to be not irradiated. Conclusion: The LAL/GNB method is available for detecting irradiated chicken.

Effect of Low-oxygen Storage on Fatty Acid Oxidation of Korea Pine Nut Kernel at Ambient Temperature
LI Peng-xia1,WANG Wei1,HUANG Kai-hong1,LIANG Li-song2,WANG Gui-xi2,*
2009, 30(6):  246-249.  doi:10.7506/spkx1002-6630-200906058
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In this study, the changes of fatty acid oxidation in nut kernel of Korea pine (Pinus koraiensis Sieb. et Zucc.) which were stored in air or air-tight container containing 2%±1%, 5%±1% or 10%±1% O2 for 180 days at ambient temperature (20 to 30 ℃) were investigated. The results showed that total fat, iodine value of Korea pine nut kernel decrease but the acid value, peroxide value, saponification value increase during storage. Low O2 concentration is effective to slow down the decrease of fat content. After 180 days of storage, the Korea pine nut kernel stored in low O2 environment has lower acid value and peroxide value but higher iodine value compared with that stored in air. Furthermore, 2% O2 can inhibit the rise of saponification value of Korea pine nut kernel effectively. All these indicated that low O2 storage can inhibit fat acid oxidation of Korea pine nut kernel, and is beneficial to its storage quality. 2% O2 storage has the best effect.

Effects of Nitric Oxide Fumigation on Postharvest Quality and Antioxidant Enzymes of Brassica alboglabra Bailey
DAN Yang1,2,WU Cheng-yong2,LIN Jie2,HUANG Xiao-fang2,CHEN Bin2
2009, 30(6):  250-254.  doi:10.7506/spkx1002-6630-200906059
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In order to determine the proper fumigation time of nitric oxide (NO), the change tendencies of NO concentration from 60 μl/L and 100μl/L were investigated in the presence of Brassica alboglabra Bailey. Furthermore, the effects of NO concentrations of 60 μl/L and 100 μl/L on postharvest weight loss, flowering ratio, yellowing ratio of leaves and anti-oxidation enzymes were also investigated. The results showed that the proper fumigation time of NO is 30 minutes. The presence of Brassica alboglabra Bailey can control the accumulation of NO2, which is the product of NO oxidation. The fumigation of NO could effectively inhibit the flowering ratio and the yellowing ratio of leaves of Brassica alboglabra Bailey, but has no effects on the postharvest weight loss. Moreover, the fumigation of NO could control the activity decreases of SOD and CAT and the increase of MDA content.

Chemical and Physiological Changes of Agrocybe chaxingu Huang during Controlled Atmosphere Storage with Silicon Gum Film Window
LI Tie-hua1,2,ZHANG Min2
2009, 30(6):  255-259.  doi:10.7506/spkx1002-6630-200906060
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Agrocybe chaxingu Huang were stored in the packages with or without silicon gum film window in different controlled atmospheres (10% O2, 10% CO2, 80% N2 or 10% O2, 15% CO2 and 75% N2) at 3 ± 1℃. Then changes of gas composition in the packages, respiration rate, ascorbic acid content, total acid content, soluble solid content, conductivity and protein content were examined. The results showed that there are significant differences in all examined parameters between the packages with and without silicon gum film window. Compared with the package without silicon gum film window, the package with silicon gum film window are highly effective for quality preservation of stored mushrooms because silicon gum film window has good gas exchange ability to keep the gas compositions in the package relatively stable and avoid the occur of anaerobic respiration. Moreover, the initial gas concentration also has some effects on quality preservation of mushrooms during storage. In conclusion, with 10% O2, 10% CO2 and 80% N2 as the initial gas concentrations, the package with silicon gum film window can keep O2 concentration above 1.5% and CO2 concentration under 12.6% during the whole storage period, which are the optimal conditions for the storage of Agrocybe chaxingu Huang.

Study on Formula Optimization of Compound Preservative of Chilled Pork
LI Zeng-li,JIANG Li-ke*,WANG Hong-mei
2009, 30(6):  260-263.  doi:10.7506/spkx1002-6630-200906061
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In this study, L9(33) orthogonal test was designed to investigate the preservation effects of tea polyphenol, phytic acid and vitamin C on chilled pork. Based on the measurement of pH value, TVB-N value and microorganism indexes as well as the H2S test in chilled pork, the optimal formula of a compound preservative for chilled pork was confirmed as follows: tea polyphenol 0.75%, phytic acid 0.10%, vitamin C 0.40%. This compound preservative can may effectively improve the quality and prolong the storage of chilled pork.

