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25 November 2013, Volume 34 Issue 22
Preparation and Immunoregulatory Activity of Acetylated Polysaccharide from the Seeds of Plantago asiatica L.
HUANG Dan-fei,NIE Shao-ping,JIANG Le-ming,XIE Ming-yong
2013, 34(22):  1-4.  doi:10.7506/spkx1002-6630-201322001
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Acetylated polysaccharide from the seeds of Plantago asiatica L. (Ac-PLP) which provides materials for studying the
structure-activity relationship of plant polysaccharides was prepared by using acetic anhydride as acetylating agent. Factors
influencing the modification reaction, such as acetic anhydride dosage, temperature and reaction time, were investigated.
The optimal reaction conditions were determined using orthogonal array design as 10% of acetic anhydride, 30 ℃ and
2.5 h. Further in vitro investigation demonstrated that Ac-PLPs with a substitution degree from 0.06 to 0.1 promoted
IL-12p70 secretion by dendritic cells and the strongest effect was observed when the degree of substitution was about 0.08.
The results in the current study reveal that acetylation can be an alternative way to modify PLPs and provide a theoretic basis
for the development of functional products with PLPs.

Ultrasonic Extraction and Composition Identification of Saponins from Aralia continentalis Leaves
FENG Ying,SUN Shi-hui,ZHAO Lin-na,FAN Wen-li
2013, 34(22):  5-9.  doi:10.7506/spkx1002-6630-201322002
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One-factor-at-a-time method and L9(34) orthogonal array design were employed to optimize the extraction process
of saponins from Aralia contenentalis leaves. The results showed that the optimal conditions of ultrasonic extraction
were determined as follows: ethanol concentration of 70%, material-to-liquid ratio of 1:50 (g/mL), extraction duration of 30 min
and ultrasonic power of 200 W. Under the optimal extraction process, the extraction yield of saponins was up to 26.78 mg/g. Macroporous
adsorption resin HPD-100, silica gel, SephadexLH-20 and preparative HPLC were used to separate the extracted
saponin and congmuyenoside A was identified by NMR.

Preparation and Immunoregulatory Activity of Carboxymethyl Polysaccharide from the Seeds of Plantago asiatica L.
JIANG Le-ming,FAN Can-mei,NIE Shao-ping,ZHOU Hua-lu,LI Jian-yu,XIE Ming-yong
2013, 34(22):  10-14.  doi:10.7506/spkx1002-6630-201322003
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Polysaccharide derived from the seeds of Plantago asiatica L. (PLP) was carboxymethylated in aqueous alkaline
medium of sodium hydroxide (NaOH) using monochloroacetic acid (MCA) as etherifying agent. The effects of reaction
parameters such as NaOH concentration, the amount of added MCA, temperature and reaction time were investigated using
single-factor and orthogonal array design. Temperature effect on the reaction was not significant. Caboxymethylated PLP
(CM-PLP) with the highest degree of substitution (DS) was obtained in 4.5 mol/L aqueous NaOH with the addition of 2.835 g
of MCA at 50 ℃. Meanwhile, CM-PLPs with high DS showed a significantly enhanced effect on IL-12p70 secretion by
dendritic cells (DCs). This study indicates a new approach to exploit the resource of PLP.

Macroporous Resin Adsorption for Purification of Hop Polyphenols from and Compositional Analysis
WANG Xu-ping,YANG Lei,YANG Xiao-lan,LUO Zheng-ming
2013, 34(22):  15-20.  doi:10.7506/spkx1002-6630-201322004
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Hop polyphenols were extracted from spent hops, purified by macroporous resin adsorption and subjected to
compositional analysis by HPLC. The results showed that the adsorption and desorption capacities of hop polyphenols on
SP850 resin were 79.8 mg/g and 78.4%, respectively, and the adsorption and desorption processes were equilibrated in a
short time, indicating the suitability of this resin for purifying the crude phenols extracted from hops. The optimal purification
conditions were loading of 6 BV of 7.3 mg/mL sample solution at a flow rate of 3 BV/h followed by washing with 5 BV
of deionized water and elution with 4 BV of 60% ethanol at a flow rate of 2 BV/h. Under the optimized conditions, the purity
of polyphenols in hop extracts was increased from 13.2% to 56.6%. The compositional analysis indicated that 55.2% of the
purified polyphenols were proanthocyanidins and 10 individual phenols were identified by HPLC, which were gallic acid,
catechin, chlorogenic acid, epicatechin, rutin, hyperoside, astragalin, resveratrol, isoquercitrin and xanthohumol

Optimization of Extraction Technique and Component Analysis of Polysaccharide from Dendrobium officinale
HUANG Xiao-jun,NIE Shao-ping,WANG Yu-ting,WANG Ya-wei,CAI Hai-lan,TIAN Fang,CUI Wu-wei
2013, 34(22):  21-26. 
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采用响应曲面法优化铁皮石斛多糖的提取工艺,并对经优化提取得到的多糖基本理化性质进行分析。结果表明铁皮石斛多糖提取的最佳工艺条件为:水料比30:1,提取温度90℃,提取时间2h,多糖得率为30.56%。铁皮石斛多糖中性糖含量为78.21%,淀粉含量为18.64%,蛋白含量为5.8%,灰分含量为1.28%,主要由甘露糖、葡萄糖组成,两者的摩尔比为5.2:1。铁皮石斛多糖富含Ca(1.07%)、Mg(0.11%)、Fe(0.0012%)、Zn(0.0039%)等元素。高效凝胶渗透色谱结果显示铁皮石斛多糖呈单一色谱峰,均一性较好。通过本方法制得的铁皮石斛多糖糖含量较高,除淀粉和蛋白外无其它含量较高的杂质成分;且该多糖均一性较好,并且富含Ca、Mg、Fe、Zn等矿物质,研究成果可为日后铁皮石斛多糖活性研究以及构效关系讨论提供基础。

Optimization of Aqueous Enzymatic Extraction of Hemp Seed Oil and Analysis of Its Fatty Acid Composition
WANG Huan,LI Yang,JIANG Lian-zhou,WANG Yan,WANG Zhong-jiang,FENG Hong-xia,FENG Dan,LIU Hai-ying
2013, 34(22):  27-32.  doi:10.7506/spkx1002-6630-201322006
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The yields of hemp seed oil from peeled hemp seeds by aqueous enzymatic extraction with Protex 6L, Protex 7L,
Alcalase 2.4L, Viscozyme L and Babaowei 2X were 3.62%, 36.88%, 17.05%, 50.98%, and 33.33%, respectively. Viscozyme L
was chosen as the best enzyme according to the oil contents in the emulsions, hydrolysates and precipitates. The enzymatic
hydrolysis process was optimized by response surface methodology to obtain maximum free oil yield. As a result, the optimal
hydrolysis conditions were determined as 7000 U/g of enzyme dosage, 60 ℃, initial pH 5, 1:6 of solid/liquid ratio and 3 h.
By using GC analysis, 11 fatty acids were detected in the seed oil, including saturated fatty acids (mainly palmitic, arachidic
and stearic acid) and unsaturated fatty acids (mainly oleic, linoleic and α-linolenic acid). Among these fatty acids, the most
abundant was linoleic acid with a relative content of 47.5%.

Effect of Rolling-Over on Overall Quality of Lentinula edodes Stipe and Process Optimization
WANG Da-wei,DAI Long,XU Xu,ZHANG Xu
2013, 34(22):  33-39.  doi:10.7506/spkx1002-6630-201322007
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Single-factor design and response surface analysis were used to explore the effects of raw material moisture
content, rolling gap and number of rolling cycles on the comprehensive quality of Lentinus edodes stipe such as adsorption
capability, texture properties, spatial conformation and sensory quality. The results indicated that the adsorption capacity
of Lentinus edodes stipe containing 64% water rolled over twice with a rolling gap of 3.5 mm was 191.87% for compound
flavoring liquid, which was 69.1% higher than that of intact samples. In addition, the hardness and chewiness of Lentinus
edodes stipe were reduced by 34.7% and 44.7%, respectively, and sensory evaluation score was increased by 6.8% after this
treatment. The scanning electron micrograph of the rolled Lentinus edodes stipe showed more loose texture with a hollow
network structure, suggesting that rolling-over is effective in enhancing the holding capacity of Lentinus edodes stipe for flavor
compounds and thus improving the overall quality.

Optimization of Enzymatic Removal of Urethane from Hakka Mother Wine Using Random Centroid Optimization Methodology
SHEN Peng,HUANG Min-xin,BAI Wei-dong,QIAN Min,ZHU Hao
2013, 34(22):  40-43.  doi:10.7506/spkx1002-6630-201322008
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The enzymatic removal of urethane from Hakka mother wine with acid urease was optimized by using randomcentriod
optimization through random search, centroid search and optimal mapping of the random centroid diffraction
procedure. The optimal enzymatic hydrolysis conditions were found to be hydrolysis at 20.70 ℃, initial pH 4.26 for 50 h
with an enzyme of 48.06 mg/L repeated twice. The urea content in Hakka mother wine after the enzymatic treatment was
decreased to (2.134 ± 0.024) mg/L. The urethane content in Hakka mother liquor after one-year storage was measured to
be (25.632 ± 0.017) μg/kg, which showed an 88.5% reduction compared to that without enzymatic treatment. Therefore,
the urethane content in Hakka mother wine can be reduced effectively by the optimized enzymatic treatment and the
consumption safety is improved greatly.

Effect of Rapid Pulping on Water-Absorbing Capacity of Soybean and Emulsifying Capability of Soy Milk
JIN Yang,CHAI Ping-ping,BAO Lu-sheng,Lü Xiao-lian,TIAN Xu,PENG Yi-jiao,GUO Hong
2013, 34(22):  44-47.  doi:10.7506/spkx1002-6630-201322009
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In this study, different soaking methods were used to explore water-absorbing capacity of dehulled soybean and
emulsifying capability of soy milk. Single factor and orthogonal array designs were employed to study the effects of soybean
granularity, soaking time and soaking temperature on water-absorbing capacity of soybean. Meanwhile, the effect of soaking
time on emulsifying capability of soy milk was also investigated. The results indicated that the optimum soaking conditions
were soybean granular size of 2 mm, soaking temperature of 25 ℃, and soaking duration of 150 min. The soy milk prepared
with ground soybean with a particle size of 2 mm by 150 min soaking revealed the same emulsifying capability as that prepared
by the traditional method of 12 h soaking.

