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25 June 2013, Volume 34 Issue 12
Enzymatic Extraction of Protein from Crayfish Head and Shell
WANG Yan,DENG Fang-ming*,LIU Yan,LIAO Quan,LIU Wen-qian
2013, 34(12):  1-5.  doi:10.7506/spkx1002-6630-201312001
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This paper describes the enzymatic extraction of protein from crayfish head and shell. Using one-factor-at-atime
and orthogonal array design, we established the optimum conditions for extracting protein from crayfish head and
shell as follows: 1:1.5 of papain/flavourzyme ratio with a total enzyme concentration of 1.0%, pH 6.5, 1:10 of solid/liquid
ratio, 50 ℃ and a hydrolysis duration of 3 h. The extraction efficiency of protein under the optimized conditions was 54.22%.

Separation and Preparation of Flavonoids from Zanthoxylum bungeanum by High-speed Countercurrent Chromatography
SHI Xue-ping,WU Liang-liang,ZHANG Wei-ming
2013, 34(12):  6-10.  doi:10.7506/spkx1002-6630-201312002
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Flavonoids from Zanthoxylum bungeanum were separated by high-speed countercurrent chromatography. The separation was performed using a two-phase solvent system composed of chloroform, methanol, n-butanol and water(4:3:0.5:2, V/V) at a flow rate of 2.0 mL/min, and rotation speed and detection wavelength were set at 850 r/min and 254 nm, respectively. Six flavonoids were detected by HPLC. The purities of peaks 1, 2, 3, 4, 5 and 6 were 72.7%, 67.8%, 89.6%,96.5%, 94.1% and 91.3%, respectively. Their structures were characterized as foeniculin, quercetin-7-glucoside, rutin and quercetin-3-galactoside by MS and 1H-NMR.

Separation and Purification of β-Cryptoxanthin from Satsuma Mandarin Peel
SUN Zhi-gao,JIANG Guo-ling,ZHANG Meng-meng,MA Ya-qin,LI Qin,TAN An-qun
2013, 34(12):  11-15.  doi:10.7506/spkx1002-6630-201312003
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In the present study, we investigated optimal conditions of saponification and column chromatography
for β-cryptoxanthin purification from satsuma mandarin. The optimal saponification conditions were found to be
saponification with 40 mL of KOH-ethanol (10 mg/100 mL) at 20 ℃ for 12 h with stirring at 400 r/min. The optimal
column chromatography conditions were 1:25 (mL/g), n-hexane-acetone-methanol (92.5:5:0.5, V/V) and 1.0 mL/min for
sample/silica gel ratio, eluant and flow rate, respectively. The purity of the β-cryptoxanthin under the optimized conditions
exceeded 90%.

Effects of Extraction Methods on Contents and Compositions of Ginsenosides from Cultivated Jilin Ginseng Extracts
ZHANG Yan-rong,ZHANG Shuai,FAN Hong-xiu,LIU Hong-cheng,ZOU Di,WANG Da-wei
2013, 34(12):  16-21.  doi:10.7506/spkx1002-6630-201312004
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The effect of different extraction methods, supercritical fluid extraction (SFE), ultrasound-assisted extraction and
heat reflux extraction, on the extraction efficiencies and compositions of 6 major ginsenosides including Rg1, Re, Rb1, Rc,
Rb2 and Rd from cultivated Jilin ginseng was investigated. The ginsenosides were determined by HPLC. The total yield of
ginsenosides extracted by SFE, ultrasound-assisted extraction and heat reflux extraction was respectively 0.8557%, 2.2938%
and 2.4804%, and the yields of Rg1, Re, Rb1, Rc, Rb2 and Rd were 0.1287%, 0.1169%, 0.2830%, 0.1090%, 0.1061%
and 0.1120% when using SFE, 0.3892%, 0.3414%, 0.8088%, 0.2932%, 0.3180% and 0.1432% when using ultrasoundassisted
extraction, and 0.3914%, 0.3396%, 0.8898%, 0.3300%, 0.3620% and 0.1676% when using heat reflux extraction,
respectively. In the HPLC chromatogram of the heat reflux extract, several peaks disappeared, suggesting the degradation
of malonyl ginsenoside. In addition to six common gensinosides, a small amount of unknown secondary ginsenosides were
also detected in the extracts from three methods. Based on this, we deduced that neutral ginsenosides were degraded to
different extents under SFE, ultrasound assisted-extraction and heat reflux extraction. The above results showed that there
was a significant difference in the extract yields and compositions of ginsenosides when different extraction methods were
employed. In respect to SFE, the extraction yields of ginsenosides were significantly lower than those observed when using
ultrasound-assisted extraction and heat reflux extraction. However, SFE had excellent advantages such as simpler separation
process, the absence of solvent contamination and better thermo-sensitive substance protection and higher re-utilization
value of the remaining residue.

Microwave-Assisted Extraction and Characterization of Konjac Glucomannan from Konjac Flour
2013, 34(12):  22-26.  doi:10.7506/spkx1002-6630-201312005
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The microwave-assisted extraction of konjac glucomannan (KGM) from konjac flour was studied. The
influence of extraction parameters including extraction temperature, microwave power and solid/liquid ratio on KGM
content was examined by one-factor-at-a-time and orthogonal array design. The optimal process conditions for KGM
extraction were found to be extraction at 90 ℃ and a microwave power of 700 W for 60 min with a solid-to-liquid ratio
of 1:160. The KGM content of crude extracts under the optimized conditions was 70.75%. Temperature significantly
affected the extraction of KGM. The optimized extraction process provided a stable extraction technique which had
the advantages of high KGM content, short extraction time and high antibacterial activity of konjac flour extracts.
The superiority of the microwave-assisted extraction method has been verified by infrared and scanning electron
microscopy (SEM).

Macroporous Resin Adsorption for Separation and Purification of ACE Inhibitory Peptides from Porcine Hemoglobin
DENG Hui-ling,ZHENG Jiong,KAN Jian-quan
2013, 34(12):  27-31.  doi:10.7506/spkx1002-6630-201312006
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Based on static and dynamic adsorption performance, DA201-C type macroporous resin was selected as a more
appropriate carrier to separate and purify ACE inhibitory peptides from the pepsin hydrolysate of porcine hemoglobin. The
optimal process parameters for dynamic adsorption and desorption were determined as follows: 60 mL of 40 mg/mL samples
at pH 5.0 and 0.5 mL/min of loading flow rate, followed by desorption with 75% ethanol at a flow rate of 1.0 mL/min.
The IC50 of the ACE inhibitory peptides obtained under the optimized conditions was 0.87 mg/mL. Comparison of static
adsorption and desorption with dynamic adsorption and desorption indicated that the static adsorption rate of ACE inhibitory
peptides on DA201-C was 59.4%, which was higher than the dynamci adsorption rate of 48.1%.

Optimal Infusion Conditions for γ-Aminobutyric Acid Instant Tea
XU Yong-quan,YIN Jun-feng,TAN Jun-feng,YUAN Hai-bo,LIN Zhi
2013, 34(12):  32-35.  doi:10.7506/spkx1002-6630-201312007
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One-factor-at-a-time and orthogonal array design were employed to optimize water temperature, infusion time
and tea type ( pan fried green, roasted green or green leaves) for γ-aminobutyric acid instant tea based on total solid yield,
the contents of tea polyphenols and γ-aminobutyric acid in tea infusion, color parameters L, a and b, turbidity and sensory
quality (color, aroma and taste). Data analysis with SPSS 13.0 software showed that the optimal infusion conditions for
γ-aminobutyric acid instant tea were 20 min infusion of roasted green tea with 60 ℃ water.

Optimization of Extraction Conditions for Anthocyanin Anthocyanins from Dark Maize
WANG Xu,QIN Hong-ni,YUAN Wen-juan,WANG Jiu-guang,WANG Guo-qiang,LIU Zhi-zhai,CAI Yi-lin
2013, 34(12):  36-39.  doi:10.7506/spkx1002-6630-201312008
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An orthogonal array design was applied to establish the optimum conditions of ethanol concentration, solidto-
liquid ratio, solvent pH, temperature and time for increased yield and purity of anthocyanins from grains of Super Dark
Maize (SDM). The results showed that maximum yield (18.71%) but minimum purity (A550nm/A275nm = 0.10) of anthocyanins
were observed under the conditions of 90%, 1:15 (g/mL), 1, 80 ℃ and 15 h for ethanol concentration, solid-to-liquid ratio, pH,
temperature and and time, respectively. The optimum extraction conditions to achieve maximum yield while increasing the purity of
anthocyanins were 90% ethanol acidified to pH 1.5 as the extraction solvent with a solid-to-liquid ratio of 1:15, 70 ℃ and 15 h.

Purification of Total Flavonoids from Hop (Humulus lupulus L.)
HU Jun-ping,IZZATGUL Ismayil,YANG Jian-hua
2013, 34(12):  40-44.  doi:10.7506/spkx1002-6630-201312009
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The purificaiton of total flavonoids from hop (Humulus lupulus L.) was investigated. Colorimetric determination
of total flavonoids was carried out with NaNO2-Al(NO3)3-NaOH. We compared the efficiencies of nine types of macroporous
adsorption resin for static adsorption and desorption of hop flavonoids. In addition, the effects of pH, concentration and
flow rate of sample and pH, concentration and dose of eluent on the purificaiton efficiency of flavonoids were examined.
Polyamide was identified as the most appropriate resin for purifying total flavonoids from hop. The optimal purification
conditions were obtained when 10 mL of sample was loaded onto an 1-g polyamide column at a flow rate of 1.0 mL/min
followed by desorption with 8 BV of 80% methanol. Under these conditions, the yield of flavonoids from hop was 32.69%
with a purity of 50.05%.

Preparation of Capsaicin Molecular Imprinting Polymers and Application to Solid Phase Extraction
WANG Zun-chen,YU Hai-ning,SHEN Sheng-rong,HOU Xiao-rong,SHAN Wei-guang
2013, 34(12):  45-50.  doi:10.7506/spkx1002-6630-201312010
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Molecular imprinting polymers (MIPs) were synthesized by bulk polymerization, using capsaicin as the template
molecule and 2-vinylpyridine (2-VP) and Acrylamide (AM) as the function monomers. The specific adsorption ability of the
molecularly imprinted polymers (MIPs) to capsaicin was evaluated by equilibrium binding experiments, saturated adsorption
time was assessed by saturated adsorption experiments and selective adsorption ability to capsaicin analogs was appraised
by selective adsorption experiments. The results showed that MIPs exerted the best adsorption efficiency to capsaicin
when the ratio of capsaicin:2-VP:AM was 1:2:2, with a adsorption capacity of 20.46 mg/g and a recognition factor of
3.05. Morevoer saturated adsorption time was 6 h and better selective recognition to capsaicin was found. In this study, the
elution efficiencies of eluents of different polarity for specific adsorption and non-specific adsorption of capsaicin in solid
phace extraction column of MIPs were investigated. The specific adsorption was kept while the non-specific adsorption was
discharged to the greatest extent when using chloroform as the eluent.

