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Table of Content

25 June 2015, Volume 36 Issue 12
Processing Technology
Maillard Reaction between Chitosan and Xylose in Dry State
LI Yanlong, HUANG Guoqing, XIAO Junxia*
2015, 36(12):  1-6.  doi:10.7506/spkx1002-6630-201512001
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This experiment explored the possibility of the Maillard reaction between chitosan and xylose in the dry heat state
and investigated the effects of reaction temperature, relative humidity, reaction duration, and mixing ratio on the reaction.
Meanwhile, the thermal behavior and rheological properties of the resultant Maillard reaction products were characterized
as well. The results indicated that the Maillard reaction between chitosan and xylose occurred readily in the dry state
and the optimum conditions were determined as follows: chitosan-xylose mixing ratio, 1:1; reaction temperature,
90 ℃; relative humidity, 61.2%; and reaction duration, 4 h. The resultant Maillard reaction products displayed
a reduced thermal degradation temperature compared with chitosan. Rheological measurements revealed greatly
enhanced elastic property in solution.

Optimizing the Saponification of Lutein Esters from Marigold Flowers
MA Kongjun1, PAN Yanliang2, ZHANG Weihong1, XU Sumei1, GAO Chao1
2015, 36(12):  7-11.  doi:10.7506/spkx1002-6630-201512002
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This work was conducted to investigate the saponification of lutein esters from marigold flowers. The effects
of type and amount of organic solvent, saponification temperature and time on the saponification rate of lutein esters as
determined by thin layer chromatography were explored. The optimal conditions for the saponification of lutein esters were
determined by single factor experiment and response surface analysis as follows: 2.0 g of lutein esters, 31.3 mL of absolute
ethanol, 2.1 g of potassium hydroxide, a saponification temperature of 60 ℃, and a saponification duration of 4 hours. Under
these optimal conditions, the average saponification rate of lutein esters reached 78.4%.

Optimizing Microwave-Assisted Vacuum Freeze-Drying of Dioscorea opposite by Orthogonal Array Design
REN Guangyue, REN Liying, ZHANG Wei, DUAN Xu, LUO Lei, ZHU Wenxue
2015, 36(12):  12-16.  doi:10.7506/spkx1002-6630-201512003
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The microwave-assisted vacuum freeze-drying of Dioscorea opposite was executed to obtain high-quality dried
products. Drying characteristics and quality traits of dried Dioscorea opposita were investigated. The effects of three drying
conditions including sample slice thickness, vacuum degree in drying chamber and microwave power on the rehydration
ration, polysaccharide yield and L value (brightness) of dried products were examined. Linear weighting method was used
to analyze comprehensive multi-objective optimization to determine the optimal values of the studied parameters. The
results showed that the influences of these three factors on the overall index score were in the decreasing order of slice
thickness > vacuum degree > microwave power. The optimal drying conditions were slice thickness of 5 mm, degree of
vacuum of 100 Pa, and microwave power of 3.75 W. The drying time to achieve safe moisture content of 0.12 g/g (dry
basis) was 150 min and drying energy consumption was 7 875.9 kJ/kg. Under these conditions, the quality of the dried
product was excellent with good rehydration ratio (95.6%), pure color (the value of color difference was 92.90) and
high polysaccharide yield (18.97%).

Optimized Synthesis and Stability of Feruloylated Acylglycerols
WANG Qiang1,2, LONG Jie1, REN Yanrong1, WANG Cun1, PENG Rong3, YUAN Jun4
2015, 36(12):  17-21.  doi:10.7506/spkx1002-6630-201512004
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This study was intended to model and optimize the reaction conditions for enzymatic esterification of ferulic acid
with maize germ oil using a commercial lipase, Lipozyme RM IM, in a solvent system to obtain feruloylated acylglycerols
by response surface methodology (RSM). The experiments were designed with central composite design. The reaction
factors investigated were molar ratio of maize germ oil to ferulic acid, temperature and time. The yield of feruloylated
acylglycerols was selected as the response variable. All the factors investigated significantly affected the yield of feruloylated
acylglycerols. The optimal reaction conditions were found to be a molar ratio of maize germ oil to ferulic acid of 8.9:1 (g/g),
76.0 ℃ and 28.1 h, leading to a feruloylated acylglycerol yield of 59.1%, which was in good agreement with the predicted
value of 58.8%. The prepared acylglycerols produced low polymer during frying process, and they had high storage stability.