Optimizing Ultrasonic-Assisted Extraction of Pigment from Lonicera maackii Fruit by
WANG Li-zhi,TANG Ke-hua
2013, 34(22):  48-53.  doi:10.7506/spkx1002-6630-201322010
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Following a period of spontaneous solvent extraction at a constant temperature, ultrasonication was applied to
enhance pigment extraction from crushed Lonicera maackii fruit. Three extraction parameters including material/solvent ratio,
ultrasonication time and power were optimized by using response surface methodology. All the operating parameters had
a significant effect on extraction efficiency and the optimal extraction conditions were determined as 1:15 (g/mL), 30 min
and 500 W for material/solvent ratio, ultrasonication time and power, respectively. The predicted absorbance at 450 nm of
the pigment extracted under the optimized conditions after 10-fold dilution was 0.836, showing a relative error of only 1.08%
in comparison to the experimental absorbance of 0.827. Thus the optimized process established using response surface methodology
is feasible for pigment extraction from Lonicera maackii fruit.

Optimized Refining and Fatty Acid Composition of Akebia trifoliata var. australis Seed Oil
ZHAO Shi-qiang,ZHU Xue-mei,XIONG Hua,BAI Chun-qing
2013, 34(22):  54-58. 
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The crude seed oil of Akebia trifoliata var. australis obtained by mechanical pressing was degummed by
hydration, deacidified by alkaline treatment, decolorized with adsorbent and deodorized in this study. After optimization
of the process parameters, refined seed oil was obtained. The optimal refining conditions were determined as degumming
at 60 ℃ for 35 min with rapid and then slow stirring after the addition of 3% of water, deacidification at an alkalinity of 16° Bé,
and decolorization at 70 ℃ for 40 min after the addition of 3.5% of white clay (m/m). Sensory evaluation of the crude and
refined seed oils indicated no bitter taste in the refined oil. There was no significant difference in fatty acid composition
among samples collected from the various procedures in the refining process. The seed oil of Akebia trifoliata var. australis
was rich in oleic and linoleic acid with amounts in the range of 44.07%–45.44% and 29.75%–30.86%, respectively.

Optimization of Pigment Extraction from Lagerstroemia indica Flowers by Response Surface Methodology
YAN Li,WANG Li-zhi,MA Ming-you
2013, 34(22):  59-63.  doi:10.7506/spkx1002-6630-201322012
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A three-variable, three-level Box-Behnken experimental design combined with response surface analysis was
employed to optimize the conditions for pigment extraction from Lagerstroemia indica flowers. The extracted pigment was
determined by measuring the absorbance at the maximum absorption wavelength of 546 nm. The best solvent for the extraction
of pigment was found to be 50% ethanol. The optimal conditions for ultrasonic-assisted extraction were determined as
400 W ultrasonic power, 22 min irradiation time and a liquid-material ratio of 45:1 (mL/g). The predicted absorbance of pigment
extracts under the optimized conditions was 0.608 and the actual value was 0.610, showing a small error between both.
Thus, the optimized extraction conditions are reliable.

Supercritical CO2 Extraction and Bioactivity of Polyphenols from Chinese Jujube Seeds
LIU Jie-chao,ZHANG Chun-ling,LIU Hui,ZHENG Xiao-wei,WANG Si-xin,JIAO Zhong-gao
2013, 34(22):  64-69.  doi:10.7506/spkx1002-6630-201322013
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Polyphenols from Chinese jujube seeds were extracted by supercritical carbon dioxide extraction and their
DPPH radical scavenging activity and inhibitory activities against α-amylase, α-glucosidase and hyaluronidase were
evaluated. The optimal extraction conditions that provided maximum extraction efficiency were determined as 2.5 h,
35 MPa, 50 ℃ and 2 for time, pressure, temperature and extraction number, respectively. The extracted polyphenols
possessed strong DPPH radical scavenging activity and could effectively inhibit α-amylase, α-glucosidase and hyaluronidase
and the corresponding inhibition rates were 93.52%, 86.67%, 98.73% and 96.86% over the concentration
range tested with IC50 values of 6.16, 9.81, 7.29 mg/mL and 5.59 mg/mL (expressed as the weight of jujube seeds),
respectively. Correlation analysis suggested an extremely significant positive correlation between the content of
polyphenols and the activities to scavenge DPPH free radical and inhibit three enzymes in jujube seed extracts.
Interestingly, it was also found that the optimal conditions for high yield of polyphenols were not in accordance
with those obtained for high activity, suggesting that the extraction conditions pressure, temperature, duration
and number of repeats could not only affect the yield of polyphenols, but the biological activity as well.

Optimization of Ultrasonic-Assisted Alkaline Extraction of Soluble Dietary Fiber from Eucommia Seed Meal
HUANG Qun,YANG Wan-gen,YU Ji,MA Cheng-jin,WU Li-ya,ZHONG Li-hong
2013, 34(22):  70-74.  doi:10.7506/spkx1002-6630-201322014
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Response surface methodology was applied to optimize the extraction process conditions of soluble dietary
fiber (SDF) from Eucommia seed meal. Three independent variables including material/liquid ratio, ultrasonication time and
temperature were chosen with respect to the dependent variable SDF yield for one-factor-at-a-time design. A mathematical
model was established by Box-Behnken experimental design and analyzed by response surface methodology. The results
showed that the optimal extraction conditions were determined as follows: alkali concentration 2.0 g/100 mL, material/liquid
ratio 1:23 (g/mL), ultrasonication time 23 min, and extraction temperature 43 ℃. Under the optimal extraction conditions,
the yield of SDF was 22.92%.

Extraction of Soluble Dietary Fiber from Apple Pomace and Its Scavenging Capacity against Free Radicals
ZHAO Ming-hui,Lü Chun-mao,MENG Xian-jun,HAN Lu,ZHENG Peng
2013, 34(22):  75-80.  doi:10.7506/spkx1002-6630-201322015
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The extraction of soluble dietary fiber (SDF) from Hanfu apple pomace by hydrolysis with cellulose after pretreatment
with α-amylase and papain was optimized by response surface methodology using a Box-Behnken design on the basis of onefactor-
at-a-time experiments. Four variables influencing the extraction process, such as enzyme dosage, initial pH, temperature
and time were investigated. At the same time, the scavenging effects of apple pomace SDF against DPPH, superoxide anion and
hydroxyl free radicals were evaluated. The results indicated that the optimal extraction conditions were 1.06%, 4.9, 48 ℃ and
228 min for enzyme dosage, initial pH, temperature and time, respectively. The yield of SDF under the optimized conditions was
(18.21±0.21)%. The SDF obtained was able to scavenge all the three free radicals.

Optimization of Extraction Conditions of Antioxidant Components from Stevia Residue after Stevioside Extraction by Response Surface Methdology by Response Surface Methodology
HONG Yi-lan,XU Wen-bin,REN Xiao-jin,CHEN Jie,XI Yin-ci
2013, 34(22):  81-86.  doi:10.7506/spkx1002-6630-201322016
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The ultrasonic extraction of antioxidant components from Stevia residue after stevioside extraction was studied
by single factor approach and response surface methodology. The extraction conditions were optimized with respect to
material/liquid ratio, ultrasonication duration and ultrasonic power using a three-variable, three-level experimental design.
In the optimization, DPPH radical scavenging capacity and the extraction yield of total polyphenols were used as response
variables. The optimal extraction conditions of material/liquid ratio, ultrasonication duration and ultrasonic power were
found to be 1:24.41 (g/mL), 38.05 min and 164.62 W, respectively. The predicted DPPH radical scavenging capacity and
yield of total polyphenol under the optimized conditions were 91.18% and 16.49 mg/g, respectively. From the view of practical
application, the modified extraction conditions were 1:24 (g/mL), 38 min and 164 W, under which repeated experiments
showed an average DPPH radical scavenging efficiency of (90.47 ± 1.43)% and an average yield of total polyphenols of
(16.14 ± 0.36) mg/g with good agreement with the predicted results.

Optimization and Effect Evaluation of Clarification Technology of Euryale Ferox Wine with Pectinase by Response Surface Methodology
LIU Jing,HU Yan-ying,LI Xiang-li,FENG Lei,LIU Kai-wei,SUN Ning-fu
2013, 34(22):  87-91. 
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Response surface methodology was used to optimize the decolorization process of Semen Euryales wine by
pectinase treatment. The clarity of Semen Euryales wine was investigated with respect to four variables including enzyme
dosage, pH, temperature and hydrolysis time by using a Box-Behnken design. As a result, a quadratic polynomial regression
equation was built. The equation could well describe the relationship between the dependent and independent variables.
The optimal experimental conditions for decolorizing Semen Euryales wine were determined as hydrolysis with an enzyme
dosage of 0.13 g/L at 38 ℃ for 41 h at initial pH 3.57. The clarity of samples under the optimized conditions was 95.5%.
In addition, the pectin content was reduced significantly, other physiochemical properties showed minor changes and nonbiostability
was evidently improved.

Distribution and Change of Nutrients in Tartary Buckwheat Endosperm and Plumule during Germination and Optimization of Pulping Process
LING Meng-shuo,TANG Nian-chu,ZHAO Chen-wei,GAO Hui
2013, 34(22):  92-96. 
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The endosperm and plumule of germinating tartary buckwheat seeds were stripped and analyzed for distribution
and change of various nutrients such as moisture, crude protein, starch, α-amylase activity, β-amylase activity, reducing
sugar and total flavonoid. Based on an overall consideration of all the nutrients, the optimal germination time for tartary
buckwheat pulping was 5 days. Using one-factor-at-a-time and orthogonal array designs, the optimal pulping parameters
were determined as 1:4 (g/mL), 7, 50 ℃ and 3 min for material/liquid ratio, pH, temperature and time, respectively. The
utilization of raw material was 73.38% and the total flavonoid content was 25.59 mg/100 mL.