Extraction of Polysaccharides and Analysis of Ingredients in Mallotus furetianus Tea
SU Bing-xia,GE Hui-lin,DUAN Yun,YE Hai-hui
2013, 34(12):  51-55.  doi:10.7506/spkx1002-6630-201312011
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This paper describes a reasonable ultrasonic-assisted extraction (UAE) techinque for water-soluble
polysaccharides (WSPs) from Mallotus furetianus tea. Crude polysaccharides were deproteinized by the combined use
of Sevag reagent and protease. The optimum process conditions for enhanced UAE extraction of WSPs were 250 W, 40
min, 60 ℃, 15:1 (mL/g) and 30 min for ultrasonic power, ultrasonication time, temperature, solid/liquid ratio and hot
water extraction time, respectively. Under these conditions, the extraction yield of WSPs was 9.976%. Five extraction
parameters in decreasing order of their importance were ultrasonic power, ultrasonication time, temperature, extraction
time and solid/liquid ratio. The resulting crude extract gave rise to a deproteinization rate of 17.7%. Both Mallotus
furetianus tea and the remaining residue after WSPs extraction contained a small amount of water and showed no obvious
differences in the contents of soluble ash or insoluble ash, with good repeatability. The 15 elements detected in Mallotus
furetianus tea were K, Ca, Mg, Na, S, P, Ba, Mn, Fe, Ni, Zn, Sc, Cu, Cr and Li in the decreasing order of content. The
contents of K, Mg, Na, Mn, Zn, S and P in the WSPs were higher than in the residue, but Ba, Cr, Li, Fe, Cu, Ca, Sc and
Ni were richer in the residue.

Optimization by Response Surface Analysis of Microwave-Assisted Extraction and Hydroxyl Radical Scavenging Activity of Polysaccharide from Hovenia acerba Lindl
FENG Zi-li,DANG Ya
2013, 34(12):  56-60.  doi:10.7506/spkx1002-6630-201312012
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Objective: To establish optimal conditions for the microwave-assisted extraction of ploysaccharide from
Hovenia acerba Lindl by means of mathematical modeling and to explore the hydroxyl radical scavenging activity of the
polysaccharide extract from Hovenia acerba Lindl. Methods: Box-Behnken design was used to develop a regression model
indicating the effect of three key process parameters including microwave power, solvent-to-solid ratio and extractiom time
on the extraction efficiency of polysaccharide. Based on the model, these extraction prameters were optimized by response
surface analysis. The antioxidant activity in vitro of the polysaccharide obtained was evaluated based on the reaction
between hydroxyl radical and salicylic acid. Results: The optimal extraction conditions were obtained as follows: 504.3 W,
25:1 and 21.9 min for microwave power, solvent-to-solid ratio and extraction time, respectively. The extraction efficiency
of polysaccharide under these conditions was 10.84%. The resulting polysaccharide had strong hydroxyl radical scavenging
activity with an IC50 of 205.87 μg/mL.

Weight-reducing Effect of Bacterial Cellulose and Its Application in Bacterial Cellulose Yogurt
ZHANG Ji-liang,HE Xin,LI Yuan-jing,TIAN Hua,LEI Hong*
2013, 34(12):  61-66.  doi:10.7506/spkx1002-6630-201312013
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This study was designed to examine the weight-reducing effect of bacterial cellulose (BC) in mice. For this
purpose, mouse models of obesity were created and administered by gavage with BC at high, medium and low doses of 500,
417 mg/kg and 333 mg/kg, respectively, once a day for 2 continuous weeks. After the end of the administration period, blood
samples from all mouse were taken for analysis of blood lipid indexes. Important process parameters for producing BC
supplemented yorghurt were established through sensory evaluation and texture analysis. The results indicated that the highdose
and medium-dose BC groups as well as the positive control group exhibited a significant weight-reducing effect in mice
with nutritional obesity (P < 0.01). The levels of serum TG, TC, and LDL significantly declined in all mice that fed BC,
regardless of dose (P < 0.05), whereas the level of serum HDL-C significantly rose. The addition of 3% BC with an average
particle size of 0.1 cm and 7% white sugar to milk (both proportions relative to he mass of milk) gave rise to remarkably
improved flexibility and cohesiveness of yogurt. Yogurt products supplemented with each dose of BC were proved to have
an obvious weight-reducing function in alimentary obesity mice. In all, we conclude from the current research that both BC
and BC supplemented yogurt have significant weight reducing effects in alimentary obesity mice. Furthermore, the quality
of yogurt can be well improved by BC addition.

Effect of Twin-Screw Extrusion Parameters on the Sensory Quality of Extruded Cereals
WANG Li-juan,YANG Xue-fei,HUANG Yi,JIANG Shao-tong,ZHENG Zhi
2013, 34(12):  67-70.  doi:10.7506/spkx1002-6630-201312014
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Extruded cereals were produced from millet, glutinous rice, soybean, wheat, oat, brown rice and wheat bran flours
using a DS32-I twin-screw extrusion machine. The sensory quality of extruded cereals was investigated with respect to three
operating parameters including moisture content, barrel temperature distribution, screw rotation speed and feeding rotation
speed. These variables were ranked in descending order of importance: moisture content, barrel temperature distribution,
feeding rotation and speed screw rotation speed. Under the conditions of 16%, 150 r/min, 80 ℃ then 145 ℃ and finally 165 ℃
and 20 r/min for moisture content, screw rotation speed, barrel temperature distribution and feeding rotation speed, respectively,
The extruded cereals had improved sensory quality, a faint aroma of cereals, a light yellow color and a delicate taste. In addition,
they easily formed a paste in water without agglomeration or settlement but with good dispersity.

Production and Shelf Life of Red Glutinous Rice Soft Cookie
LIU Jing-jing,CAI Jing,XU Zhe-xian,QIAN Li-dan,FANG Jiao,HAN Yao-ping,WANG Xue-feng,DAI Yang-jun
2013, 34(12):  71-75.  doi:10.7506/spkx1002-6630-201312015
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The production and shelf life of red glutinous rice soft cookie with partial replacement of red glutinous rice
for wheat flour were studied. The effect of red glutinous rice, white sugar and oil concentration, whipping time and
baking temperature on the sensory quality of the cookie was explored by one-factor-at-a-time design. The optimal process
parameters were determined as follows: 100% of low gluten flour, partial replacement of 18% of low gluten flour with red
glutinous rice, 36% of white sugar, 75% of oil and fat (consisting of 70% of butter, 14% of shortening and 16% of cream),
36% of egg, 0.2% of calcium propionate, 50 min of whipping, baking at an upper temperature of 150 ℃ and an lower
temperature of 130 ℃, and 20 min of baking. The shelf life of the cookie obtained under the optimized conditions was
predicted by ASLT method to be 150 d.

Optimization of Plastein Synthesis and Amino Acid Analysis of Products
LIU Zhen-chun,FENG Jian-guo,LIU Chun-meng,FAN Guo-ting,SU Tong
2013, 34(12):  76-81.  doi:10.7506/spkx1002-6630-201312016
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The synthesis of plastein from hydrolysates of soybean protein isolate and oat protein isolate was investigated
in this work. Of the reaction conditions substrate concentration, temperature, pH and time, 3 were identified as main
variables by one-factor-at-a-time design. The main variables were optimized by response surface methodology based on a
Box-Behnken design. Meanwhile the synthetic plastein was analyzed for animo acid composition. The observed yield of
plastein was 31.46% under the optimal conditions of 31 g/100 mL of substrate concentration, 45 ℃, pH 4.7 and 12 h. The
plastein obtained exhibited significantly different amino acid composition in comparison with both starting raw materials; in
particular, the content of essential amino acids was increased by 17.7% and 16.5%, respectively. Therefore, the nutritional
value of both raw materials was increased.

Preparation of Time-Temperature Indicator Reaction System Based on Glucoamylase
ZHENG Guang-lin,QIAN Jing*,FENG Qin
2013, 34(12):  82-85.  doi:10.7506/spkx1002-6630-201312017
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Color changes occuring during the course of reaction between glucoamylase and starch in the presence of iodine
solution as an indicator display the cumulative effects of time and temperature. A time-temperature indicator reaction
system was developed with 10 mL of 40 g/L maltodextrin as reaction substrate, 3 mL of 1 g/L iodine solution and variable
amounts of glucoamylase. The time-temperature indicator was widely applicable for products at different times of cold chain
transportation. The reaction system with 50 μL of glucoamylase was suitable for low temperature controlled packaging for
3 to 4 d at about 4 ℃, and the activation energy was found to be 75.94 kJ/mol. This system had potential application for
chilled fresh meat, which is vulnerable to quality deterioration caused by lipid peroxidation.

Preparation and Application of Octenylsuccinate Soybean Dietary Fiber Ester
YANG Jing,ZHENG Wei-wan*,GAO Yuan-yuan,XUE Jun,FENG Tao-lin,CHEN Qian-wen,LIU Fan
2013, 34(12):  86-89.  doi:10.7506/spkx1002-6630-201312018
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The present study was intended to investigate reaction conditions for esterifying dietary fiber from soybean dregs
with octenylsuccinate and to explore the practical application of the esterification product in detergent. The optimum reaction
conditions were found to be 1 h of reaction at 55 ℃ in the presence of 10% octenylsuccinate. A degree of substitution (DS)
of 0.0681 was obtained under these conditions. Detergent paste prepared with the octenylsuccinate ester as main filling
material and active compounds had strong detersive power as an excellent product friendly to both the environment and the
human body.