Optimization of Purification Process for Crude Polysaccharides from the Pomace of Wild Crataegus songorica in Xinjiang by Response Surface Methodology
ZHANG Yu, LI Jin*, Lü Haiying, ZHANG Xia, ZHANG Huali
2015, 36(12):  22-28.  doi:10.7506/spkx1002-6630-201512005
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In order to improve the purity of polysaccharides from the pomace of wild Crataegus songorica, NKA-9 and D101
were selected from 7 kinds of macroporous resins by static adsorption-desorption experiments, and the two selected resins
were mixed at an appropriate ratio. On the basis of single factor experiments, response surface methodology was used to
optimize process parameters. The optimal mixing ratio of NKA-9 to D101-1 was 2:3 (by mass). The optimum experimental
parameters for adsorption were as follows: sample loading flow rate, 3.75 mL/min; sample concentration, 1.32 g/L; and resin
diameter-to-height ratio, 1:13, yielding a rate of adsorption of 60.75%. Under the optimal desorption conditions: 7 BV of
0.27 mol/L NaCl as eluent at a f??l ow rate of 3.5 mL/min, a rate of desorption of 84.22% could be achieved. The content of
polysaccharides was increased from 5.06% to 21.13%.

Optimization of Ultrasound-Assisted Extraction of Ellagic Acid and Total Phenols from Muscadine (Vitis rotundifolia) by Response Surface Methodology
WEI Zheng1, ZHAO Yajiao1, HUANG Yu2, ZHANG Yali1, LU Jiang1,*
2015, 36(12):  29-35.  doi:10.7506/spkx1002-6630-201512006
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The extraction conditions of ellagic acid and total phenols from the skin and seeds of the Noble muscadine
using acetone/water/hydrochloric acid (70:29:1, V/V) by ultrasonic-assisted extraction (UAE) were optimized employing a
combination of single-factor experiments and response surface methodology through mathematical modeling. The analysis
of two-factor interactions was carried out. The results indicated the ratio of solid to liquid, extraction time and ultrasonic
power to be the most significant factors affecting the extraction efficiencies of ellagic acid and total phenols. The optimum
extraction conditions for ellagic acid and total phenols from muscadine skin were determined as follows: ratio of solid to
liquid, 1:30; extraction time, 28 min; and ultrasonic power, 616 W. The predicted contents of ellagic acid and total phenols
under these conditions were 616.21 μg/g and 15.06 mg/g (using gallic acid equivalent, fresh weight), respectively, agreeing
with the experimental values. In conclusion, UAE can be applied to the extraction of ellagic acid.

Optimization of Compound Food Additives for Frozen Dough Steamed Breads Made with Mixed Starters by Response Surface Methodology
DU Haoran, ZHENG Xueling, HAN Xiaoxian, ZHANG Jie, LI Limin, LIU Chong*, BIAN Ke*
2015, 36(12):  36-43.  doi:10.7506/spkx1002-6630-201512007
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This study examined the individual effects of four food additives on the quality of frozen dough steamed bread
made with a mixed culture consisting of yeast and rice wine containing the starter strains at a mass ratio of 4:5. The
proportions of the four additives when used in combination were optimized by response surface methodology. Experiments
were designed using combination of single factor method and Box-Behnken design. As a result, a mathematical model was
established describing the effect of the four food additives on the overall quality score of steamed bread and their optimal
levels were obtained. The quality of steamed bread was affected in decreasing order by xylanase, sodium polyacrylate,
diacetyl tartaric acid ester of mono(di)glycerides (DATEM) and trehalose, and their optimum combined proportions were
0.15% DATEM, 0.05% sodium polyacrylate, 25.73 mg/kg xylanase, and 3.65% trehalose. Under these conditions, the
expected sensory score of steamed bread was 84.646, and the actual value was 84 ± 0.74. The rheological properties of
frozen dough such as elastic modulus (G’) and viscous modulus (G”) were improved when the compound food additives
were added. This study has indicated that compound food additives can inhibit the formation of ice crystallization and
prevent the dough from recrystallization, reduce the damage to the mixed starter and the structure of the gluten network from
ice crystallization, and improve the qualities of dough and steamed bread.