Ultrasonic Preparation of β-Cyclodextrin Microcapsules of Clove Oil
HAN Chun-ran,ZHANG Jing,LI Yu
2013, 34(22):  97-100.  doi:10.7506/spkx1002-6630-201322019
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In this work, clove oil was encapsulated with β-cyclodextrin (β-CD) as a wall material by means of ultrasonic
emulsification. Three experimental conditions including core material/wall material weight ratio, ultrasonic power and ultrasonication
time were optimized by response surface methodology. The optimal encapsulation conditions were determined as
follows: 1:6 of clove oil/β-CD weight ratio, 65 W and 13.4 min. The encapsulation efficiency under the optimized conditions
was 21.5%.

Optimization of Ultrasonic-Assisted Hot Water Extraction of Gelatin from Yellow River Cyprinus carpio haematopterus Scale
XIAO Feng,ZHU Wen-xue
2013, 34(22):  101-105.  doi:10.7506/spkx1002-6630-201322020
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Gelatin was extracted from fresh Cyprinus carpio haematopterus scale by ultrasound-assisted extraction method.
On the basis of single factor experiments, Box-Behnken design (BBD) and response surface methodology (RSM) were applied
to explore the effects of extraction temperature, ultrasonic treatment time, ultrasonic power and material/liquid ratio on
extraction efficiency. A mathematical model was established and analyzed to describe the relationship between the extraction
variables and the yield of gelatin. The optimum extraction conditions were found to be 70 ℃ extraction temperature, 300 W
ultrasonic power, 100 min ultrasonic treatment time, and a liquid-to-solid ratio of 10:1 (mL/g), resulting in a yield of gelatin
of 64.18%, which was in good agreement with the model predicted value. Therefore, this method can be applied in the
natural product industry.

Synthesis and Process Optimization of Sucralose-6-acetate
LENG Yi-xin,LIU Xiao-cheng,SU Ji-guang,ZHANG Yun,WU Yu-zhen,HUANG Cheng-long,WAN Yi-dong
2013, 34(22):  106-110.  doi:10.7506/spkx1002-6630-201322021
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Sucrose-6-acetate was chlorinated in the presence of Vilsmeier reagent, which was synthesized with SOCl2 and
DMF. The structure of the sucralose-6-acetate obtained was confirmed by IR and 1H NMR. Chlorination temperature, the
molar ratio of reaction substrates, the amount of toluene added and pH in the reduction reaction were optimized. The most
suitable temperature to prepare the Vilsmeier reagent was 80 ℃. The molar ratio of Vilsmeier reagent to sucrose-6-acetate
was 11:1 and mass ratio of toluene to N,N-dimethylformamide was 1:10. The optimized pH was 7.5 in the reduction reaction.
This chlorination reaction was divided into three steps with three chlorination temperatures of 70, 90 ℃ and 110 ℃, respectively.
The yield of sucralose-6-acetate under the optimized reaction conditions was 55.7%.

Rapid Determination of Enrofloxacin in Milk by Fluorescence Spectroscopy Combined with Chemometrics
LIU Xiao-ming,FENG Shi-yun,ZHOU Ying-zhe,TIAN Feng-wei,ZHAO Jian-xin,ZHANG Hao,CHEN Wei
2013, 34(22):  111-114. 
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Though there are many analytical methods available to determine antibiotic residues in milk, most of them are
rather complicated. A rapid screening method for enrofloxacin in milk was proposed by fluorescence spectroscopy combined
with chemometrics. The fluorescence spectra of milk samples spiked with different concentrations of enrofloaxcin (ENRO)
were recorded and partial least square discriminate analysis (PLSDA) and partial least square (PLS) regression methods were
conducted for use as calibration and prediction models. The results showed that the PLS model could determine the concentration
of ENRO in milk, and the recovery rate for milk samples was in the range of 96% to 111.4%. The PLSDA model
could accurately identify whether ENRO levels in milk samples exceeded the maximum residue limit with good repeatability.
Therefore the established models are useful for rapid determination of ENRO residues in milk.

Analysis of Aroma Components in Jing’an White Tea by HS-GC-QQQ-MS
2013, 34(22):  115-118.  doi:10.7506/spkx1002-6630-201322023
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The composition of aroma compounds in Jing’an White Tea was analyzed by headspace extraction and gas chromatography-
triple quadrupole mass spectrometry (HS-GC-QQQ-MS). Results showed that a total of 37 major volatile compounds
were identified, including 7 hydrocarbons, 6 esters, 6 alcohols, 6 ketones, 4 olefins, 3 acids, 2 aldehydes, 1 phenols
and 2 other compounds. Among them, menthol, limonene, menthone, isopulegol, nonanal, ethyl caproate, caryophyllene,
linalool, piperitone and n-hexadecanoic acid were the major components. The main aroma components were alcohols and
olefins in Jing’an White Tea, with menthol being the most abundant aroma component.

Purification and HPLC Analysis of Caffeoylquinic Acids from Kudingcha Made from Ilex kudingcha C.J. Tseng
WANG Qing-chuan,ZHANG Xin,ZHANG Wen-qin,SUN Xin-qi,HU Bing,SUN Yi,ZENG Xiao-xiong
2013, 34(22):  119-122.  doi:10.7506/spkx1002-6630-201322024
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Six caffeoylquinic acid (CQA) derivatives were separated by column chromatography and semi-preparative
high performance liquid chromatography (HPLC) from the crude extract of Ilex kudingcha C.J. Tseng. An HPLC method
with DAD and TSKgel ODS-80 TsQA column was developed for the simultaneous determination of CQAs in Kudingcha
made from Ilex kudingcha C.J. Tseng. The results demonstrated that six CQA derivatives with 95% purity, 3-CQA,
4-CQA, 5-CQA, 3,4-diCQA, 3,5-diCQA and 4,5-diCQA, could be obtained through the purification of Ilex kudingcha
C.J. Tseng by semi-preparative high performance liquid chromatography (HPLC). The chromatographic conditions were
determined as follows: oven temperature set at 40 ℃, gradient elution with methanol/formic acid (5‰) with a flow rate
0.5 mL/min, and detection at a wavelength of 326 nm. As results, good linearity was observed with correlation coefficients of
0.9992–0.9999, the average recovery of the CQA derivatives from spiked samples was 96.34%, with relative standard
deviations (RSD) less than 3% (n = 3).

Development of Semisynthetic Soyasaponin Derivatives
GUO Wen-xiu,YAN Xin-bin,ZHAO Da-yun
2013, 34(22):  123-127.  doi:10.7506/spkx1002-6630-201322025
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The natural structure of saponins may not stay in the best active state. To enlarge its application and gain intensive
insight into the relationship between structure and function, modification of sugar chains in soyasaponins is required.
Derivatives of soyasaponin Ab were prepared by adding either dodecylamine or phenylethylamine in the presence of carbodiimide.
The semi-synthesized derivatives of soyasaponin Ab with weak polarity were identified by IR, EMI-MS, and
NMR. The derivatives can be used for further exploration of the relationship between immunostimulating adjuvant/haemolytic
activities and molecular structure of soyasaponins and their derivatives.

Detection of Pistachio Allergen in Foods by Loop-Mediated Isothermal Amplification Method
LIU Hao,HUANG Wen-sheng,DENG Ting-ting,FU Kai,JU Xing-rong,CHEN Ying
2013, 34(22):  128-132.  doi:10.7506/spkx1002-6630-201322026
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Loop-mediated isothermal amplification (LAMP) was applied for the rapid detection of pistachio allergen in
foods. According to the sequence of Pistacia vera (Pis v1) allergen 2S albumin, a set of primers was designed. Various
LAMP parameters including reaction temperature and inner primer concentration were optimized and finally the optimal
LAMP assay for the detection of pistachio allergen in foods was established. The specificity, sensitivity and robustness of
the developed method were tested. The results indicated that no cross reaction was observed with other common tree nuts
such as pistachio, cashew, walnut or crops such as soybean, maize, wheat and rice. The absolute limit of detection for pistachio
DNA was 0.2 ng/reaction and the relative limit of detection was 0.1% (m/m) for simulated samples made by mixed
pistachio with wheat as the matrix. Since the LAMP assay could be completed within 60 minutes, only a regular water bath
was required, and the results could be observed by the naked eye according to the color change produced by SYBR GreenⅠ.
This method allows easy, rapid and accurate detection of pistachio allergen in foods and can be especially applicable in a
resource-limited situation.

Wavelength Selection for FT-NIR Spectroscopic Analysis of Protein in Chimonobambusa quadrangularis Shoot Based on iPLS and BiPLS Models
HUANG Wei,TIAN Feng-ling,LIU Zhen-yao,YANG Qiong,ZHAO Xiao-hui,YANG Ji-dong
2013, 34(22):  133-137.  doi:10.7506/spkx1002-6630-201322027
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Objective: To select the characteristic wavelength bands for non-destructive analysis of proteins in
Chimonobambusa quadrangularis shoot by FT-NIR spectroscopy combined with interval partial least squares (iPLS) and
backward interval partial least squares (BiPLS). Methods: The full wavelength range was divided into 12 or 17 bands. PLS
models were developed based on the full wavelength range or on each band and then BiPLS models were built by optimized
combinations of various intervals. The models were evaluated by the mean square error of cross validation (RMSECV) and
root mean square error of prediction (RMSEP). Results: The iPLS and BiPLS models were both more effective than the PLS
models based on the full wavelength range and the BiPLS model was the best one. When 12 intervals were adopted, the
combination of 7 ([5, 3, 6, 12, 4, 2 and 11]) spectral intervals provided the best model showing a 0.321% RMSECV and a
0.218% RMSEP. The proposed method allowed rapid and non-destructive determination of proteins with less variables used
in the modeling and thus improved prediction accuracy.