Optimization by Orthogonal Array Design of Decolorization of Soybean Peptide
DAI Li-jun,LIANG Yun-xiang
2013, 34(12):  90-94.  doi:10.7506/spkx1002-6630-201312019
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In this study, an optimized method was presented for the decolorization of soybean peptide by stepwise treatment
with activated carbon and AB-8 resin. An orthogonal array design was used to optimize activated carbon amount, time,
temperature and pH based on decolorization rate and peptide loss rate. The optimal conditions for activated carbon treatment
were determined to be decolorization at 55 ℃ for 50 min with the addition of 2.0% of activated carbon adjusted to pH
8.0, giving rise to a decolorization rate of 57.13% and a peptide loss of 11.37%. Further decolorization was performed by
9 h treatment with AB-8 resin (0.5 g/mL), resulting in a decolorization rate of 57.99% and a peptide loss of 16.19%. The
total decolorization rate and total peptide loss were 81.97% and 26.74%, respectively, after the two-stage decolorization.

Preparation of Perilla Seed Oil Powder and Its Antioxidant Activity
JIANG Hui-juan,Lü Xiao-lan,HUANG Gan-hui
2013, 34(12):  95-98.  doi:10.7506/spkx1002-6630-201312020
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Perilla seed oil (PSO) powder was prepared by physical adsorption with cross-linked esterified porous starch
(CEPS) as the wall material. Several process conditions were optimized by one-factor-at-a-time and orthogonal array design
to achieve the highest embedding efficiency (EE). The optimum conditions for preparing PSO powder were established as
follows: embedding at 55 ℃ for 50 min with a PSO/ CEPS ratio of 4:1. PSO powder under the optimized conditions gave
rise to the highest EE of more than 30%. The peroxide values (POV) of PSO and the PSO powder under the optimized
conditions were determined under accelerated oxidation conditions. From the results obtained, we found that the lipid
oxidation time of the PSO powder was substantially prolonged in comparison with native PSO, indicating enhanced
oxidation resistance.

Effect of Twin-Screw Extrusion Parameters on Water Absorption Index of Extruded Cereals
WEI Zai-hong,ZHOU Yang,WANG Dan-hui,CAO Xuan,CHANG Ya-ning
2013, 34(12):  99-103.  doi:10.7506/spkx1002-6630-201312021
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Response surface analysis was used to establish optimal process parameters to obtain maximum water absorption
index (WAI) of extruded cereals. Under the optimized conditions of 238.2 r/min, 26.8%, 86.1 ℃, then 96.1 ℃ and finally
106.1 ℃ for screw rotation speed, moisture content and barrel temperature distribution, respectively, the predicted WAI
value of extruded cereals was 4.0350, which indicated a relative error of 1.01% compared to the experimental value of 3.9945.
This demonstrates the reliability of the optimized extrusion. Sensory evaluation showed that the resulting extruded cereals
had similar quality to commercial quality rice from northeast China. Moreover, compact microporous structure was observed
for the extruded cereals under scanning electron microscopy (SEM).

 

Extraction and Antioxidant Activity of Total Flavonoids from Leaves of Vitis viniferal L. Grown in Xinjiang GULIBAHAER Ababaikeli
GULIBAHAER Ababaikeli
2013, 34(12):  104-108.  doi:10.7506/spkx1002-6630-201312022
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The extraction of total flavonoids from leaves of Vitis viniferal L. was optimized by orthogonal array design with
the objective of developing a sample preparation method for the spectrophotometric determination of total flavonoids with rutin
as a standard reference material. Four extraction parameters were ranked in decreasing order of importance as follows: time,
ethanol concentration, temperature and solid-to-solvent ratio, and their optimal conditions were 100 min, 50%, 70 ℃ and 1:50,
respectively. The total flavonoids obtained under the optimized conditions possessed free radical scavanging activity against
DPPH, hydroxyl and superoxide anion radicals in decreasing order as well as reducing power.

Determination of Nitrite in Food by Carbon Paste Electrode Modified with Ni/Mg/Fe Ternary LDH
SHI Feng,LI Kan,JIA Jin-ping*,WANG Ya-lin
2013, 34(12):  109-113.  doi:10.7506/spkx1002-6630-201312023
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Hydrotalcite-like compounds are layered double hydroxide composite metal compounds (LDHs), which show good
electrical adsorption and electrocatalytic properties. In this study Ni/Mg/Fe ternary LDH was synthesized by coprecipitation
and mixed with carbon paste to prepare carbon paste electrodes for detection of nitrite in food. The results showed that the
synthesized LDH had obvious adsorption and catalytic oxidation effects on nitrite iron and the electrochemical performance
of the chemically modified carbon paste electrode was greatly improved. There was a good linear relationship (correlation
coefficient was higher than 0.998) over the concentration range of 5-700 μmol/L and the minimum detection limit was
0.49 μmol/L. The conditions of scanning potential, scanning speed, accumulation time, pH and the amount of modifier were
also optimized to further improve the detection sensitivity. The method was further applied to analyze food samples, and the
average recovery rates were (100 ± 10)%, which showed good detection peformance. Compared with other detection methods,
this method showed the advantages of high stability, reproducibility and sensitivity, rapid response, wide liner range, little
interference and simple instruments. The new electrode can be used in pratice with good application prospects.

Development of Colloidal-Gold Immunochromatographic Strip for Rapid and Quantitative Detection of Clenbuterol in Swine Urine
LI Chao-hui,LUO Wei,XU Bo,LIU Wen-juan,XU Heng-yi,XIONG Yong-hua
2013, 34(12):  114-118.  doi:10.7506/spkx1002-6630-201312024
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We report on the development of a rapid and quantitative colloidal gold immunochromatographic strip for
clenbuterol (CLE) detection in swine urine. The parameters that influenced the assay performance of immunochromatographic
strip were optimized by an orthogonal array design L9 (3)3 and a quantitative method based on T/C ratio was developed to
detect CLE residue in swine urine. The limit of detection (LOD) of immunochromatographic strip for CLE in swine urine was
0.22 ng/mL and a linear calibration curve was obtained over the concentration range of 0.1 to 2.0 ng/mL with a half maximal
inhibitory concentration (IC50) of 0.36 ng/mL. For spiked blank urines, mean recoveries were (102.4 ± 7.8)% at 0.5 ng/mL,
(96.5 ± 6.8)% at 1.0 ng/mL and (103.3 ± 7.2)% at 1.5 ng/mL, respectively. In conclusion, we have successfully developed a
rapid and quantitative method based on colloidal gold immunochromatographic strip for CLE residue in swine urine.

Microwave-Assisted Extraction, Purification and Identification of Polysaccharide BBP0-2 from Blueberry Fruit
MENG Xian-jun,CHANG Yu,SUN Xi-yun*,LIU Xiao-jing,SHEN Yi-xiao
2013, 34(12):  119-124.  doi:10.7506/spkx1002-6630-201312025
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The microwave-assisted extraction of polysaccharide from blueberry fruit was optimized by respons surface
methdology in this work. Hydrogen peroxide, trichloroacetic acid-n-butanol and polyamide column chromatography were
compared for their efficiencies in removing pigment and protein from crude polysaccharide from blueberry fruit. After
further purification by DEAE-cellulose 52 column and Sephadex G-100 column chromagraphy, we analyzed the purity
by HPLC and monosaccharide composition of purifed polysaccharide by GC. The optimal conditions for polysaccharide
extraction were found to be 1:8 (g/mL), 600 W and 30 min for solid/solvent ratio, microwave power and extraction time,
respectively. The extraction efficiency of ploysaccharide under the optimized conditions was 3.32%. Polyamide column
chromatography was considerably more effective than the traditional methods with hydrogen peroxide and trichloroacetic
acid-n-butanol. Three polysaccharides were separated from DEAE-cellulose 52 column chromatography, namely BBP0,
BBP1 and BBP2. BBP0 were further separated by Sephadex G-100 column chromagraphy to obtain BBP0-2, which was
composed of arabinose, galactose, xylose and glucose with a molar ratio of 2:5:3:4.

Determination of (-) and (+)-Gossypols in Cottonseed Kernel by High-Performance Liquid Chromatography with Chiral Pre-column Derivatization
HE Xiao-wen,LI Xin-xia,YAO Jun,ZHANG Huang-tao,XUE Hai-yan
2013, 34(12):  125-128.  doi:10.7506/spkx1002-6630-201312026
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An HPLC with chiral pre-column derivatization method was developed for the determination of (-)-and
(+)-gossypols in cottonseed kernel. Chromatographic separation was carried out on an Agilent XDB-C18 column (250
mm × 4.6 mm, 5 μm) with a mobile phase which consisted of 80% acetonitrile and 20% 10 mmol/L KH2PO4 buffer adjusted
to pH 3.0 with H3PO4 at a flow rate of 1.0 mL/min. (R)-(-)-2-amino-1-propanol was used as a chiral separation reagent
and the detection wavelength was set at 247 nm. A good linear relationship between HPLC peak area and (-)-gossypol
concentration was obtained over the range of 1.96 to 29.46 μg/mL, and the mean recoveries of (-)-gossypol at three spiked
levels were 99.7% -104.1%, with RSDs rangeing from 1.50% to 3.07%. As for (+)-gossypol, the linear range was 1.82-
27.30 μg/mL, mean recoveries at three spiked levels were 100.6%-105.8% with RSDs ranging from 1.08% to 3.53%. The
method provides simplicity, rapidity, sensitivity and accuracy, and therefore is applicable to the determination of (-)-and
(+)-gossypols in cottonseed kernel and related foods.

PCR-DGGE Analysis of Microbial Diversity of Homemade Pickles in Sichuan Region
ZHANG Xian-qin,ZHANG Xiao-ping,AO Xiao-lin,LIU Xiao-qian,PU Biao
2013, 34(12):  129-134.  doi:10.7506/spkx1002-6630-201312027
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The microbial diversity of 20 homemade pickles in Sichuan region was analyzed by PCR-DGGE. Meanwhile,
representative stripes were selected to be sequenced for construction of a phylogentic tree based on their sequences.
The results revealed abundant bacteria species but a few fungi in the pickles. The genus Lactobacillus was the dominant
populations while uncultured bacteria were sub-dominant populations, which accounted for 56% and 32% of the total
bacteria species, respectively. Lactobacillus plantarum played an important role in pickle fermentation. The closely related
species of Meyerozyma guilliermondii and Kodamaea ohmeri were the predominant fungi in Sichuan homemade pickles.