Optimization of Simultaneous Ultrasonic-Assisted Extraction of Total Flavonoids and Tannins from Mulberry Leaves
ZHONG Yushen1, WANG Liqiong1, HAN Xiaodan1, HUANG Xianzhi2, DING Xiaowen1,*
2015, 36(12):  44-48.  doi:10.7506/spkx1002-6630-201512008
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Ultrasonic-assisted extraction was adopted to simultaneously extract total flavonoids and tannins from mulberry
leaves and these two classes of compounds were spectrophotometrically determined. Results showed that the best conditions
for simultaneous ultrasonic-assisted extraction of total flavonoids and tannins from mulberry leaves were as follows: ethanol
concentration, 75%; material to liquid ratio, 1:30; extraction temperature, 80 ℃; extraction time, 10 min; and ultrasonic
power, 128 W. The yields of tannins and total flavonoids were 6.32 mg/g and 18.55 mg/g, respectively under these optimized
conditions. Compared with the traditional extraction methods, UAE achieved a higher extraction efficiency and a higher
accuracy in a shorter time at a lower extraction temperature, making it an appropriate method to extract total flavonoids and
tannins from mulberry leaves.

Orthogonal Array Design for the Optimization of Deacidification of Peony Seed Oil by Solvent Extraction
LU Shaolan1, WU Suxi1,2,*, SONG Yanqiu1, ZHANG Chunli1
2015, 36(12):  49-53.  doi:10.7506/spkx1002-6630-201512009
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The deacidification of crude peony seed oil by a solvent extraction method which can avoid the flavor
deterioration of peony seed oil when purified by alkali refining was optimized using single factor and orthogonal array
experiments. The optimal extraction conditions were determined to be 20 min extractions at 40 ℃ performed three times
using 95% ethanol as the extraction solvent with a solid to solvent ratio of 1:2.5 (g/mL), resulting in a removal rate of free
fatty acids of 93.12% and a deacidified oil yield of 83.23%. After the deacidification process, the acid value of peony seed
oil could be reduced from 10.18 to 0.70 mg KOH/g while maintaining the delicate scent of peony seed oil. The quality of
peony seed oil was suitable for subsequent processing.

Optimization of Formulation of Low-Sugar White Gourd Stuffing in Cantonese-Style Moon Cake Based on TPA Parameters
CHEN Xian1,2, ZHANG Yan1,*, MA Yongxuan1, ZHANG Linghong1,2, WEI Zhencheng1
2015, 36(12):  54-59.  doi:10.7506/spkx1002-6630-201512010
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This study investigated the optimization of low-sugar white gourd stuffing formulations for Cantonese-style
moon cake by correlating sensory score with texture profile analysis (TPA) parameters including hardness, cohesiveness
and resilience of moon cake. The results showed that all the three TPA parameters were significantly negatively correlated
with the sensory score of moon cake (P < 0.01) and that they could be used as indicators to evaluate the quality of low-sugar
white gourd stuffing. Maltitol, xylitol and isomaltooligosaccharide were used as sugar substitutes in the moon cake stuffing.
Two optimized formulations were obtained by simplex-centroid experiments consisting of 75.5% white gourd puree, 19.0%
maltitol, 4.5% peanut oil, and 1.0% corn starch; and 75.5% white gourd puree, 3.3% sucrose, 15.7% xylitol, 4.5% peanut oil,
and 1.0% corn starch, respectively.

Orthogonal Array Design for the Optimization of Pepsin Soluble Collagen Extraction from Cyprinus carpio haematopterus Scale
XIAO Feng1,2, ZHU Wenxue1,*, KANG Huaibin1, LIU Lili1, HE Jialiang1, REN Guoyan1
2015, 36(12):  60-64.  doi:10.7506/spkx1002-6630-201512011
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Pepsin and 0.5 mol/L acetic acid were used to enhance the extraction of collagen from Cyprinus carpio
haematopterus scale at 4 ℃. Using combination of single factor experiments and orthogonal array design, the effect of
extraction time, enzyme concentration and ratio of solid to solvent on the yield of pepsin soluble collagen (PSC) from
C. haematopterus scale were explored. The results showed that the optimal conditions for PSC extraction were determined
as follows: extraction time, 60 h; enzyme concentration, 40 kU/g; and ratio of solid to solvent, 1:10 (g/mL). The yield of
PSC under these conditions was (17.7 ± 0.7)%. The PSC had electrophoretic properties amino acid composition similar to
those of acid soluble collagen (ASC), suggesting similarity beween their molecular structures.