Analysis of Volatile Compounds in Large Yellow Croaker (Pseudosciaena crocea) Flesh by Headspace Solid-Phase Microextraction Combined with Gas Chromatography-Mass Spectrometry
Lü Wei-jin,ZHAO Jin,MAO Yun-yan,LI Jian-rong,LU Hai-xia,XU Yong-xia,LI Yu-jin
2013, 34(22):  138-142.  doi:10.7506/spkx1002-6630-201322028
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The volatile flavor compounds in fresh large yellow croaker flesh were extracted by head space solid phase microextraction
(HS-SPME) technique and determined by gas chromatography-mass spectrometry (GC-MS). Based on the
abundance of ubiquity of fish flesh volatiles (hexanal, heptanal, cedrol, decanal, 1-octanol, octanal, 1-octen-3-ol and nonanal),
the optimum extraction conditions were determined as follows: CAR-PDMS extraction head (75 μm), sample
injection volume 8 mL, NaCl concentration 0.256 g/mL, extraction temperature 60 ℃, and extraction time 50 min. Totally
39 volatile flavor compounds were identified, including alkanes, aldehydes, alcohols, ester, ketones, and N-, S- or
O-containing compounds as well as heterocyclic compounds with relative concentration of 19.91%, 16.50%, 18.01%,
38.20%, 0.60% and 6.78%, respectively.

Determination of 15 perfluorinated compounds in Chinese spirit by dispersive solidphase extraction and HPLC-MS/MS detection
2013, 34(22):  143-149. 
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A rapid dispersive solidphase extraction and HPLC-MS/MS detection method was developed for the determination of 15 perfluorinated compounds in Chinese spirit. 1.0 mL sample was extracted by 50 mg PSA dispersive solidphase extraction and eluted with 50 mmol/L triethylamine-methanol solution. Then the extract was further detected by HPLC-MS/MS. Analysis was performed by electrospray ionization in negative mode with multiple reaction monitoring(MRM) using internal standard method for quantitative determination. Good linearities were established for the 15 PFCs in the range from 0.1μg/L to 20.0μg/L. The limits of detection were between 0.03 and 0.15μg/L, while the limits of quantitation were ranged from 0.09 to 0.45μg/L. The average recoveries of 15 PFCs were between 83.8% and 119% in spiking levels of 0.5, 1.0 , 2.0and 5.0μg/L.

Simultaneous Determination of Jujuboside A, Jujuboside B and Spinosin in Ziziphi Spinosae Semen Dispersible Tablets by HPLC-MS-MS
MA Gui-jie,ZHANG Ting,XIE Jun-bo,PANG Guang-chang
2013, 34(22):  150-153.  doi:10.7506/spkx1002-6630-201322030
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Objective: A method for simultaneous determination of jujuboside A (JuA), jujuboside B (JuB) and spinosin in
ZSS (Ziziphi Spinosae Semen) dispersible tablets was established using high performance liquid chromatography tandem
electrospray ionization mass spectrometry (HPLC-ESI-MS-MS). Methods: The separation was performed on a YMC ODSAQ
TM column with acetonitrile-0.1% formic acid (36:64, V/V) as the mobile phase at flow rate of 0.3 mL/min. The column
temperature was 30 ℃. The injection volume was 20 μL. The analytes were detected by ESI-MS in the negative ion mode.
In the multiple reaction monitoring (MRM) mode, the quantitative determination of JuA at m/z of 1205.6-1073.6, JuB at m/z
of 1043.6-911.7, spinosin at m/z of 607.2-427.0 was carried out. Results: A good linear relationship between the peak area
and the concentrations of JuA, JuB and spinosin was obtained (r > 0.9992). The average recovery rates for them were 97.39%,
97.86% and 98.48%, respectively, with relative standard deviation less than 1.0%. The contents of JuA, JuB and spinosin
in ZSS dispersible tablets were 4.15, 1.46 mg/g and 21.46 mg/g, respectively. The developed method is rapid, accurate and
repeatable, which is suitable for the simultaneous determination of JuA, JuB and spinosin in ZSS dispersible tablets.

Rapid Determination of Acrylamide in Fried Food by Differential Pulse Voltammetry
ZHANG Wen-ling,WANG Li-ran,FEI Yong-le,LI Shu-guo
2013, 34(22):  154-159.  doi:10.7506/spkx1002-6630-201322031
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The electrochemical reaction of acrylamide (AA) at a platinum electrode was studied and an analytical method
for the determination of AA in fried foods was proposed by differential pulse voltammetry (DPV). The cyclic voltammogram
of acrylamide at the platinum electrode in an electrolyte solution containing 2 × 10-3 mol/L H2SO4 and 0.1 mol/L LiCl
showed one well-defined reduction peak at -0.58 V and oxidation peak at -0.38 V. The optimal experimental conditions
for determining acrylamide by DPV were determined as follows: scanning range 0--1.0 V, pulse increment 0.005 V, pulse
amplitude 0.05 V, pulse width 0.05 s, pulse interval 2.0 s, and sensitivity 100 μA. A linear relationship was found between
the reduction peak current of acrylamide and its concentration in the range of 3.0 × 10-8-9.0 × 10-8 mol/L, with the linear
equation of y = 440.95x-1.4893 (correlation coefficient 0.9954). The recovery rate of AA was 94.4%-103.2% with RSD
of 0.324%-1.785%, and the limit of detection (LOD) was 1.0 × 10-8 mol/L. Compared with the current HPLC method, the
DPV method was more sensitive without any complicated pre-treatments or expensive equipment. Therefore, the developed
method is applicable for the rapid determination of acrylamide in fried foods.

Comparative Study of Quality Changes in Three Kinds of Edible Vegetable Oils during Deep Frying of Dough Sticks
ZHANG Hai-feng,ZHOU Xiao-yan,LI Hui,LI Xiang
2013, 34(22):  160-164.  doi:10.7506/spkx1002-6630-201322032
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Three different edible vegetable oils, blended palm, canola and soybean oils were used to make deep-fried dough
sticks. Used oil samples were collected at the end of each frying cycle for analysis of changes in acid value (AV), peroxide value
(PV), viscosity, color, fatty acid composition, trans fatty acids and VE. Results showed that the acid value, peroxide value and trans
fatty acid content of all the vegetable oils increased with increasing number of heating cycles, while VE content decreased without
significant difference. Moreover, the quality of deep-fried dough sticks was not significantly affected.

Comparison of Taste Quality and Chemical Composition of Rice from Different Growing Areas
LIU Chang-jin,XIE Yan-hui,LI Jing,HUA Ze-tian,ZHANG Jie,LIU Sheng-bin,WAN Hong-ying
2013, 34(22):  165-169.  doi:10.7506/spkx1002-6630-201322033
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On the basis of sensory evaluation of taste quality, the amylose and protein contents in 21 groups of rice
harvested from Tianjin, Heilongjiang and Hainan were analyzed using a conventional method. The results showed that the
sensory score of cooked rice grown in North China ranged from 66.6 to 82.11, while the sensory score of cooked rice grown
in Hainan ranged from 64.23 to 79.99. A significant difference in rice taste quality between the two growing areas was
observed (P < 0.05). The protein content of rice grown in North China was 6.23%–8.99%, compared to 6.78%–11.19%
for those from Hainan indicating a significant difference (P < 0.01). Meanwhile, rice from higher geographic altitude areas
exhibited lower protein content. This result suggests that higher temperature could result in more protein accumulation in
rice. The amylose contents of rice from northern areas and Hainan were 15.39%–19.75% and 14.68%–19.34%, respectively.
The contents of both protein and amylose had a negative correlation with taste quality of cooked rice. Scanning electronic
microscopy showed that the structure of rice endosperm starch granule as well as gelatinization degree of cooked rice was
different in different rice varieties.

Rapid and High Throughput Quantitative Analysis of Catechin Polyphenols in Tea Beverages by Ultra-High Performance Liquid Chromatography with Photodiode Array Detection (UPLC-PDA)
ZHANG Shuang,HUANG Meng-tian,JIAO Yan-jin,TAO Guan-jun,ZENG Mao-mao,CHEN Jie
2013, 34(22):  170-173.  doi:10.7506/spkx1002-6630-201322034
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An efficient and high throughput analytical method was developed for the determination of galiic acid (GA) and
five catechin polyphenols including catechin (C), epicatechin (EC), epigallocatechin gallate (EGCG), epicatechin gollate
(ECG), and epigallocatechin (EGC) in tea. A Kinetex-C18 (2.1 mm×100 mm, 1.7 μm) column was employed at 45 ℃.
Gradient elution was applied with 0.1% acidic methane (V/V) and acetonitrile (from 5% to 30% in 10 min) as the mobile
phase at a flow rate of 0.3 mL/min. The detector wavelength was set at 280 nm. The results demonstrated that six standard
polyphenols could be separated in approximately 7 min. A good linear relationship between polyphenol concentration and
peak area was observed in the range of 0.25-50 mg/L for GA and C and of 1-100 mg/L for EGC, EC, EGCG and ECG,
with correlation coefficients of 0.9993-0.9999. Samples were purified by solid phase extraction. The recoveries of six
polyphenols were in the range of 92.5%-98.5% (GA), 95.9%-98.5% (ECG), 97.8%-101.0% (C), 95.5%-96.7% (EC),
95.5%-98.9% (EGC), and 95.1%-103.4% (EGCG), with relative standard deviation (RSD) of 0.8%-4.7%, respectively.

Lipid Content and Fatty Acid Composition of Eriocheir sinensis at Different Stages of Growth
TANG Chen-jing,SONGQIAN Cheng-hui,FU Na,LIU Yuan,TAO Ning-ping,WANG Xi-chang
2013, 34(22):  174-178.  doi:10.7506/spkx1002-6630-201322035
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The lipid content and fatty acid composition of body meat, crab spawn and crab paste at different growth
stages (October, November and December) of E.sinensis were analyzed by Soxhlet extraction method and gas
chromatography (GC). The results showed that the lipid content showed a descending trend in the body meat of female
crab but an ascending trend in male crab. The highest lipid content was found in crab spawn and crab paste in October,
with the best quality at this growth stage, but descended as the growth proceeded; the lipid content was relatively lower
in body meat and indicated a higher level in female crab than in male one, while crab spawn and crab paste contained
a higher amount of lipids and the lipid content of crab paste was higher than that of crab spawn. Sixteen fatty acids
were detected in E.sinensis including 5 saturated fatty acids (SFA), 4 monounsaturated fatty acids (MUFA) and 7
polyunsaturated fatty acids (PUFA). Among these fatty acids, oleic acid (C18:1) was the most abundant and unsaturated
fatty acids had a higher proportion than saturated ones. According to the ω3/ω6 ratio recommended by the FAO/
WHO, the crab body meat and crab spawn in November and the crab paste in October were most beneficial to human
health. All the body meat, crab spawn and crab paste of E.sinensis at three growth stages had good nutritive quality as
indicated by the dominance of oleic acid.