An Improved Enzyme Inhibition Method for Detection of Peptide Residues in Garlic
WANG Wen,LIU Jin*,SHENG Wei-nan,CAI Zi-jin,XU Ke-xin
2013, 34(12):  135-139.  doi:10.7506/spkx1002-6630-201312028
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An improved method was proposed to rectify false positive (FP) results from the determination of
organophosphorus and carbamate pesticides in garlic by enzyme inhibition method. Sample solutions were adjusted to the
optimum pH prior to detection, considerably reducing the inhibition effect of formed sulfides on acetylcholinesterase (AChE)
while allowing the determination of organophosphorus and carbamate pesticides. The results obtained for the determination
of blank garlic and pesticide solutions under different pH conditions indicated that pH adjustment in the optimum range of
about pH 8.0 to 9.0 of sample solutions was very effective for avoiding FP results without affecting qualitative identification
of organophosphorus and carbamate pesticides. For garlic samples spiked with varying conditions of 8 pesticides
(methamidophos, trichlorphon dimethoate, carbofuran, phoxim, chlorpyrifos, dichlorvos and carbary), the results obtained
at pH 9.0 showed a 91.7% consistency with those observed at pH 7.5. In conclusion, the improved pretreatment method
presented by adjusting pH in this study is simple, low-cost and effective and applicable for in situ rapid detection and can
also be expanded to other sulfur-containing vegetables.

Amino Acid and Fatty Acid Profiles of Muscles of Zhedong Geese of Different Ages
ZHENG Xiao,PAN Dao-dong,CAO Jin-xuan
2013, 34(12):  140-142.  doi:10.7506/spkx1002-6630-201312029
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This study was designed to detect the contents of amino acids and fatty acids in muscles of Zhedong goose
slaughtered at different ages. The results showed that the contents of total amino acids and tasty amino acids in muscles of
120-day-old geese were significantly higher than in mucles of 35-day-old and 70-day-old geese (P < 0.05). In addition, the
contents of total amino acids and tasty amino acids in mucles of 35-day-old goose were significantly higher than in muscles
of 70-day-old goose (P < 0.05). Moreover, the contents of saturated fatty acids (SFA) in 35-day-old geese were extremely
significantly lower than in muscles of 70-day-old and 120-day-old geese (P < 0.01), whereas the contents of unsaturated
fatty acids (UFA) in 35-day-old geese were extremely significantly higher than in mucles of 70-day-old and 120-dayold
geese (P < 0.01). The contents of polyunsaturated fatty acids (PUFA) and essential fatty acids (EFA) were extremely
significantly decreased (P < 0.01) with increasing age.

Uncertainty Evaluation for the Determination of Cholecalciferol in Infant Formula Milk Powder by Ultra Performance Liquid Chromatography
FAN Yao,HUANG Cui-li,WANG Li-qing,REN Guo-pu,ZHOU Gui-ping,CHEN Hong-tao
2013, 34(12):  143-146.  doi:10.7506/spkx1002-6630-201312030
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Based on JJF 1059—1999 Evaluation of the Uncertainty of Determination and Expression, a mathematical model
was established to assess the uncertainty of analyzing cholecalciferol (VD3) in infant milk powder by ultra performance
liquid chromatography (UPLC). Factors contributing to the uncertainty were analyzed, quantified and synthesized. The
expanded uncertainty of VD3 determination for 10.0 g of samples was 0.2091 μg. Our results showed that the uncertainty
of measurement was mainly caused by the preparation of standard solution, the establishment of the standard curve and the
uncertainty of stochastic factors during the determination of samples. The evaluation method is reasonable, clear, simple,
accurate, and suitable for the evaluation of uncertainty in UPLC determination.

Analysis of Volatile Compounds in Sanquan Braised Pork with Preserved Vegetables by Simultaneous Distillation Extraction and Gas Chromatography-Mass Spectrometry
CHENG Yue, XU Xiao-lan,ZHANG Ning,CHEN Hai-tao*,SUN Bao-guo,HUANG Ming-quan
2013, 34(12):  147-150.  doi:10.7506/spkx1002-6630-201312031
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The volatile compounds in Sanquan braised pork with preserved vegetables was extracted by simultaneous
distillation extraction (SDE) and then analyzed by gas chromatography-mass spectrometry (GC-MS). Totally 57 volatile
flavor compounds were identified including 10 hydrocarbons, 6 alcohols, 19 aldehydes, 4 ketones, 4 esters, 1 ether, 4 acids,
2 phenols and 7 nitrogen- or sulfur-containing or heterocyclic compounds, accounting for 3.5117%, 46.9174%, 13.5089%,
0.7795%, 5.5572%, 0.1286%, 0.8347%, 0.1310% and 3.1580% of the total amount of volatile compounds, respectively.
Among these compounds, aldehydes, ethers, nitrogen-and sulfur-containing and heterocyclic compounds were the important
flavor compounds in Sanquan braised pork with preserved vegetables.

A New Method for Detection of Acid Value of Laver Products
GUO Ying-ying,SHENG Xiao-feng,WANG Lian-zhu,SHANG De-rong,ZHAO Yan-fang,ZHAI Yu-xiu
2013, 34(12):  151-155.  doi:10.7506/spkx1002-6630-201312032
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The acid value is an important indicator to judge the quality of products. This paper reports on the
establishment of a new method for the detection of acid value of laver products. Compared with stirring and sonification,
Soxhlet extraction had higher extraction efficiency while avoiding interferences from oxidation products formed during
the extraction process. Separation of the oil and aqueous phases was achieved by the addition of a proper amount of
neutral saturated NaCl solution to the organic solvent dissolving the oil from laver so that the titration end could be clearly
identified. Based on this, a new method was presented for the detection of acid value of dark and dried seaweed products.
The method was validated by detecting the acid value of different processed laver products by improved volumetric
analysis to obtain RSDs between 0.6% and 7.1%. In conclusion, the new method presented in this study is simple,
accurate and applicable for a wide range of samples.

Spectrophotometric Determination of Manganese in Cooking Wine Samples by Oxidation of Chromotrope 2B
SHA Ou,CHEN Li,MA Wei-xing
2013, 34(12):  156-159. 
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A new spectrophotometric method for determining manganese in cooking wine was established by oxidation of
chromotrope 2B. In the presence of sodium bismuthate, all low-valent Mn ions in samples were oxidized to form to Mn (Ⅶ), which
oxided chromotrope 2B at room temperature in sulfuric acid medium resulting in fading. The most considerable reduction in the
absorbance at 515 nm was observed, which was directly proportional to Mn (Ⅶ) concentration. The absorbance obeyed Beer’s law
in the Mn (Ⅶ) concentration range of 0.05 to 5.0 μg/mL with an apparent molar absorption coefficient of 2.05 × 104 L/(mol•cm).
The recovery of the developed method for spiked samples of commercial liquor and cooking wine ranged between 98.5% and
101.9%, and the results obtained were consistent with those reported with ICP-AES.

Simultaneous Determination of 3 Antioxidants in Foods by Gas Chromatography-Tandem Mass Spectrometry Coupled with Gel Permeation Chromatography
CAO Shu-rui,XU Fen,ZHANG Lei,LI Xian-liang,WANG Guo-min,MING De-wang,YUAN Ruo
2013, 34(12):  160-164.  doi:10.7506/spkx1002-6630-201312034
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A novel method has been established for the rapid separation and determination of 3 antioxidants (TBHQ, BHA and
BHT) in foods. The target analytes were extracted with hexane-saturated acetonitrile and the extract was purified by gel permeation
chromatography (GPC). The analytes were separated on a TR-35ms column (30 m × 0.25 mm, 0.25 μm) and detected by tandem
mass spectrometry with EI under multiple reaction-monitoring (MRM) mode. An excellent linearity (r > 0.99) was observed in
the concentration range of 0.05 to 10 mg/L for each antioxidant. The recovery rates ranged from 77.6% to 95.4% at three
levels of 0.5, 1.0 mg/L and 2.0 mg/L, with relative standard deviations (RSDs) of 2.7%-8.5%. The limits of detection were
0.03-0.1 mg/kg (n = 3) for these analytes. The established method is rapid, precise, sensitive, efficient and applicable for
the analysis of TBHQ, BHA and BHT in foods.

On-line HPLC Determination of Antioxidants in Fruit Juice
ZHANG Qiang,ZHANG Jing-fang,SU Yin-quan
2013, 34(12):  165-170.  doi:10.7506/spkx1002-6630-201312035
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An on-line HPLC method was developed to analyze natural antioxidants in a mixed juice by testing ABTS
radical scavenging activity. Rutin was used as a model antioxidant. Optimized system settings for improved RSN (signal/
noise) were obtained when 0.32 mmol/L ABTS radical solution was flowed through a 10.0 m reaction coil at a flow rate
0.5 mL/min. The limits of detection of the method for rutin, ascorbic acid, quercetin and α-tocopherol were in the range of
0.12-0.37 μmol/L. About 20 antioixdants were detected in the tert-butyl methyl ether of a commercial mixed juice by this
method. The most dominant antioxidants in the extract were chlorogenic acid and a compound similar structure. This method
is simple, convinent, fast and suitable for online assay of soluble antioxidants.

Determination of Malachite Green and Its Metabolite Leucomalachite Green in Aquatic Fingerlings by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry (UPLC-ESI-MS/MS)
TIAN Xiu-hui,YU Zhao-qiang,CHEN Wei,REN Chuan-bo,ZOU Rong-jie,ZHANG Hua-wei
2013, 34(12):  171-177.  doi:10.7506/spkx1002-6630-201312036
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A UPLC-ESI-MS/MS method was established for rapid determination of malachite green (MG) and its metabolite
leucomalachite green (LMG) in aquatic fingerlings with quantification by isotope-labeled internal standard method. UPLC
and MS/MS analytical conditions were examined and optimized by a series of experiments. Samples were extracted with
acetonitrile, purified on a neutral Al2O3 solid phase extraction cartridge. All eluates were collected and blown to dryness under a
nitrogen stream. The residue was re-dissolved in acetonitrile and ammonium acetate (1+1), sonficated and filtered prior to UPLC
analysis. The mobile phase was composed of A (acetonitrile) and B (5 mmol/L of ammonium acetate containing 0.1% formic
acid) at a flow rate of 0.25 mL/min. The analytes were finally detected and quantified using a triple Quadrapole MS/MS system
in positive polarity multiple reaction mode. Malachite green and leucomalachite green showed good linearity over the range of
0.5 to 20.0 ng/ mL with correlation coefficient of 0.9991 and 0.9999, respectively. The limits of detection of this method were
0.03 μg/kg for malachite green and leucomalachite green, and limits of quantification were 0.10 μg/kg. The average recoveries
at three spiked levels (0.10, 1.0 μg/kg and 2.0 μg/kg) ranged from 84.3% to 100.7% with relative standard deviations from
4.12% to 9.18%. In addition, the method showed advantages of simplicity, sensitivity and accuracy, and could be applied for
simultaneous determination of malachite green and leucomalachite green in aquatic fingerlings.