Effects of Benzothiadiazole on Diseases and Quality of Postharvest Loquat Fruit
ZHANG Zi-wei,ZHU Shi-jiang*
2009, 30(6):  264-267.  doi:10.7506/spkx1002-6630-200906062
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Postharvest loquat (Eriobotrya japonica Lindley) fruits were treated with different concentrations of BTH solution and stored at normal temperature (22 ℃) or low temperature (3 ℃) for observing the occurrence of pathogenic diseases and changes in fruit quality. The results showed that BTH reduces the disease index of natural infection of loquats at normal temperature and lesion diameters of loquats inoculated with Colletotrichum acutatum. At the same time, BTH elevates the content of lignin and the activity of phenylalanine ammonia-lyase (PAL)in peel of loquat, which implies that BTH activates the defense system of postharvest loquat. Moreover, compared with the control, BTH decreases pulp firmness, increases contents of total soluble solids and titrable acids at both of normal and low temperatures, which indicates that BTH has positive effects on postharvest fruit quality.

Effects of Calcium Treatment on Physiological and Biochemical Characteristics of Fraiar Plum Fruit
ZHANG Guang-yan1,LIU Yun-qiang1,ZHANG Ping2,YANG Jian-min3
2009, 30(6):  268-271.  doi:10.7506/spkx1002-6630-200906063
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Using Fraiar plum fruit as the test material,the changes in quality and physiology characteristic of fruits treated by different concentrations (0.5%, 1%, 2% and 4%) of calcium were investigated. The results showed that the reduction of the contents of titratable acid and soluble sugar is slowdown, the increase of soluble solid content is inhibited, and the hardness of plum fruits is kept, thus calcium treatment improves the fruit quality. In addition, the accumulation of MDA content is inhibited, which keeps the cell membrane intact; the activity of POD is depressed, while the activity of SOD is enhanced, which enhance the antioxidant activity of fruits; the activity of PPO is inhibited, and the brownness, the ripening and the senescence of plum fruits are effectively lingered. Therefore the calcium treatments prolong the storage duration of fruits, especially 1% CaCl2 presents the optimum protection effects.

Study on Effects of High Intensity Pulsed Electric Field on Antioxidant Substances in Postharvest Garlic
LI Ting-ting1,SONG Shu-yao1,*,CHI Yan-ping2
2009, 30(6):  272-274.  doi:10.7506/spkx1002-6630-200906064
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The effects of high intensity pulsed electric field (HIPEF) treatment at 1.7 kV/cm for 5 min or at 1.7 kV/cm for 10 min on vitamin C content, total flavonoid content, superoxidae disumutast (SOD) activity and polyphenol oxidase (PPO) activity in garlic were investigated. The results showed that HIPEF can restrain the degradation of vitamin C and total flavonoids, enhance the SOD activity, inhibit the enzymatic browning of garlic to some extent, and well keep the quality of postharvest garlic during storage. Especially, the 5-min HIPEF treatment has better effect than 10-min treatment.

Effects of Pre-cooling Delay and Different Packaging Treatments on Quality of “Bayuecui” Peach Fruits in Model Condition of Cold-chain Transportation and Shelf-life
ZHAO Xiao-fang1,2,WANG Gui-xi1,*,LIANG Li-song1,ZHU Mei-yun2
2009, 30(6 ):  275-278.  doi:10.7506/spkx1002-6630-200906065
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Effects of pre-cooling delay and different packaging treatments on firmness, soluble solid content (SSC), peel and pulp color, weight loss rate, rot rate and internal browning of “Bayuecui” peach fruits after 15-day storage at - 0.5 to 0 ℃ and subsequent 3-day shelf-life at 25 ℃ were investigated, respectively. The results showed that firmness and SSC of peach fruits in wrapping paper plus carton (X1) and net-cover plus gift box (X2) do not significantly change during low tenperature storage, non-packed peach fruits (X3) are easy to lose water, and the rot rate of peach fruits in X1 is clearly higher than that of peach fruits in X2 and non-packed peach fruits. During 3-day shelf-life, the peach fruits in X2 keep higher firmness (11.45 N) and SSC (9.99%) than those in X1, lower rot rate and water loss rate, their color is sufficient on the surface, and also the internal browning is slight. For the peach fruits subjected to pre-cooling after 6-h (compared with 12-h and 18-h) post-harvest storage, their firmnesses after 5-day storage at -0.5 to 0 ℃ subsequent 3-day shelf-life at 25 ℃ are both higher, but the rot tate and water loss rate are both lower, and their color is sufficient and light red on the surface without browning pit. Assessed generally, the peach fruit should be pre-cooled in 6 h after harvest and packaged with net-cover plus gift box during storage and transportation.