Analysis of Aroma Components in Mango Chips Prepared by Different Drying Methods
LIU Xuan,LAI Bi-hui,BI Jin-feng,Lü Jian,DING Yuan-yuan
2013, 34(22):  179-184.  doi:10.7506/spkx1002-6630-201322036
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Gas chromatography coupled to mass spectrometry (GC-MS) was used to analyze aroma components of fresh
mango samples and mango chips prepared by four different drying methods. The results showed that the main aroma
components of fresh mango sample were 66.25% terpenes (mainly δ-3-carene, 4-carene and caryophyllene), 12.42%
alcohols (mainly 3,6-nonadien-1-ol) and 19.26% alkanes. More ester, aldehyde, and alkane compounds were produced
while terpenes showed an obvious reduction during hot-air drying. Meanwhile, obvious loss of some characteristic aroma
compounds in fresh mango was observed. The contents of all other aroma compounds were increased except terpenes and
alcohols by microwave vacuum drying. Compared with three other drying methods, the most significant loss of terpenes but
the most obvious increase in alkanes were observed accompanied with the highest concentration of phenolic compounds
during vacuum freeze drying. Compared with samples dried by three other methods, mango chips by explosion puffing
drying showed the least loss of terpenes, which were considered as the characteristic aroma components in flesh mango. The
concentrations of aldehydes were also high and phenolic compounds were also found.

Qualitative Identification of Mopan Persimmon Shelf-life by Near Infrared Spectroscopy
WANG Dan,LU Xiao-xiang,ZHANG Peng,CHEN Shao-hui,LI Jiang-kuo
2013, 34(22):  185-188.  doi:10.7506/spkx1002-6630-201322037
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Near-infrared spectroscopy was used for qualitative identification of Mopan persimmon shelf-life. Different
spectral pre-treatment methods and different spectral ranges for the shelf-life of Mopan persimmon were compared. The best
results of spectral pretreatment were obtained by using secondary derivative model combined with standard normal variate
and detrend (SNVD) in the wavelength range of 1100–1800 nm. The percentage of correct classification of samples by using
the developed discriminant model was 95.4% with a forecast accuracy of 93.3%. Therefore, near-infrared spectroscopy is a
useful technique to predict the shelf life of Mopan persimmon.

Speciation of Iron in Grifola frondosa
CHEN Chen,SU Ke,CHEN Gui-tang,ZHAO Guo-qiang,HU Qiu-hui,ZHAO Li-yan
2013, 34(22):  189-192.  doi:10.7506/spkx1002-6630-201322038
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An optimized process for the extraction of iron from fruit bodies of Grifola frondosa was proposed for
analysis of iron content and speciation in water extracts of the mushroom Grifola frondosa by flame atomic absorption
spectrophotometry. Four aqueous iron species such as suspended, soluble, inorganic and organic irons were obtained by using a 0.45 μm
filtration membrane and D-101 macroreticular resin. The organic states of iron in its complexes with protein and polysaccharide
were isolated. The results showed that the optimal extraction conditions for iron were determined as follows: extraction
temperature 100 ℃, extraction time 120 min and material/liquid ratio 1:60 (g/mL), resulting in an extraction yield of 72.7%.
The soluble Fe was approximately 64.4% and the suspended Fe was approximately 8.3% in the water extract. The populations
of aqueous inorganic Fe and organic Fe were 39.0% and 26.1%, respectively. Organic Fe was mainly bound to protein and
polysaccharide with contents of 12.8% and 10.5%, respectively.

Speciation Analysis of Mercury in Shellfish Muscle
CAO Cheng-ming,LENG Tao-hua,XIE Nan,NING Xiao-jun,ZHOU Yao
2013, 34(22):  193-197.  doi:10.7506/spkx1002-6630-201322039
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Four mercury species (inorganic mercury, methyl-mercury, ethyl-mercury and phenyl-mercury) in shellfish muscle
were analyzed by high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS). A
C18 reverse phase HPLC column was applied to separate four mercury species, and their concentrations were measured by using
ICP-MS through an external standard method. The method was optimized and the four mercury species could be effectively
separated within 15 min using gradient elution with methanol/ammonium acetate as the mobile phase. This developed method is
simple, efficient and sensitive, which can be suitable for determination of mercury species in shellfish muscle.

Molecular Subtyping of Salmonella enteritidis in Imported and Exported Foods Using Pulsed Field Gel Electrophoresis
FAN Fang,TANG Mu-jin,Lü Jing-zhang,WAN Zhi-gang,Lü Dong-yue,ZHANG Heng,MA Shu-mian
2013, 34(22):  198-201.  doi:10.7506/spkx1002-6630-201322040
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Objective: To explore the relationship among Salmonella enteritidis strains isolated from imported and
exported foods in Shenzhen during 2005–2011, and develop a DNA fingerprint database of Salmonella enteritidis.
Methods: Chromosomal DNAs from 58 isolates in agarose were digested with the restriction enzyme Xba Ⅰ, and then
were analyzed by pulsed-field gel electrophoresis (PFGE). PFGE patterns were clustered using BioNumerics software.
Results: DNA fingerprint database of imported and exported foods in Shenzhen was successfully developed. The
results showed that there were 18 distractive PFGE patterns including 2 clusters. In cluster 1, Salmonella enteritidis
strains isolated from American poultry meat products had 91.45% similarity, and pattern 2 was the dominant type. In
cluster 2, 38 Salmonella enteritidis strains isolated from Chinese and Argentinian poultry meat products had 91.03%
similarity and its dominant type was P8. Conclusion: There were two closely correlated pandemic clones of Salmonella
enteritidis isolated from imported and exported foods. The development of DNA fingerprint database of imported and
exported foods can contribute to develop molecular subtyping surveillance network for active surveillance and source
tracking of food-borne pathogenic bacteria.

Determination of Polycyclic Aromatic Hydrocarbons (PAHs) in Vegetable Oil by Gas Chromatography Coupled with Triple Quadrupole Mass Spectrometry Using Isotope Dilution
YANG Jun,WANG Jian-hua,GONG Ping,LIU Jing-jing
2013, 34(22):  202-207.  doi:10.7506/spkx1002-6630-201322041
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An analytical method for the determination of 16 types of polycyclic aromatic hydrocarbons (PAHs) in vegetable
oil has been developed. Samples that had been spiked with isotope standard solution were extracted using acetonitrile/acetone
(60:40, V/V) and purified by gel permeation chromatography (GPC). Identification and quantification were performed
using gas chromatography-triple quadrupole fandem mass spectrometry (GC-MS-MS) in the selected reaction monitoring
(SRM) mode. The efficiency of GPC was compared with that of solid phase extraction (SPE) for purifying crude extracts
and the instrument parameters were optimized. The recovery rates of 16 PAH standards were in the range of 70.8%–123.1%
from samples spiked with 4–6 μg/kg internal standard. The precision (RSD) of the developed method was 1.0%–6.5% with a
limit of quantification of 0.22–0.74 μg/kg (r ≥ 0.9982). Therefore, it is suitable for the analysis of 16 types of PAHs.

Determination of Estradiol Benzoate Residues in Aquatic Products by LC-MS-MS
ZHANG Shan-shan,YU Hui-juan,HUI Yun-hua,FENG Bing,ZHANG Xiao-ling
2013, 34(22):  208-211.  doi:10.7506/spkx1002-6630-201322042
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A high performance liquid chromatography-tandem mass spectrometric (LC-MS-MS) method has been
established for the determination of estradiol benzoate residues in aquatic products. Sample pretreatment conditions and
instrumental parameters were optimized. Samples were extracted with methyl tert-butyl ether, cleaned up on an LC-C18 solid
phase extraction column and degreased with methanol-water. Separation of the analyte was carried out on Waters XBridge
RP-18 column (150 mm × 4.6 mm i.d., 5 μm) using a mobile phase made up of methanol and water before analysis by
electrospray ionization LC-MS-MS using medroxyprogesterone-D3 as internal standard. The limit of quantification of this
method was 1 μg/kg. The average recovery from samples spiked in the range of 1 to 10 μg/kg was 77.9%–113.5%, with
RSD less than 9.4%. This method was sensitive, reproducible, and suitable for the determination of estradiol benzoate in
various aquatic products.

Determination of Sulfite in Vegetables and Derived Products by Nitrogen Distillation-Pararosaniline Hydrochloride Spectrophotometric Method
FANG Chang-yun,DUAN Bin-wu,SUN Cheng-xiao,LU Lin,HE Xiao-yan
2013, 34(22):  213-218.  doi:10.7506/spkx1002-6630-201322043
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A nitrogen distillation-formaldehyde solution absorption-pararosaniline hydrochloride spectrophotometric
method for the determination of sulfite in vegetables and derived products was developed. The results showed that the
detection limit for sulfite was 0.5 mg/kg in 5.0 g of samples. This method had a good linearity (R2 = 0.9998) for sulfur
dioxide with a concentration ranging from 0 to 10 mg. The relative standard deviation of the proposed method ranged from
0.75% to 3.78%. The recovery rate was in the range of 89.8% ~ 98.3%. The developed method has less color interference
from samples and less pollution. It is easy and simple with good repeatability, which is suitable for the determination of
sulfite in vegetables and derived products.