Lipophilic Bioactive Components in Queen Bee Larvae
XU Xiang,GAO Yan-xiang
2013, 34(12):  178-181.  doi:10.7506/spkx1002-6630-201312037
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Lipids from fresh queen bee larvae were extracted and separated by column chromatography. A comprehensive
analysis of the chemical composition of fatty acids and other lipophilic compounds was carried out. The results showed that
the queen bee larvae lipids were composed of 74.4% triglyceride with palmitic acid (43.16%) and oleic acid (40.70%) as
dominant fatty acids. Other neutral lipids and phospholipids contained a high amount of capric acid. In addition, queen bee
larvae also contained various types of sterol compounds such as 24-methylene cholesterol (57.67%), campesterol (4.76%),
β-sitosterol (16.56%), Δ5-avenasterol (19.45%) and cycloartenol (1.56%). Moreover, queen bee larvae comprised rich
coenzyme Q10 and phospholipids, in which the phosphatidyl ethanolamine content was (1299.65 ± 50.12) mg /100 g lipid.

One-Step Real-Time Reverse Transcription PCR for Detection of Food-Borne Salmonella
ZHOU Xiao-qing,LI Miao-yun,LIU Jie,ZHAO Gai-ming*,LIU Yan-xia,TIAN Wei,HUANG Xian-qing,GAO Xiao-ping
2013, 34(12):  182-187.  doi:10.7506/spkx1002-6630-201312038
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The objective of this study was to develop and apply a one-step real-time reverse transcription PCR (real-time RTPCR)
assay for the specific detection of Salmonella. A pair of primers was designed using a Salmonella spp. specific 284-bp
fragment of the invA gene (GeneBank ID: AE008832) as the target sequence. The reaction system and conditions of real-time
RT-PCR were optimized. The specificity, sensitivity and repeatability of the RT-PCR method were analyzed. Pork artificially
contaminated with Salmonella were detected using the new method and traditional method, and the results obtained were
compared. The optimal reaction conditions were 42 ℃ for 5 min, 95 ℃ for 10 s, 95 ℃ for 5 s, and then 67 ℃ for 34 s for 40
cycles; both the optimal concentrations of forward primer and reverse primer were 0.16 μmol/L. Results showed that the new
method was 100% specific. The sensitivity of the method was sufficient to detect 1.5 × 102 CFU/mL of Salmonella in pure
culture with good stability and repeatability. The results of detection of artificially contaminated foods were in accordance
with those obtained with the traditional method. This method could prevent RNAnase effectively and it was proved to be a
simple method for the detection of food-borne Salmonella.

Determination of Four Arsenic Species in Bee Pollen by High Performance Liquid Chromatography-Hydride Generation-Atomic Fluorescence Spectrometry
WANG Su-fen,CHEN Fang,WANG Peng,WU Li-ming
2013, 34(12):  189-193. 
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This paper describes a high performance liquid chromatography- hydride generation-atomic fluorescence
spectrometry (HPLC-HG-AFS) method for the determination of arsenite (AsⅢ), monomethylarsonic acid (MMA),
dimethylarsinic acid (DMA) and arsenate (AsⅤ) in bee pollen. Sample preparation was achieved by ultrasonic extraction
with 0.20 mol/L sulfuric acid. The detection limits for AsⅢ, DMA, MMA and AsⅤ were 1.0, 2.1, 1.2 and 3.1 μg/kg,
respectively, and recoveries at two spiked levels were in the range of 79%–100% with relative standard deviations (RSDs)
of 4.5%, 2.3%, 11.0% and 7.7%, respectively. In conclusion, we have established a good, fast qualitative and quantitative
method for analysis of arsenic compounds in bee pollen with high sensitivity and good accuracy.

Development and Application of Fluorescence Probe Method for Superoxide Anion Radical Detection
ZHAO Yong-qiang,LIN Hong,LI Lai-hao,YANG Xian-qing,HAO Shu-xian,ZHANG Mu-tian
2013, 34(12):  194-198.  doi:10.7506/spkx1002-6630-201312040
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A novel fluorescence probe 2-APC was synthesized based on nucleophilic substitution reaction of 2-aminopyridine
and 2-pyridinecarbaldehyde in this study. The reaction product was characterization by melting test, elemental analysis,
infrared spectrum and 1HNMR. A fluorescence probe method for superoxide anion radical detection was established using
the probe. The optimum reaction conditions were pH 8.2, 40 ℃ and 40 min. The conditions of fluorimetric determination
were established as follows: λex = 295 nm, λex = 365 nm and slit width = 5 nm. In the range from 0.4 × 10-6 to 8.0×10-6 mol/L,
relative fluorescence intensity (y) and pyrogallol concentration (x) showed a good linear relationship: y =37.567x + 55.581,
R2 = 0.9834. Superoxide anion radical (O2 - •) scavenging activity of L-ascorbic acid was evaluated using the method and an
IC50 of 0.182 mmol/L was obtained.

Determination of Peroxide Value of Edible Oils by Ultraviolet Spectrophotometry
QIN Xiao-yuan,ZHANG Jian-xin,YU Xiu-zhu*,LI Qing-hua,XU Chun-jin
2013, 34(12):  199-202.  doi:10.7506/spkx1002-6630-201312041
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An ultraviolet spectrophotometric method for determining perioxide value (POV) of edible oils was developed
based on the stoichiometric reaction of hydroperoxides with triphenylphosphine (TPP) showing characteristic adsorption
at 264 nm to TPPO showing characteristic adsorption at 266 nm. The presented prediction equations for TPPO were
validated with known and unkown samples, and analyzed in comparison with the national standard method (iodimetry).
Very comparable results of POV were obtained by both methods. In conclusion, the spectrophotometric method may be a
promising alternative to the national standard method for POV determination of edile oils.

Screening and Identification of Antioxidants in Glycyrrhiza Extract Rich in Glycyrrhizine by High Performance Liquid Chromatography Coupled with Post Column DPPH Assay
XING Zhen-zhen,MENG Qing-yan,LU Ya-ling,ZHANG Hong-xi,SHEN Xue-hua,LIU Wen-jie
2013, 34(12):  203-207.  doi:10.7506/spkx1002-6630-201312042
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A new method based on HPLC online scavenging DPPH radical activity and HPLC-MS/MS method for
the identification of antioxidants from glycyrrhiza extract rich in glycyrrhizine was developed. The glycyrrhiza extract
was separated by HPLC and the outlet of HPLC photo diode array detector flow cell was connected to a DPPH flow.
Antioxidants were reacted with DPPH in post-column reaction coil and monitored by UV detector at 517 nm. The results
showed that eight compounds with scavenging radical activity were found in the glycyrrhiza extract, which were identified
as formononetin, choerospondin, apioliquiritin, liquiritigenin, liquiritin, echinatin, glyyunnansapogenin F, glabrone and
licochalcone C by MS/MS and UV spectrometry.

Sensor Array for Discrimination between Raw Milk and Deteriorated Milk
ZENG Xiang-sheng,DENG Dan-wen,SHI Lei,HUANG Gan-hui
2013, 34(12):  208-212.  doi:10.7506/spkx1002-6630-201312043
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The purpose of this study was to discriminate among raw milk, pasteurized milk, aged milk, rancid milk and
adulterated milk based on sensor arrays constructed with inert metal electrodes and to investigate identification ability of the
sensor array for different milk samples. The data obtained from the determination of samples by differential pulse voltammetry
(DPV) were analyzed by one-way analysis of variance (ANOVA) and principal component analysis (PCA). Six sensors were
primarily screened and assigned to different groups by response performance with respect to the ANOVA mean square values
as well as P or F values, and the discrimination efficiencies of different combinations of the sensors were tested by PCA. As
a result, optimal sensor combination was establsihed. The results showed that Euclidean distance above 2 between every two
samples and good separation of all the samples in the PCA plots. Detection by DPV with a sensor array consisting of palladium,
platinum and gold electrodes and horizonal summation of acquired data allowed effective disrimination among the six milk
samples by Euclidean distance and PCA.

Determination of 2-Naphthol in Fruits and Vegetables by High Performance Liquid Chromatography-Tandem Mass Spectrometry
XIA Shuang,XI Cun-xian,ZHANG Lei,YAN Ai-hua,TANG Bo-bin,WANG Guo-min,MU Zhao-de
2013, 34(12):  213-216.  doi:10.7506/spkx1002-6630-201312044
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An analytical method based on high performance liquid chromatography-tandem mass spectrometry was
developed for the determination of 2-naphthol in fruits and vegetables. Samples were extracted with acetonitrile, and the
extract was then cleaned up on an LC-NH2 cartridge. The analytes were determined by LC-MS/MS with electrospray
ionization source in multiple reaction monitoring (MRM). Quantification was conducted by external standard calibration.
Good linearity was observed in the range of 50.00 to 1000.00 μg/L (r2 ≥ 0.9997). The limit of detection of the established
method was 10 μg/kg. The recovery rate of 2-naphthol was 70.4%–105.5% at spiked levels of 10, 20 μg/kg and 50 μg/kg in
deferent samples, with relative standard deviation of 4.1%–10.6%.

Rapid Detection of Bt Gene in Cooked Rice and Rice Wine
SUO Na,LIU Jia,LIU Mei,WANG Xue-qiang,WANG Yu-jian,XIAO Hong-mei*,ZHOU Guang-hong
2013, 34(12):  217-222.  doi:10.7506/spkx1002-6630-201312045
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We developed a loop-mediated isothermal amplification (LAMP) method for the detection of Bt gene in cooked
rice and rice wine. Bt gene (GeneBank accession number Y09787) was amplified by a set of four special primers that
were designed according to six regions of the target gene. We optimized the reaction conditions Mg2+ concentration, Bst
DNA polymerase concentration, temperature and time. We also explored the specificity and sensitivity of the reaction. The
results showed that the LAMP reaction system allowed easy and effective detection of Bt gene with a high specificity and
sensitivity. The limit of detection was 0.005%. The LAMP detection method is specific, sensitive and reliable without need
for special instruments.