A New Beer Clarificant: Carrageenan Effervescent Tablets
WANG Jia-liang,ZHAO Da-qing,WANG Yong-bin
2009, 30(6):  279-281.  doi:10.7506/spkx1002-6630-200906066
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Objective: To investigate a kind of new beer clarificant. Method and Results: The low-temperature air drying technology of carrageenan effervescent tablets was optimized by single factor tests as follows: drying-temperature 45 ℃ and drying-time 6 h. Then the formula of effervescent tablets was optimized by orthogonal test as follows: effervescent 20%, carragenan 30%, citric acid and NaHCO3 mixture (citric acid:NaHCO3=1:1) 20%, PEG6000 2.5%. Conclusion: The addition of effervescent tablets after wort boiling can improve wort appearance, quicken wort filtration rate, save diatomite and electricity consumption. All physiochemical indexes of beer product fit the relative national standards.

Study on Fermentation Technology of Pyracantha fortuneana Fruit Vinegar
ZHOU Wen-bin,WANG Chong-jun,GAN Xiao-hua
2009, 30(6):  282-284.  doi:10.7506/spkx1002-6630-200906067
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Pyracantha fortuneana fruit vinegar was produced from Pyracantha fortuneana fruits by the procedures of clearing, crushing, filtration, composition adjustment, alcohol fermentation, pasteurization, acetic acid fermentation, canning and second pasteurization. The orthogonal test results showed that the optimum initial sugar, initial pH value, inoculation quantity of yeast, temperature and fermentation time in alcohol fermentation is 18%, 6, 0.6%, 28 ℃ and 3 d, respectively; the optimum initial alcohol concentration, initial pH value, temperature and inoculation quantity of acetic acid bacteria in acetic acid fermentation are 7%, 7, 32 ℃, and 12%, respectively. Under the above conditions, the acetic acid concentration of Pyracantha fortuneana fruit vinegar is up to 6.026 g/100 ml.

Development of Low-salt Sweet Calabash Pickle by Dynamic Vacuum Pickling Method
SUN Yuan-bin1,TIAN Hai-juan2,ZHU Zhu2,JIANG Wei2
2009, 30(6):  285-287.  doi:10.7506/spkx1002-6630-200906068
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In this study, sweet calabash was used as raw material to develop a low-salt sweet calabash pickle by dynamic vacuum pickling method. The pickling process was optimized via orthogonal test. And the qualities of sweet calabash products pickled by traditional method and this method were compared. The results indicated that both temperature and vacuum degree affect significantly quality of sweet calabash pickle. The optimum pickling parameters are as follows: temperature 20 ℃, vacuum degree 85 kPa, rotational speed of agitating shaft 1 r/min and salt concentration 2%. The dynamic vacuum pickling method is better than traditional pickling method in terms of sensory evaluation, edibility, edible nutrition and safety. Moreover, due to shorter processing period of dynamic vacuum pickling method, it is more suitable for mass production in practice.

Study on Stability of Formulated Sour Milk Drink with Mixed Stabilizers
LUO Ling-quan
2009, 30(6 ):  288-291.  doi:10.7506/spkx1002-6630-200906069
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On the single-factor test basis of impact of CMC-Na, locust bean gum and guar gum on the stability of formulated sour milk drink, the Box-Behnken design was used to study the compound of the three stabilizers. The results showed that the simplex critical additive volume of CMC-Na, locust bean gum and guar gum is 0.25%, 0.2%, 0.25% to control centrifugal percent of formulated sour milk drink respectively. While mixed, the proper additive volume is 0.072%, 0.042% and 0.059% respectively, total volume is 0.173%. Under these conditions, the minimum centrifugal percent of product is 2.408%.

Study on Microwave Kill Enzyme and Its Application on Processing of Non-sulfur Preserved Apricots
KANG Jian,WANG Ai-qin,GU Jing-jing
2009, 30(6 ):  292-294.  doi:10.7506/spkx1002-6630-200906070
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In order to solve the problems of high-sugar and high-sulfur existing in preserved apricots, a new processing technology and method of preserved apricots was studied. Do changes steeping sugar in several times to one time, and uses microwave kill enzyme technology to replace the past smoked sulfur color technology, and proves on microwave advantages in processing nonsulfur preserved apricots. Through orthogonal test to optimum conditions, the optimum production process parameters as follows: microwave power 600 W,fresh apricot weights 45 g, heating time 180 s. After several experiments, the results of the preserved apricot RGB color values which are determined by scanner, computer and software consistent with the sensory evaluation results.