Rapid Determination of 14 Psychoactive Drugs in Sleep-Improving Health-Care Foods by Ultra-High Performance Liquid Chromatography-Photodiode Array Detection
LIN Fang,LI Tao,LI Ji,ZHU Xiao-hong,YANG Miao
2013, 34(22):  218-223.  doi:10.7506/spkx1002-6630-201322044
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A method of ultra performance liquid chromatography-photodiode array detection (UPLC-DAD) has been established
for the rapid simultaneous determination of 14 psychoactive drugs (alprazolam, estazolam, clonazepam, diazepam, phenobarbital,
midazolam maleate, triazolam, nitrazepam, barbital, secobarbital, chlordiazepoxide, lorazepam, amobarbital, and oxazepam) that
are illegally added in sleep-improving health-care foods. A ZORBAX SB-C18 column (2.1 mm × 100 mm, 1.8 μm) was applied.
Methanol-0.2% acetic acid was selected as the mobile phase in a linear gradient elution mode,with flow rate of 0.4 mL/min.
The detection wavelengths were 210 nm and 230 nm for rapid screening and quantitation. The results showed that the 14
psychoactive drugs could be effectively separated in 13.5 min, and the standard curves had good linearity over the concentration
range of 5–50 μg/mL or 10–100 μg/mL. The correlation coefficients (r) were all above 0.9995. The average recoveries varied
from 80.4%–106.2% and the detection limits were in the range of 3–6 ng for the psychoactive drugs. This developed method is
characteristics of simple operation, rapid determination, high sensitivity and excellent reproducibility so that it is suitable for the
rapid determination of d 14 illegal psychoactive drugs in sleep-improving health-care foods.

Effect of SPME Conditions on the Determination of Volatile Compounds in Orange Juice Using GC-FID Method
NIU Li-ying,YU Meng,WU Ji-hong,LIU Fu-guo,LIU Chun-quan
2013, 34(22):  224-233.  doi:10.7506/spkx1002-6630-201322045
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The effect of NaCl concentration, extraction duration, extraction temperature and desorption time during
headspace solid phase microextraction (HS-SPME) on the analysis of 14 flavor compounds in orange juice was investigated
by using gas chromatogram with hydrogen flame ionization detection (GC-FID) and optimized by orthogonal array design.
The results showed that the flavor compounds could be categorized into 2 groups: one group with five isomers of C10H16
as well as octanal, octanol, carvone and valencene; the other group with three isomers of C10H18O as well as ehtyl butyrate
and octyl acetate. The NaCl concentration had the most significant effect on the first group, followed by desorption time,
extraction temperature and extraction duration, while the desorption time showed the least significant effect on the second
group. These results would offer valuable information for precise quantification of multiple flavor compounds in orange
juice by an internal standard or standard addition method due to the behavior consistency to the HS-SPME conditions in
each group.

Effect of Processing Conditions on the Key Flavor Compounds of Baked Quail Eggs as Analyzed by “ROAV” Method
WANG Wu,WU Qiao,DONG Qi,XIA Xin-wu,CHEN Cong-gui
2013, 34(22):  234-238.  doi:10.7506/spkx1002-6630-201322046
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The volatile flavor compounds in quail eggs under different baking conditions were analyzed by headspace solid
phase micro-extraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS). Relative odor activity value
(ROAV) was applied to evaluate the contribution of various ingredients to the overall flavor of baked quail eggs. Results
indicated that 1-octene-3-ol, isoamyl acetate, saturated or unsaturated fatty aldehydes (carbon atom number ≤ 10) were the
major flavor components of baked quail eggs. With increasing of temperature and extended baking time, the concentration
of aldehydes was increased while the concentration of isoamyl acetate was reduced. In addition, the concentration of
heterocycle was increased first and then decreased. The flavor of quail eggs baked at different temperatures for different
times revealed both identical and different characteristics.

Determination of Acrylamide in Fried Foods by Flow Injection-Chemiluminescence Method
GAO Xiang-yang,ZHAO Chen,YOU Xin-xia,WANG Ying-ying
2013, 34(22):  239-242.  doi:10.7506/spkx1002-6630-201322047
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A new sensitive accurate and cost-effective method established for the determnation of trace acrylamide in
fried foods by using flow injection chemiluminescence. The proposed method was based on enhanced chemiluminescence detection
of the luminal/hydrogen peroxide system in the presence of the acrylamide extracted from samples. Instrumental
parameters and the reaction system were optimized. The linear range of this method was 1.0 × 10-6–1.0 × 10-3 mol/L with a
correlation coefficient of 0.9993, and the detection limit was 3.95 × 10-8 mol/L. The recovery rate was 91%–107%, with
RSD (n = 9) of 1.3%. Satisfactory results were obtained in its practical application.

Determination of β-Carotene in Spirulina by RP-HPLC
LUO Guang-hong,WANG Qin,YUAN Xiao-long,ZU Ting-xun
2013, 34(22):  243-245.  doi:RP-HPLC;Spirulina;β-carotene;content
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Objective: To establish a method for the determination of β-carotene in Spirulina using RP-HPLC. Methods:
A Hypersil ODS-2 C18 (150 mm×4.6 mm, 5 μm) was used for the analysis with methanol-acetonitrile (90:10, V/V) as the
mobile phase at a flow rate of 1.2 mL/min at 30℃. The detection wavelength was 448 nm. Results: The linear regression
equation for β-carotene was Y = 1388.33X + 17.74 (r = 0.9999), which was linear over the range of 0.517–4.653 μg, and the
average recovery rate was 98.03% with RSD of 0.94% (n = 6). Conclusion: This method is accurate and repeatable, and can
provide a scientific basis for the quality standardization of Spirulina products.

Determination of Chondroitin Sulfate from Sea Cucumber by Methylene Blue Colorimetry
XU Xiao-qi,XUE Chang-hu,ZHANG Cui-yu,YU Long,WANG Yan-chao,CHANG Yao-guang
2013, 34(22):  246-249.  doi:10.7506/spkx1002-6630-20132249
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In this study, employing sea cucumber chondroitin sulfate standard samples extracted from 5 species of sea
cucumber, an efficient and rapid colorimetric method for determination of chondroitin sulfate from sea cucumber was established
based on the theory that methylene blue and anionic polymer can form supramolecular complex. The colorimetric
method was determined as follows: detection at 545 nm immediately following mixing of 1.00 mL of sea cucumber
chondroitin sulfate solution with 8.00 mL of 5 mmol/L pH 7.0 K2HPO4/KH2PO4 buffer and 1.00 mL of methylene blue
(0.18 mg/mL) and subsequent calculation of chondroitin sulfate concentration from the absorbance using the pre-prepared
calibration curve. This method proved to be simple, accurate and high-recovery and allow rapid quantitative determination
of sea cucumber chondroitin sulfate.

Analysis of Volatile Components and Fatty Acids in Silurus meridionalis Chen×Silurus spp.
LONG Bin,WANG Xi-chang,ZHANG Feng-ping,CAO Jing,LIU Yao-min
2013, 34(22):  250-256.  doi:10.7506/spkx1002-6630-201322050
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The volatile flavor composition of farmed Silurus meridionalis Chen×Silurus spp. was analyzed by simultaneous
distillation extraction and gas chromatography-mass spectrometry (SDE-GC-MS). Totally 67 volatile compounds were
isolated and identified from belly meat, and 45 compounds from dorsal meat, in which 38 compounds including hydrocarbons,
aldehydes, ketones and esters were common to both. The contents of hydrocarbons and aldehydes were 4525.36 ng/g and
1889.02 ng/g in belly meat and 1706.61 ng/g and 2117.39 ng/g in dorsal meat, respectively. The major compounds that
contributed the most to the flavor of Silurus meridionalis Chen×Silurus spp. included hexanal, octanal, heptanal, nonanal,
(Z)-2-heptenal, (E)-2-octenal, (E,E)-2,4-decadienal, and 1-octen-3-ol. Unsaturated fatty acids (UFA) were the major fatty
acid components in both belly meat and dorsal meat, which accounted for 69.48% and 68.36% of the total fatty acids,
respectively. After SDE, the concentrations of polyunsaturated fatty acids (PUFA) in raw belly meat and dorsal meat
dropped from 35.36% and 34.12% to 33.04% and 32.51%, respectively. PUFAs were the important aromatic precursors in
Silurus meridionalis Chen×Silurus spp. meat.

Application of Inductively Coupled Plasma Mass Spectrometry (ICP-MS) for Determination of 28 Trace Elements in Chinese Liquor
ZHANG Jian,TIAN Zhi-qiang,LU Yuan-yu,CHEN Xing-lin,SUN Zong-qi
2013, 34(22):  257-260.  doi:10.7506/spkx1002-6630-201322051
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This paper describes a simple method for the determination of 28 micro-elements including Ag, Cd, Cs, Ba, Li, Be,
Na, Mg, Al, K, Ca, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Tl, Pb, Bi, U, Rb, and Sr in Chinese liquor by using inductively
coupled plasma mass spectrometry (ICP-MS). For digestion of samples, 10 mL of a mixture of HNO3 with HClO4 (4:1, V/V) was
used. The results revealed that the method had some advantages, such as simple sample pretreatment, fast analysis, low detection
limit, high precision and accuracy, and wide linear dynamic range (0–300 μg/L for 21 of these micro-elements, 0–30 μg/L for the
rest). The recovery rates for all the micro-elements were between 85.19% and 104.01% with RSD less than 4.7%. This method can
completely meet the requirements for determination of the 28 micro-elements in Chinese liquor.

Determination of Chlorite Chlorate and Perchlorate in Carbonated Beverage by Ion Chromatography-Electrospray Ionization Tandem Mass Spectrometry
GAO Feng,LIU Yan,KONG Wei-heng,CHENG Xi-ming,LI Jing,ZHANG Jie
2013, 34(22):  261-264.  doi:10.7506/spkx1002-6630-201322052
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A method has been developed for the determination of chlorite, chlorate and perchlorate in carbonated beverage
by using ion-chromatography-electrospray tandem mass spectrometry (IC-ESI-MS) in a negative ESI mode. Chlorite
chlorate and perchlorate were separated on a high-capacity, hydroxide-selective column by gradient elution with KOH eluent
generated from an eluent generator cartridge (EGC). The linear range was 1–200 ng/mL with a linear correlation coefficient
of 0.997. The quantitation limits for chlorite, chlorate and perchlorate were 1.5, 1.0 μg/L and 0.6 μg/L, respectively. The
recovery rates from spiked standard samples were in the range of 79%–104% with RSD in the range of 0.54%–4.49%
(n = 6). This method proved to be simple, quick, sensitive and precise. It can be applied widely and suitable for simultaneous
determination of chlorite chlorate and perchlorate in carbonated beverage.