Analysis of Organic Acid Contents in Wine Grape from Different Cultivars
CHENG Bing,ZHANG Jing-fang*,XU Hong-yu,HOU Li-xuan,WANG Yue-hui,ZHANG Yan,WANG Cheng
2013, 34(12):  223-228.  doi:10.7506/spkx1002-6630-201312046
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Six organic acids including tartaric, malic, citric, oxalic, succinic and lactic acids in wine grape from 55
cultivars (including 28 white grape cultivars and 27 red ones) were determined by reversed-phase high performance liquid
chromatography (RP-HPLC). The results showed that tartaric, malic and citric acids were major organic acids in wine grapes.
The contents of oxalic, succinic and lactic acids were too low to be detected. The total content of six organic acids in white wine
grapes were significantly higher than in red ones. The content of malic acid in red grape cultivars was higher than in white ones,
while the five other organic acids were lower in red grape cultivars. Among the 28 white grape cultivars, the highest contents of
total acids (21.580 g/L), tartaric acid (11.790 g/L) and malic acid (9.630 g/L) were detected in Pinot Blanc and higher critic acid
(5.400 g/L) was detected in White Riesling, while the lowest contents of total organic acid (7.250 g/L) and malic acid (0 g/L)
were detected in Влощ Vioshi. Among the 27 red wine grape cultivars, Bacco nion had both the highest contents of total organic
acid and malic acid (22.27 g/L and 18.210 g/L, respectively) and the lowest tartaric acid content (2.060 g/L); Heihou exhibited
the highest content of citric acid (2.510 g/L), whereas Muscat Hamburg showed the lowest content of total organic (4.94 g/L).

Determination of Biogenic Amines in Rice Wine by High Performance Liquid Chromatography
CHEN Zhi-yi,CHEN Cong-han,XIAO Yong-jian,HUANG Jin,YANG Chun-ying,LIU Xue-ming
2013, 34(12):  229-233.  doi:10.7506/spkx1002-6630-201312047
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A high performance liquid chromatography (HPLC) method was established to simultaneously detect biogenic amines in four types of rice wine, strong aroma, soaked, Douchi-like aroma and mixed aroma. The results showed that β-phenylethylamine and putrescine were detected in all the rice wines. Spermidine and tyramine were detected only in some of them at a level lower than 0.5 mg/L, both within the safe range.

Determination of Impurity Elements in Food Preservative Calcium Propionate by Inductively Coupled Plasma Optical Emission Spectrometry
FU Liang
2013, 34(12):  234-236.  doi:10.7506/spkx1002-6630-201312048
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The contents of impurity elements including Mg, Al, Ti, Cr, Mn, Fe, Ni, Cu, Zn, As, Cd and Pb from the food
preservative calcium propionate were determined by inductively coupled plasma optical emission spectrometry (ICP-OES).
Samples were dissolved and diluted with 5% (V/V) HNO3 before ICP-OES analysis. Detection wavelength, matrix effects and
plasma parameters were explored and the optimal working conditions for ICP-OES were established. The recovery rates for
spiked samples were between 91.2% and 110.6%, with relative standard deviation less than 3.9%. This method was simple,
sensitive and precise and was successfully applied to simultaneous determination of impurity elements in calcium propionate.

Determination of 72 Pesticide Residues in Tomato Paste by TSQ QUANTUMN-GC
SHANG De-jun,WEI Shuai,LI Shi-yu
2013, 34(12):  237-242.  doi:10.7506/spkx1002-6630-201312049
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A novel method was developed for the determination of 72 pesticide residues in tomato paste by TSQ
QUANTUMN GC (GC-MS/MS) combined with QueChers extraction. Optimal concentrations of standard working
solutions, SEM (selected ion monitoring) ion pairs, acquisition time window and collision energy were established for MS/
MS analysis of methamidophos and 71 other pesticides in full scan, daughter ion scan and selected ion scan modes. Over the
linear range of 5 to 2000 μg/L, the correlation coefficient for each pesticide was bigger than 0.99. Recoveries from spiked
samples at three levels indicated that 95.8% of the tested pesticides exhibited a recovery range of 80% to 120% with relative
standard deviation smaller than 15% for 87.5% of them. The limits of detection (RSN = 3) varied over the range of 0.04 to 7.5
μg/kg, and limits of quantification (RSN = 10) ranged from 0.1 to 12.9 μg/kg. This method could provide a sensitive, accurate
and reilable approach that meets the requirments for quantitative analysis of low levels of pesticides.

Real-Time PCR Assay for Detection of Banana Ingredients in Foods
LI Fu-wei,ZHANG Shu-ya,YE Jun,YU Cui,BAO Jian-qiang,YIN Li-ping
2013, 34(12):  243-246.  doi:10.7506/spkx1002-6630-201312050
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Specific primers and probe were designed according to the highly conserved sequence of ribulose-1,5-
bisphosphate carboxylase (rbcL) gene in banana. A real-time fluorescence polymerase chain reaction (real-time PCR) assay
for banana ingredients in foods was developed. The probe and primers were highly specific to banana, and resulted in no
positive reaction signal when applied to 55 other kinds of food materials. The detection limit of the method was 0.0001 ng/μL
for banana DNA and 0.001% (m/m) for banana powder. All these results confirm that the real-time PCR assay is a rapid,
sensitive and specific method for detecting banana ingredients in foods.

Chemical Characterization of Different Vinegars by NMR-Based Metabolomic Approach
LI Ai-ping,LI Zhen-yu,XING Jie,ZHANG Li-zeng,QIN Xue-mei
2013, 34(12):  247-253. 
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In this study, chemical constituents of different vinegars were analyzed and compared using a NMR based
chemical profiling approach, and the differential components in different vinegars were identified by multivariate statistical
analysis. For NMR analysis, 0.1 mL of D2O solution containing TSP (0.05 g/100 mL) were added to 0.6 mL of degassed
vinegar samples. The 1H-NMR spectral data were reduced to integral regions of equal width of δ 0.04 using MestRec
software, and then imported into the SIMCA-P (Version 11.0, Umetrics, Umea, Sweden) for PCA analysis, which showed
a clear separation in 26 vinegar samples. PLS-DA was used to find the characteristic components in each group, among
which the results for amino acids were consistent with those obtained with Hitachi 835-50 amino acid automatic analyzer.
In conclusion, the present study provided a new method for comprehensive analysis of complex liquid food samples, which
can not only clarify the chemical compositions in different samples, but also identify characteristic components quickly. This
method is simple and can be used for rapid analysis of vinegars.

Major Components and Flavor Substances in the Marinade of Water-Boiled Salted Chicken
HUANG Kai-xin,CHEN Qing,SONG Xian-liang,YE Sheng-ying,WU Shao-lie
2013, 34(12):  254-256.  doi:10.7506/spkx1002-6630-201312052
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The contents of protein, salt-free solids, free amino acids and flavor elements in the marinade of water-boiled
salted chicken were analyzed. The results showed that there were abundant protein and salt-free solids in fresh and used
samples of the marinade. The total content of free amino acids exhibited only slight differences in the fresh and used
marinades, but the contents of different amino acids varied greatly, and the proportion of essential amino acids in the fresh
marinade increased remarkably after use. Both marinade samples contained hydrocarbons, organic acids and esters and other
flavor substances, of which the main components were esters.

Development of a High-Performance Liquid Chromatographic Method for Detection of Chlorfluazuron Residues in Fruits Cultivated in Southeast Asian
Lü Ping,DU Guo-dong,WEI Li-jun,NONG Yao-jing
2013, 34(12):  257-260.  doi:10.7506/spkx1002-6630-201312053
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A analytical method was established to determine chlorfluazuron residues in banana, mango and litchi
cultivated in Southeast Asia by high performance liquid chromatography (HPLC). Samples were extracted acetone
and the extact was then cleaned up on a Florisil column prior to analysis by HPLC with UV detection. The analytical
column was an Agilent Eclip se XDB C18 column (4.6 mm × 250 mm, 5 μm) and the mobile phase was methyl alcoholwater
(90:10, by volume) at a flow rate of 1.0 mL/min. The detection wavelength was set at 258 nm. Quantification was
performed by the external standard method. The results showed that the linear range for chlorfluazuron was in the range
of 0.05-5.00 mg/L with a correlation coefficient of 0.99996. The average recoveries of chlorfluazuron were between 84.7%
and 102%, with a variation coefficient ranging from 2.0% to 6.7%. The limit of quantification of this method was 0.02 mg/kg.
This method met the national requirements for pesticide determination and was applicable to food quality supervision and
control on chlorfluazuron.

Determination of Selenium in Nanyang Colored Wheat by Intermittent Flow-Double Channel-Atomic Fluorescence Spectrometry after Microwave Digestion
GAO Xiang-yang,GAO Xin-zhen,ZHU Ying-rui,ZHANG Pin
2013, 34(12):  261-264.  doi:10.7506/spkx1002-6630-201312054
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An analytical method for the determination of selenium in Nanyang colored wheat was presented by intermittent
flow-hydride generation (by using acidic KBH4 system)-atomic fluorescence spectrometry (HGAFS) after microwave
digesiton with nitric acid-perchloric acid. Under optimized conditions, the calibration curve of selenium standard solution
showed a good linear relationship over the range of 0-24 μg/L (r = 0.9996). The average recovery for spiked sampled was
99.42%, and a relative standard deviation (RSD) of 2.6% was obtained from 11 parallel determinations. Five wheat cultivars
were ranked in decreasing order of selenium content (on a dry matter basis): Nanyang grey, Yanmai 4110, Nanyang blue,
large purple and small purple. The method was characterized by simple operation, low volatile loss of selenium during
sample digestion, low matrix interference and high applicability.

Rapid Determination of Pesticide Residues in Tea by QuEChERS and Gas Chromatography-Mass Spectrometry (GC-MS)
YE Jiang-lei,JIN Gui-e,WU Yun-hui,ZHENG Wen-hui
2013, 34(12):  265-271.  doi:10.7506/spkx1002-6630-201312055
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A method to determine 47 pesticide residues in tea using QuEChERS and GC-MS was established. For the
extraction of pesticide residues, dry samples were vortex-mixed with 40 mg of NaCl dissolved in 2 mL of MeCN and
centrifuged (5000 r/min for 5 min). Then 1 mL aliquot of the supernatant was taken and vortex-mixed for 2 min after the
addition of 25 mg of PSA, 7.5 mg of GCB, 150 mg of MgSO4 and 40 mg of NaCl and entrifuged (5000 r/min for 5 min).
The resulting supernatant was injected in to a GC-MS for analysis of pesticide residues. Under the optimized conditions of
particle size and amount of samples, extraction solvent type and volume and mixing method and purificant, the recovery of
the method for spiked samples ranged from 81% to 102.2%, and precision from 6.5% to 18.3% (RSD). The linear range was
0.00195-1.0 mg/kg (R2 > 0.97), limit of detection (LOD) 0.0009-0.0214 mg/kg, and limit of quantitation (LOQ) 0.0029-
0.0712 mg/kg. This method could substantially meet the “Uniform Limits” of Japan and the EU for analysis of pesticide
residues.

Frabrication of Benzoyl Peroxide Biosensor Based on Carbon Nanotube-Modified Electrode
DING Jian-ying,PAN Huan-huan,ZHANG Gen-hua,QUAN Ying,ZHAN Yue-hua
2013, 34(12):  272-275.  doi:10.7506/spkx1002-6630-201312056
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An electrochemical enzyme biosensor was developed to determine benzoyl peroxide (BPO) in flour. Carbon
nanotube was modified on the surface of glassy carbon electrode as an electron mediator, followed by coating the electrode
surface with horseradish peroxidase embedded in chitosan sol-gel. A new type of benzoyl peroxide biosensor was fabricated
based on changes in the electrode current response caused by the catalytic action of horseradish peroxidase on BPO. The results
showed that the response current of the sensor was linearly related to BPO concentration over the range of 8.3 × 10-6 mol/L
to 3.4 × 10-3 mol/L with a detection limit of 2.3 × 10-6 mol/L. This biosensor is sensitive, fast and convenient and has the
potential to be applied for the determination of benzoyl peroxide in flour.

Determination of Flavonoids in Fuzhuan Tea by HPLC
LI Shi,LU Qiang,LI Yin-hua,HUANG Jian-an,LIU Zhong-hua
2013, 34(12):  276-280.  doi:10.7506/spkx1002-6630-201312057
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An HPLC method for the determination of flavonoids in Fuzhuan tea was presented. Chromatographic separation
was performed on Welchrom C18 (250 mm × 4.6 mm, 5 μm) column by graditent elution with methanol as mobile phase A and
0.5% acetic acid as mobile phase B at a flow rate of 0.8 mL/min. Detection wavelength was 295 nm. It took 80 min to complete
the analytical process. The established method was precise, stable and repeatable, with an average recovery of 94.88%. Thanks
to its ease of use, specificity and accuracy, this method can be used for the determination of flavonoids of Fuzhuan tea.

Headspace Solid Phase Microextraction of Volatile Flavor Components from Rapeseed Oil
XIE Jing,XU Li*,ZHANG Qiu-hong,WU Hong-yun
2013, 34(12):  281-285.  doi:10.7506/spkx1002-6630-201312058
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In comparison with steam distillation extraction (SDE) and supercritical fluid extraction (SFE), headspace solid
phase microextraction (HS-SPME) was identified as a better method for sample pretreatment in the analysis of volatile
compounds of rapeseed oil by GC-MS due to its rapid, simple, solvent-free and nondestructive procedure. The optimal HSSPME
conditions were established by the use of a DVB/CAR/PDMS fiber and magnetic stirring, extraction temperature 70 ℃
extraction for 30 min and desorption for 3 min. A total of 47 major volatile compounds were found in rapeseed oil, including
16 degraded glucosinolate products, 10 oxidative volatiles (alkenes, aldehydes and alcohols), 20 heterocyelic compounds and
1 benzene compound. Predominant degraded glueosinolated products were methallyl cyanide, 4-(methylthio)-butanenitrile,
3-phenyl propionitrile and 4-isothiocyanato-1-butene. 1,5-Hexadien-3-ol and furfural were dominant among the identified
volatile oxidation components while pyrazines were main heterocyclic compounds in rapeseed oil.

Simultaneous Determination by HPLC-ELSD of Ten Kinds of Sugars and Sugar Alcohols in Foods
LIN Hui,YAN Chun-rong,XU Chun-xiang,CAI Jing,WANG Duo-jiao
2013, 34(12):  286-291.  doi:10.7506/spkx1002-6630-201312059
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A high performance liquid chromatography with evaporative light-scattering detection (HPLC-ELSD) method
was developed for the simultaneous determination of 5 sugars including fructose, glucose, sucrose, maltose, lactose and
5 sugar alcohols inlcuding erythritol, xylitol, sorbitol, mannitol, and maltitol in foods. Extracts of samples were separated
on a Carbohydrate ES HPLC column at 30 ℃ using acetonitrile-water as mobile phase at a flow rate of 1.0 mL/min. The
detector drift tube was kept at 95 ℃ and the nitrogen rate was set at 2.5 L/min. The results showed that the linear range of all
these analytes was 0.2–20 mg/mL. The precision of the HPLC-ELSD method was < 5% in 6 replicate determinations, and
average spike recoveries were 91.53%–105.2%. Successful separation and sensitive and reproducible detection of the sugars
and sugar alcohols were achieved by this method within 30 min, thereby providing a promising approach for simultaneous
determination of sugar and sugar alcohols in food.

Lycium barbarum;polysaccharides;authenticity;composition;content;determination method
LIU Yuan-cai,SUN Xi-zhen*,XU Yin,LI Xian-zhi,YAN Ling
2013, 34(12):  292-295.  doi:10.7506/spkx1002-6630-201312060
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An improved phenol-sulfuric acid method for the determination of Lycium barbarum polysaccharides was
proposed by using mixed monosaccharide standards instead of glucose alone for prepration of a standard curve. The
monosacccharide composition of samples was determined by HPLC after hydrolysis and subsequent derivatization
for disrimination between real and fake Lycium barbarum polysaccharides. The polysaccharide content of LBP-1, a
polysaccharide extract of Lycium barbarum prepared in our laboratory, was determined by the improved method to be 30%
compared to only 14% with the traditional method.

Rapid Detection of Cronobacter sakazakii Using a Loop-Mediated Isothermal Amplification (LAMP) Assay
REN Li-song,CHEN Meng-xin,CHEN Zhuo,MA Long
2013, 34(12):  296-299.  doi:10.7506/spkx1002-6630-201312061
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This study aimed to establish a loop-mediated isothermal amplification (LAMP) method for rapid detection of
Cronobacter sakazakii. The gene sequences of ompA were aligned using the biologic software and four specific primers used for
LAMP were designed and the reaction condition was optimized. DNA templates from different cell concentrations were extracted by
boiling, FTA card and kit methods and detected by the LAMP method to obtain detection limits of 104, 103 CFU/mL and 103 CFU/mL,
respectively. Seven of 12 Cronobacter sakazakii isolates investigated were positive while all the others were negative. This method
may provide a more simple and rapid approach to detecting Cronobacter sakazakii in comparison with PCR method.

Determination of Cadmium, Mercury, Lead and Chromium in Alcoholic Drinks by Inductively Coupled Plasma-Mass Spectrometry with Dynamic Reaction Cell
YAN Na,ZHAO Sheng-guo,GAO Yun-yun
2013, 34(12):  300-303.  doi:10.7506/spkx1002-6630-201312062
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Digestion with dillute nitric acid followed by inductively coupled plasma-mass spectrometry (ICP-MS) with
dynamic reaction cell (DRC) was used to determine the levels of cadmium, mercury, lead and chromium in alcoholic
drinks. The optimal levels of nitric acid concentration (volume fraction), temperature, time and sample dilution factor for
the digestion process were found to be 50%, 95 ℃, 1 h and 5, respectively. Further investigations were also carried out
into reduction of matrix interferences, eliminiation of mercury adsorption and optimization of instrumental conditions. The
contents of cadmium, mercury, lead, chromium in red wine, white wine, liquor, beer and rice wine was determined by the
presented method. The limits of detection for cadmium, mercury, lead, chromium were found to be 0.01, 0.01, 0.08 μg/L,
and 0.03 μg/L, respectively. The precision of this method was in the range of 0.48% to 12.87% (RSD), and recovery rates
ranged from 89.6% to 106.5%. This method was efficient, sensitive, accurate and suitable for large-scale determination.

Effect of Storage Conditions on Aromatic Components of Litchi Wine
DENG Kai-ye,HUANG Xiao-hong,BAI Wei-dong
2013, 34(12):  304-307.  doi:10.7506/spkx1002-6630-201312063
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Headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS)
were used to investigate how aromatic components of litchi wine could be affected by different storage conditions: ambient
temperature bottle, low temperature bottle (6-8 ℃) and stainless steel tank. The results showed that the main components
of litchi wine were octanoic acid ethyl ester, hexanoic acid ethyl ester, decanoic acid ethyl ester, 3-methyl-1-butanol acetate,
ethyl acetate, 3-methyl-1-butanol and ethyl butyrate. As compared to ambient temperature bottle storage and stainless steel tank
storage, low temperature bottle storage was more favorable for the formation retention of aromatic components in litchi wine.

Effects of Different Temperature Modes on Storage of Wujiuxiang Pear
LI Li-mei,WANG Jing-tao,HE Jin-gang,CHENG Yu-dou,GUAN Jun-feng
2013, 34(12):  308-311.  doi:10.7506/spkx1002-6630-201312064
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The effects of different temperature modes, including non-gradual cooling, gradual cooling, non-gradual
cooling combined with stepwise heating and gradual cooling combined with stepwise heating, on storage qualities
of Wujiuxiang pear, such as firmness, soluble solid content(SSC), titritable acidity, relative membrane permeability
and peel browning, were studied. All pears in this study were packaged in polyethylene film 0.010 mm thick. The
gradual cooling mode started from 10 ℃, reducing by 1 ℃ a day to 7 ℃, then by 2 ℃ a day to 3 ℃ and finally to
0 ℃ in one day. The non-gradual cooling mode was storage at 0 ℃ without gradual cooling. The sepwise heating
mode was exposure to 10 ℃ for 24 h followed by 25 ℃ for 24 h. Results showed that gradual cooling storage did not
significantly influence firmness, SSC or relative membrane permeability and favored the maintenance of titratable
acid content and inhibition of peel browning. Stepwise heating caused normal post-harvest ripening and softening of
pears which were manifested by a decrease in hardness and no significant variations in SSC, titratable acid content
or relative membrane permeability. During the first 150 d of storage peel browning became more serious and then no
significnat changes were observed. As a result, gradual cooling combined with stepwise heating may help preserve
Wujiuxiang pear by alleviating the reduction of hardness and peel browning.