Effect of Microwave Roasting Temperature on Characteristic Flavor Compounds of Sesame Oil
CONG Shan,HUANG Ji-nian,ZHANG Li-xia,ZHANG Guo-zhi
2013, 34(22):  265-268.  doi:10.7506/spkx1002-6630-201322053
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The effect of microwave roasting temperature on the characteristic flavor compounds in sesame oil extracted
with water from white sesame was explored. Headspace solid phase microextraction combined with gas chromatographymass
spectrometry (HS-SPME-GC-MS) was used to analyze the characteristic flavor compounds in sesame oil. The results
showed that the contents of pyrazines, pyrroles, furans and phenols were increased with the increase of microwave roasting
temperature while the content of aldehydes was decreased.

Simultaneous Determination of Folic Acid, Vitamin B12 and Biotin in Infant Formula by HPLC-MS-MS
WANG Feng-ling,LIU Ai-guo,SUN Jia-jia,PENG Cheng
2013, 34(22):  269-272.  doi:10.7506/spkx1002-6630-201322054
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A method using high performance liquid chromatography tandem mass spectrometry (HPLC-MS-MS) for
simultaneous determination of folic acid, vitamin B12 and biotin in infant milk power was presented. Samples were
sequentially extracted and then subjected to isoelectric precipitation (pH 1.90/4.70). The analysis was carried out on an
SB-Aq column (2.1 mm × 100 mm, 1.8 μm) with isocratic elution using a mobile phase made up of 0.1% (V/V) aqueous
formic acid and acetonitrile (16.5:83.5, V/V). The analytes were detected in the MRM mode. Folic acid, vitamin B12 and
biotin in samples could be separately well within 5 min. The calibration curves were linear over the concentration range of
3.5 - 250 ng/mL for folic acid, 0.8 - 5 ng/mL for vitamin B12, and 0.7 - 50 ng/mL for biotin. The average recovery rates
were 97.8%, 102.3% and 96.9%, with RSD of 1.33%, 0.9% and 1.37% for folic acid, vitamin B12 and biotin, respectively.
The developed method is precise, accurate, sensitive, fast and simple, which can thereforebe applied for the analysis of folic
acid, vitamin B12 and biotin in infant formula.

Separation and Purification of Small-Molecule Peptides with Immunomodulating Activity from Goat Placenta
LIU Long-xing,REN Xing-hong,TANG He-jing,TANG Zhao-yong,HE Cheng-ming,FANG Liao-qiong
2013, 34(22):  273-276.  doi:10.7506/spkx1002-6630-201322055
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The purpose of this study was to isolate and purify small-molecule peptides with immunomodulating activity
from goat placenta. Ultrafiltration fraction from goat placenta was prepared by a conventional method, followed by
isolation, purification and analysis by reversed phase-high performance liquid chromatography (RT-HPLC). The immunomodulating
activity of its components was measured by E-rosette test and the N-terminal sequence was measured
by Edman degradation reaction. Three small-molecule peptides with high purity were obtained, two of which were immune-
active. The results of sequencing and retrieving showed that they were new peptides. RT-HPLC was one of the
optimal methods to purify and analyze bioactive peptides. The small-molecule peptides from goat placenta revealed
strong immune activity.

Determination of Asulam in Agricultural Products by LC-MS-MS
ZHANG Qi-feng,KAZUO Matsumoto,ZHANG Mao-qiang,JIANG Jian-mei,ZHAO Hua-feng
2013, 34(22):  277-280.  doi:10.7506/spkx1002-6630-201322056
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A simplified pretreatment coupled with reliable liquid chromatography-tandem mass spectrometry (LC-MS-MS)
method has been developed for the determination of asulam in agricultural products. Samples were extracted with methanol,
and then divided into equal portions. After evaporation, residues were dissolved in 0.1% formic acid solution containing 1%
disodium ethylenediamine tetraacetic acid (EDTANa2). The sample was applied to a pre-conditioned hydrophilic lipophilic
balanced reversed solid-phase extraction column (HLB). Under these conditions, asulam was retained in the adsorbent of
HLB. After flushing of the column, asulam was eluted with 50% methanol solution. It was filtered through a 0.45 μm filter
to a vial before analysis by LC-MS-MS. The average recoveries from 6 agricultural samples varied from 70.6% to 107.8%,
the repeatability varied from 1.0% to 14.0%, the inter-day precision varied from 4.4% to 17.7% and the matrix recoveries
varied from 81.4% to 115.0%, showing little matrix effect. The validation experiments showed that the method was simple,
fast, accurate and sensitive and could meet the requirements for the determination and confirmation of asulam in agricultural
products with a limit of quantification of 0.01 mg/kg.

Prediction of Egg Storage Time Using Portable Near Infrared Spectrometer
BI Xia-kun,ZHAO Jie-wen,LIN Hao,SUN Li,GUAN Bin-bin
2013, 34(22):  281-285.  doi:10.7506/spkx1002-6630-201322057
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Two different portable near infrared spectrometers (USB 2000+ and Maya 2000) were used to acquire spectra
of eggs stored for different times with high- and low-intensity light source systems. Discrimination and classification
of storage times of eggs was achieved by two different methods, PCA and LDA analysis. The results showed that LDA
was superior to PCA and Maya 2000 which correctly discriminated 95.7% of egg samples in LDA analysis and 93.2%
of cross-validated samples was superior to USB 2000+. Even using a low-intensity light source system, discrimination
of the freshness and shelf life of eggs can be achieved by an appropriate near infrared spectrometer combined with an
appropriate discrimination method.

Induction of Disease Resistance to Gray Mold by Pichia membranaefaciens in Postharvest Strawberry Fruit
ZHANG Lu,ZHANG Yao,LIU Li-dan,ZENG Kai-fang
2013, 34(22):  286-291. 
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Strawberry is highly susceptible to pathogen infection during storage, and gray mold caused by Botrytis cinerea
is one of the common diseases of strawberry fruit. The ability of the yeast Pichia membranaefaciens to control gray mold
of strawberry fruit during storage were examined in this study. The possible biocontrol mechanism of P. membranaefaciens
was also discussed. It was showed that there was a positive correlation between yeast concentration and the effect of disease
control. Treatment with 1 × 107 CFU/mL P. membranaefaciens suspension resulted in lower disease incidence of gray mold, and
had no harm to the epidermis. The fruit treated with P. membranaefaciens demonstrated accumulated activities of defense-related
enzymes such as β-1,3-glucanase (GLU), phenylalanine ammonia-lyase (PAL) and peroxidase (POD) in strawberry fruit. These
results indicated that P. membranaefaciens could effectively reduce the incidence of gray mold in strawberry. The induction of
resistance was one of the most important mechanisms of P. membranaefaciens control of strawberry gray mold.

Predictive Modeling of Pseudomonas spp. Growth in Fish Belly and Shelf Life Prediction
SONG Zhi-qiang,LIU Chao-qun,HOU Wen-fu
2013, 34(22):  292-297.  doi:10.7506/spkx1002-6630-201322059
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Sensory evaluation of fresh fish belly was made and plotted as a function of storage time. Changes in total volatile
basic nitrogen (TVB-N) over the storage period of 7 days were measured and observed and predicted growth curves of
Pseudomonas spp. were plotted based on according to the results of viable counts and predicted results from the Gompertz
model under different temperatures. Bias factor and accuracy factor were used to verify the accuracy of the first-order model,
and the result was close to 1, indicating that the model was fitted well. Belehradek model was used to describe the correlation
between temperature and growth parameters of Pseudomonas spp. The prediction model presented in this study could
be used to predict the shelf life of fish belly. Comparison between the observed and the predicted shelf life of fish belly was
carried out to reveal the reliability of shelf-life prediction for fish belly.

Effect of Coating on Quality Change of Chilled Pork during Storage
XING Xin-tao,LEI Tian-tian,SUN Jing-xin,FENG Ting,LIN Ping
2013, 34(22):  298-302.  doi:10.7506/spkx1002-6630-201322060
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Our present work aimed to explore the effect of coating on quality change of chilled pork during storage. We
investigated the effect of temperature on the antimicrobial properties of tea polyphenols. Chilled pork was sterilized with
H2O2 to establish an aseptic meat model. The model was inoculated with a single strain of Pseudomonas and then subjected
to treatment with different coatings (sodium alginate coating, sodium alginate/tea polyphenol coating, chitosan coating and
chitosan-tea polyphenol coating). The coated samples were stored at 4 ℃ for 21 days. The pH, TVB-N, TBARs, Pseudomonas
colony counts, electrophoresis pattern and sensory score were determined every 3 days during the storage period. The results
obtained were compared among four coating treatment groups. All the coating treatments could effectively preserve chilled
pork compared to the control group, and the chitosan-tea polyphenol coating displayed the lowest values of pH, TVB-N,
TBARs and the number of Pseudomonas colonies, darker and wider electrophoresis bands and the highest sensory evaluation
score. After 21 d of storage, the meats from the group remained fresh at grade 1. Therefore, the shelf life of chilled pork
could be effectively extended by pre-coating during storage.

Effect of Temperature and Gas Composition Conditions on Bitterness of Grapefruit during Refrigerated Storage
YUAN Qi,YAO Xiao-ling,FENG Gui-ren,ZHANG Yan-nan
2013, 34(22):  303-306. 
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The effect of varying temperature (0, 5, 10 ℃ and ambient temperature) and gas composition (3%, 6% and 10% O2)
during refrigerated storage on the bitterness of grapefruit was studied. Results indicated that grapefruit bitterness varied with storage
temperature and the content of bitter compounds dramatically fluctuated in a substantially consistent manner throughout the
storage period under varying temperatures, which was manifested by an increasing trend during the first 30 days before decreasing
and then remaining stable during 30–105 days. The minimum amount of bitter compounds was detected in grapefruit stored at 10 ℃.
Compared with the control group, three MAP groups contained more or less bitter compounds, showing irregular changes. During
30–105 days, smaller fluctuations were found for the amount of bitter compounds with increasing volume fraction of oxygen and
the 10% O2 group showed the smallest change.