Effect of β-aminobutyric Acid Combined with Chitosan Treatment on Postharvest Blue Mold and Storage Quality of Red Fuji Apple
ZHANG Wei,ZHOU Hui-ling*,WEN Xiao-hong,YUAN Zhong-yu
2013, 34(12):  312-316.  doi:10.7506/spkx1002-6630-201312065
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The effect of different concentrations of β-aminobutyric acid on the prevention and control of postharvest blue mold of
Red Fuji apple was studied as well as the impact of β-aminobutyric acid combined with chitosan coating treatment on the storage
quality of apple. Results revealed that 0.75 g/L β-aminobutyric acid was the most effective treatment for the control of postharvest
blue mold while having almost no influence on respiration intensity, ethylene release rate soluble solids or titratable acid content
during storage of Red Fuji apple. However, β-aminobutyric acid treatment effectively delayed the reduction of firmness and
the increase of weight loss rate. β-aminobutyric acid treatment when combined with 1.5% of chitosan coating showed a better
preservative effect , and significantly inhibited changes in several physiological indexes during storage of Red Fuji apple.

Effect of Different Packaging Conditions on Stability of Antioxidative Functional Components and Quality of Yunnan Santai Walnut
LI Da-peng,YANG Chun-yan,WANG Wen-qian,LU Zheng,YE Lei,RONG Rui-fen*
2013, 34(12):  317-321.  doi:10.7506/spkx1002-6630-201312066
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The stability of antioxidative functional components of walnut under different packaging conditions was studied.
The contents of antioxidative functional components such as total phenols (TP), total flavonoids (TF) and γ-vitamin E (γ-VE) as
well as oxidation indexes and sensory quality were determined periodically in Yunnan Santai walnut packaged in polyethylene
pouches, vacuum packaging or silicon window bags during storage at room temperature. The results showed that oxidative
stability and sensory quality of vacuum packaged walnut were similar to that of walnut packaged in silicon window bags but
better than that of walnut packaged in polyethylene pouches after 6-month storage. The contents of TP, TF and γ-VE in walnut
packaged in polyethylene pouches were reduced by 34.5%, 22.4% and 40.1%, respectively, as opposed to 10.4%, 15.0% and
17.3% for walnut packaged in silicon window bags and 20.7%, 17.3% and 17.1% for vacuum packaged walnut, respectively.
Compared to polyethylene pouch packaging, the nutritional quality of walnut was better maintained by vacuum packaging and
silicon window bags, prolonging the shelf life by 2 to 3 months.

Effect of 1-MCP on Cold Storage Quality and Redox State of Postharvest Peach Fruits
QIAN Chun-lu,MI Hong-bo,HE Zhi-ping,ZHAO Yu-ying,MAO Lin-chun
2013, 34(12):  322-326.  doi:10.7506/spkx1002-6630-201312067
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In order to explore the effect of 1-methylcyclopropene (1-MCP) treatment on the quality and redox state of peach
fruits, ‘Yanhong’ peach fruits were treated with 0, 0.25, 0.5 μL/L and 1 μL/L 1-MCP, and stored at (4 ± 1) ℃ for 21 days
and then transferred to (20 ± 1) ℃ for 3 days. The results indicated that 1-MCP treatment reduced respiration rate, ethylene
production, weight loss rate and electrolyte leakage, and remarkably kept fruit firmness and color. The 1-MCP treatment
at a dose of 1 μL/L had the most significant effect (P < 0.05). Meanwhile, 1-MCP treatment could maintain fruit peel and
flesh ascorbate (ASC) content and ASC/dehydroascorbate ratio, inhibit the increase of fruit peel glutathione (GSH)
content and GSH/ oxidized glutathione ratio, thus causing the decrease of these in fruit flesh. In conclusion, the 1-MCP
treatment at 1 μL/L showed the most significant benefit to peach cold storage, which may be related to antioxidant capacity.

Influence of Modified Atmosphere Packaging on Physiological Characteristics of Tricholoma matsutake
XUE Wei,WANG Yue
2013, 34(12):  327-330.  doi:10.7506/spkx1002-6630-201312068
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Under the storage conditions of 2-3 ℃ and 85%-90% relative humidity, the effects of gas composition,
differnet packaging materials and film thickness on the preservation of Tricholoma matsutake were explored through
determining respiratory intensity, weight loss rate, browning index, cell membrane permeability and other physiochemical
indexes. The results showed that a V(O2): V(CO2): V(N2) ratio of 3:20:77 and packaging in a PVC film 0.05 mm thick
provided optimum preservation of Tricholoma matsutake, prolonging the shelf life to about 7 d.

Effect of Calcium Treatment on Quality of Button Mushroom (Agaricus bisporus) during Storage
SHEN Qi,SUN Ya,ZHANG Wei-min,WANG Yu-ning,LI Zhi-qiang
2013, 34(12):  331-335.  doi:10.7506/spkx1002-6630-201312069
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Using water as a control, the effects of calcium chloride treatment at various concentrations (0.5, 1 g/100 mL and
2 g/100 mL) on respiration intensity, total sugar, protein, free amino acid, vitamin C and pectin (protopectin and soluble
pectin) contents in Agaricus bisporus were studied. The results indicated that during storage at 0-2 ℃, 0.5 g/100 mL
calcium chloride treatment could effectively inhibit respiratory intensity, delay the appearance of climacteric, slow down
the reduction of total sugar, protein, vitamin C and protopectin contents, and suppress the rising speed of free amino acids
and soluble pectin contents; 1 g/100 mL calcium chloride treatment could delay the appearance of climacteric, inhibit the
decrease of protein level during the latter storage period (12-14 d), and the content of vitamin C was higher than that of the
control during 0-4 d. With 2 g/100 mL calcium chloride treatment, total sugar was higher during storage period of 0-8 d,
and the content of protein was higher than that of the control during storage period of 12-14 d.

Effect of Storage Temperature on Quality and Senescence of Pitaya
LIU Shun-zhi,SUN Ru,JIANG Yue-ling,HU Wei-rong*
2013, 34(12):  336-340.  doi:10.7506/spkx1002-6630-201312070
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Dynamic changes in fruit qualities and related enzyme activities of pitaya (Hylocereus undatus) stored at 15 or
5 ℃ for 50 d were studied. The results showed that the contents of total soluble sugar, titratable acid, vitamin C, protein in
pulp and red pigment in peel stored at 15 ℃ decreased during the whole storage period. During 5 ℃ storage, however, these
parameters showed significantly reduced losses. Amylase activity in pulp stored at 15 ℃ was higher than in pulp stored at
5 ℃. The activities of polyphenol oxidase (PPO) and phenylalanine ammonia lyase (PAL) in peel increased with storage
time at both temperatures and resulted in browning at the end of storage. The peaks of activity of peroxidase (POD) and
superoxide dismutase (SOD) were delayed and catalase (CAT) activity in peel was kept at a higher level when stored at 5 ℃,
which suppressed the increase in malondialdehyde (MDA) content compared with fruits stored at 15 ℃. Therefore, lower
temperature storage at 5 ℃ retarded fruit senescence and prolonged the storage life of pitaya by 20 days.

Softening and Softening Indices Change of Blueberry during Storage
JI Shu-juan,MA Chao,ZHOU Qian,CHENG Shun-chang,WEI Bao-dong
2013, 34(12):  341-345.  doi:10.7506/spkx1002-6630-201312071
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Blueberry fruit softening and softening indices change during storage were analyzed. Results showed that decay
index, titratable acid content, POD activity, Cx activity and β-Gal activity were closely related with firmness during storage
at room temperature. Among them, decay index and Cx activity showed highly significant negative correlation with firmness,
whereas there was a significant positive correlation between the content of titratable acid and firmness. Firmness and titratable
acid content decreased slowly, whereas decay index rose during cold storage at 0 ℃. POD activity, Cx activity and β-Gal
activity showed an obvious increasing trend along with decreasing firmness. POD activity and Cx activity rose rapidly in the
last stage of storage. Their activity peaks occurred on the 60th day of refrigeration at 0 ℃, while β-Gal activity climax occurred
in the early stage of storage and then its activity kept at a high level. Compared with fresh blueberry, blueberry refrigerated for
30 days showed smaller decreases in firmness and titratable acid content, less changes in decay index, POD activity and Cx
activity and no significant β-Gal activity climax after 4 days of storage at room temperature. From the above results, it can be
seen that blueberry refrigerated for 30 days can keep its quality for 4 days at room temperature.

Preparation of Angelica keiskei Koidzmi Flavonoid Effervescent Tablets
GUO Xiao-qing,WU Jin-hong,LIU Chang,ZHOU Yan-fu,WU Yu-di,WANG Zheng-wu,YAN Xia
2013, 34(12):  346-350.  doi:10.7506/spkx1002-6630-201312072
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The preparation of an oral effervescent tablet of Angelica keiskei Koidzmi flavonoids from flavonoid-rich
ethanol extract of this plant (mainly leaves) by a non-aqueous granulation method was optimized in the present study.
The optimum formualtion for the effervescent tablet was 18% of A. keiskei flavonoid inclusion, 9.75% of lactose, 34.00%
of citric acid, 31.00% of sodium bicarbonate, 4.90% of xylitol, 0.10% of sucralose, 0.25% of octenyl succinic anhydride
modified starch, 2.00% of PEG8000 and 0.06 mL/g PVP as determined by one-factor-at-a-time design. The resulting
product had a pleasant taste, high nutritional value and the unique refreshing fragrance and sweet flavor of Angelica
keiskei and was acceptable to consumers.

Development and Application of Colloidal Gold Rapid Test Strip for Chloramphenicol in Aquatic Products
SANG Li-ya,WU Mao-sheng,HUANG Yi-wen,SHENG Hui-ping,LIU Ai-chun
2013, 34(12):  351-355.  doi:10.7506/spkx1002-6630-201312073
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A colloidal gold test strip for rapid detection of chloramphenicol in aquatic products has been developed and
applied. Colloidal gold particles were prepared and labeled to an anti-chloramphenicol (CAP) monoclonal (MAb) antibody.
Optimum concentrations of goat anti-mouse IgG, chloramphenicol-bovine serum albumin (CAP-BSA) and the gold labeled
antibody were established by repeated testing before coating a nitrocellulose (NC) membrane and a colloidal gold conjugate
pad. After being dried at 37 ℃ for 32 h or 25 ℃ for 7 d, the NC membrane, together with a sample pad, a colloidal gold
conjugate pad, a absorbent pad and other accessories, was used to fabricate a colloidal gold test strip. The detection limit of
the test strip for chloramphenicol was 0.3 μg/kg, and false positive rate (FPR) and false negative rate (FNR) were 4% and 2%
respectively. Its period of validity was more than 6 months at room temperature.