Effect of Storage Temperature on Physico-chemical Properties of Strawberry
XIE Jing,ZHANG Li-ping,WANG Jin-feng,XIONG Qing
2013, 34(22):  307-310.  doi:10.7506/spkx1002-6630-201322062
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Strawberries from Qingpu farm were chosen as samples to investigate their freezing point and physico-chemical
properties. For this purpose, three different storage temperatures, (0.0 ± 0.8), (4.0 ± 0.6) ℃ and (20.0 ± 0.5) ℃ were set
and texture properties, VC and titratable acid contents, color parameters and sensory quality of strawberries were determined
at different periods of storage. The results indicated that strawberry fruits stored at 20 ℃ were unacceptable after 3 days
of storage, but the shelf life of strawberry fruits at the other two temperatures were close to 15 days, without significant
differences in sensory evaluation, texture parameters, color change or weight loss rate (p > 0.05). As for temperature
fluctuation in a common domestic refrigerator, 4 ℃ is recommended for the storage of strawberry furits from Qingpu farm.

Effect of Different Microvacuum Pressures on Quality Preservation of Pleurotus ostreatus
WANG Shi-kui,WANG Li-jiao,LI Wen-xiang,ZHANG Sheng-jie,SUN Shu-jie
2013, 34(22):  311-314.  doi:10.7506/spkx1002-6630-201322063
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Physiological changes of fruit bodies of Pleurotus ostreatus stored at (3.0 ± 0.5) ℃ under three different microvacuum
pressures, 53.33–66.66, 66.66–79.99 kPa and 79.99–93.33 kPa were examined in comparison to control samples stored under MAP
conditions. The results showed that respiratory intensity and the decomposition of soluble proteins in Pleurotus ostreatus were
remarkably inhibited at the microvacuum pressures as compared to the control group. Moreover, a delayed increase in the degree
of browning and a significant increase in relative cell membrane conductivity were observed (P < 0.05). However, a higher weight
loss was observed during storage under these microvacuum pressures. Significantly improved preservation of Pleurotus ostreatus
was obtained under 66.66–79.99 kPa compared to 53.33–66.66 kPa and 79.99–93.33 kPa (P < 0.05).

Effect of Different Micro-vacuum Pressure on the Storage of Pleurtus ostreatus
WANG Xiao-xia,XU Ning,QIN Xiao-jie,XU Xin,LIU Miao-yan,LIU Dan,XIAO Hong-mei
2013, 34(22):  315-321. 
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In order to evaluate the effect of micro-vacuum conditions on the storage of Pleurotus ostreatus, the physiologic change of Pleurotus ostreatus under different vacuum pressure(400-500torr、500-600torr、600-700torr) were studied contrasted with that under modified atmosphere packaging storage at 3±0.5℃. The results showed that micro-vacuum conditions could inhibit the respiratory intensity, delay the decline of soluble protein content, the rising of browning degree and the increasing of relative leakage rate significantly(P<0.05) ,but the weight loss of control group was lowest. Pleurotus ostreatus under 500-600torr had a better preservation performance than that under 400-500torr and 600-700torr(P<0.05).

Enzymatic Production of Heat-Induced Porcine Blood Gels
ZHENG Ya-mei,WANG Yu,SHANG Yong-biao
2013, 34(22):  322-326.  doi:10.7506/spkx1002-6630-201322065
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This study reports on the use of transgluminase (TG) for enzymatic preparation of heat-induced porcine blood gels
from fresh porcine blood. Various experimental conditions, such as TG dosage, the amount of added NaCl and blood-to-water
ratio were investigated for their influence on cooking loss, textural properties and color of heat-induced porcine blood gel. Results
indicated that the textural properties of heat-induced porcine blood gels exhibited a significant enhancement when added with 0.2%
of TG. The heat-induced gels revealed significantly deteriorated quality, an evident increase in cooking loss and a severe foaming
phenomenon when more TG was added. The heat-induced gels formed at NaCl concentration of 0.3 mol/L and a blood-to-water
ratio of 1:2.4 (V/V) had good textural properties, water-holding capacity and color.

Effect of Controlled Freezing Point Storage Combined with Vacuum Packaging on Texture and Histological Structure of Beef
SUN Tian-li,ZHANG Xiu-mei,ZHANG Ping,LI Jiang-kuo,YUE Xi-qing
2013, 34(22):  327-331. 
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This study investigated the effect of storage at controlled freezing point temperature (Cv), 0 ℃ (Zv) or 4 ℃
(Fv) combined with vacuum packaging on texture profile analysis (TPA) parameters (hardness, springiness, cohesiveness,
gumminess and chewiness) and sarcomere length and myofibrillar fragmentation index (MFI) of beef. The results showed
that all other TPA parameters except springiness varied more slowly under Cv conditions than under Zv and Fv conditions.
Sarcomere length reached its minimum level on the 8th day of storage under Cv conditions but on the 1st day under Zv and Fv
conditions. MFI increased gradually with prolonged storage time, and showed a significant difference between Cv and either
Zv or Fv from the 4th day. The Cv treatment was effective for delaying the processes of beef stiffening and destiffening and
the texture and histological structure changed slowly during Cv storage, resulting in quality preservation of beef for a long
time. However, the other two storage temperatures (Zv and Fv) individually combined with vacuum packaging were much
less effective in improving the structure of beef.

Fabrication of Molecularly Imprinted Electrochemical Sensor for Determination of Nicotinamide in Beverage
Jian-Ping Li
2013, 34(22):  332-335. 
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In this paper, a sensitive sensor based on the molecularly imprinted polymer(MIP) of o-phenylenediamine was proposed, and its configuration and performance were studied. The progress of the electro polymerization is performed in a acetate buffer solution (pH = 5.7) containing 1.0mmol/L nicotinamide and 3.0mmol/L o-phenylenediamine on the surface of a glassy carbon electrode. The molecularly imprinted polymer membrane was characterized using cyclic voltammetry. The linear range is 0.01?mol/L ~ 1.1?mol/L with a detection limit of 4.5×10-9 mol/L. The sensor was sensitive, selective, easy in preparing with a low price. It was applied to determination of trace nicotinamide in beverage.

Preparation and Characterization of Amylose-Phospholipid Complex
LIU Yan-qi,XU Yin-long
2013, 34(22):  336-340.  doi:amylose;phospholipid;complex
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Amylose-phospholipid complex was prepared with short chain amylase and phospholipid. IR spectroscopy,
X-ray diffractometry and DSC analyses showed structural changes of the native amylase after this complexation reaction and
an absorption peak at 1730.04 cm-1, confirming the formation of complex. Moreover, the structure of this complex showed
V-shaped crystals and it contained 19.80% phospholipid.

Fabrication and Analytical Application of Three-Dimensional Paper-Based Microfluidics for Rapid Detection of Nitrite
XIAO Liang-pin,LIU Xian-ming,LIU Qi-shun,ZHONG Run-tao,ZHOU Xiao-mian,LIN Bing-cheng,DU Yu-guang
2013, 34(22):  341-345.  doi:10.7506/spkx1002-6630-201322069
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Medium-speed qualitative filter paper was employed to fabricate paper-based microfluidics and 3D paper-based
microfluidics were integrated by wax printing-bookbinding method; a nitrite indicator containing 63.4 g/L citric Acid, 8.61 g/L sulfanilamide
and 2.59 g/L N-(1-naphthyl) ethylenediamine coupled with a lab-prepared colorimetric detection device was used
for nitrite determination. The 3D paper-based microfluidics could rapidly test nitrite, and the image acquired was analyzed
using a gray model for gray intensity representing the concentration of nitrite. The linear range was 0–10 mg/L, with correlation
coefficient of 0.9920. The detection limit of the method was 2 mg/L, and the recovery of nitrite from spiked samples
was 91.4%–102.0%. After stored under normal conditions and 4 ℃ for 7 weeks, the color intensity of the paper-based microfluidics
for nitrite detection were little change. The 3D paper-based microfluidics can provide a simple, easy to use, low-cost
and sensitive approach for rapid detection of in foods with small sample consumption.

Development of a Blended Drink Based on Mixed Fermentation of Ganoderma lucidum and Flammulina velutipes
MIAO Jing-zhi,LI Zhen-yu,DONG Yu-wei
2013, 34(22):  346-352.  doi:10.7506/spkx1002-6630-201322070
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The mixed fermentation of Ganoderma lucidum and Flammulina velutipes was optimized for developing a
blended drink in this study. After centrifugation and filtration of the fermented broth suspending disrupted mycelia, the
filtrate was blended with citric acid, sucrose and honey, and the blend was then homogenized, filled and sterilized. An
optimized blended stabilizer was developed and the proportion of ingredients in the blended drink was optimized. The
sensory, physiochemical and microbial properties of this drink were investigated. The optimal medium composition for
mixed fermentation of the two strains consisted of (m/m) 3% corn meal, 0.25% peanut meal, 0.2% peptone, 3% glucose, 0.1%
yeast extract, 0.3% monopotassium phosphate and 0.15% mangnesinm sulfte at pH 6.5, and the optimal culture conditions
were 100 mL of the medium in a 250-mL vessel, 24 ℃, 110 r/min, and 8 d. A stabilizer composed of 0.25% CMC-Na, 0.04%
xanthan gum and 0.50% β-cyclodextrine was found to be optimal to stabilize the drink. The optimal formulation of this
blended drink was composed of (m/m)1.5% honey, 16% the above filtrate, 0.15% citric acid and 6% saccharose. The drink
developed in this study had a good taste and a full range of nutrients and met the national hygienic standards.

Odor Discrimination of Eight Shellfishes Using an Electronic Nose
DING Yuan,ZHENG Ping-an,MIAO Fang-fang,SU Xiu-rong
2013, 34(22):  353-356.  doi:10.7506/spkx1002-6630-201322071
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In the present study, an electronic nose was used to characterize and classify the odors of 8 different shellfishes.
By the methods of principle component analysis (PCA) and linear discrimination analysis (LDA), the data obtained were
analyzed using an SPSS software. The shellfishes were accurately discriminated from one another with a high degree of
discrimination. Further analysis indicated differences in their odors according to the results of data processing. Therefore
analysis of the data from an electronic nose enables discrimination of different shellfishes.