Visual Optimization of Extraction Process of Tea Flower Oil with Supercritical Carbon Dioxide
XU Jing1, SUN Yimin1,*, ZOU Li1, FANG Zhuizhui1, ZONG Kan1, WANG Ju2
2015, 36(12):  65-69.  doi:10.7506/spkx1002-6630-201512012
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This paper reports a systematic investigation of the supercritical carbon dioxide extraction of essential oil from
tea flower. Extraction pressure, temperature, static extraction time, dynamic extraction time and separation temperature were
chosen as main variables influencing extraction efficiency. The multifactor and multilevel visual design method (m2VD)
was applied to design the experiments and the experimental data were analyzed by the multifactor and multilevel visual
optimization method (m2VO) to optimize the extraction conditions. Over 8 g of the essential oil was obtained when three
parallel experiments were conducted under the following conditions: extraction pressure 19–22 MPa, extraction temperature
50–60 ℃,static extraction time 30–50 min, dynamic extraction time 80–100 min and separation temperature 40–50 ℃. The
present study indicates that the m2VO method holds promise for practical application.

Lycopene from Tomato Peel: Optimization of Ultrasonic-Assisted Extraction by Response Surface Methodology and Identification by High Performance Liquid Chromatography
WANG Zhenqiang1, LI Xiaokun1, WANG Hao2,*
2015, 36(12):  70-75.  doi:10.7506/spkx1002-6630-201512013
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The extraction of lycopene from tomato peal by ultrasonic-assisted extraction (UAE) was studied. To obtain the
optimal conditions, the effects of operating conditions such as solvent to solid ratio, ultrasonic power, extraction time and
temperature on the extraction yield of lycopene were studied through response surface methodology. The best extraction
conditions were determined as follows: pretreatment with 95% ethanol, ethyl acetate as extraction solvent, extraction
temperature 50 ℃, extraction time 45 min, a solvent to solid ratio of 5:1 (mL/g) and ultrasonic power 270 W. Under
these conditions 250.1 mg of lycopene was obtained from 1 kg of tomato peal by UAE. The lycopene compositions of
extracts were identified by high-performance liquid chromatography-mass spectrometry (HPLC-MS). Compared with the
conventional solvent extraction, UAE was more efficient and rapid to extract lycopene from tomato peel, due to the strong
disruption of the structure of peel tissue under ultrasonic irradiation, as observed by microscopy.

Component Analysis
Changes in Fatty Acids during Salting and Drying of White Croaker (Argyrosomus amoyensis)
CAI Qiuxing1,2,3, WU Yanyan2, LI Laihao2,*, YANG Xianqing2, ZHAO Yongqiang2, WANG Yueqi2
2015, 36(12):  76-81.  doi:10.7506/spkx1002-6630-201512014
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In this paper, the changes in fatty acids of white croaker (Argyrosomus amoyensis) during the salting and
drying processes were analyzed by gas chromatography-mass spectrometry (GC-MS), and relevant indicators of lipid
oxidation including peroxide value (POV) and thiobarbituric acid reactive substance (TBARS) were measured to reveal
the relationship between the fatty acid composition and lipid oxidation. The results showed that white croaker contained
24 fatty acids including 26.41% saturated fatty acids (SFA), 20.26% monounsaturated fatty acids (MUFA) and 53.33%
polyunsaturated fatty acids (PUFA); 12.49% essential fatty acids; and eicosapentaenoic acid (EPA) and docosahexaenoic
acid (DHA) together accounting for 40.70% of the total fatty acids. During salting the content of SFA significantly increased
whereas those of MUFA and PUFA significantly decreased (P < 0.05). Both POV and TBARS values increased first and
then decreased, showing their peaks on day 1 and day 3, respectively. Correlation analysis showed that the increase in SFA
was negatively significantly related to MUFA (P < 0.05), and was highly negatively related to PUFA (P < 0.01). However,
there was no correlation between MUFA and PUFA; SFA was positively significantly related to POV and TBARS (P < 0.05)
whereas PUFA was negatively related to POV (P < 0.05) and highly negatively related to TBARS (P < 0.01). Thus, white
croaker was rich in unsaturated fatty acids and the salting process had significant influences on eight major fatty acids. More
SFAs were produced in response to lipid peroxidation while significantly decreasing the contents of MUFA and PUFA were
sed. PUFA were more susceptible to lipid oxidation.

 

Association between Flavor Variation and Muscle Quality of Grass Carp
YANG Jing, WANG Jianhui, LIU Yongle*, CHEN Qi, YU Jian, WANG Faxiang, LI Xianghong
2015, 36(12):  82-86.  doi:10.7506/spkx1002-6630-201512015
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This study aimed to investigate the relationship between odor and quality changes of freshwater fish. Electronic
nose was used to analyze the volatile components of grass carp muscle during different storage periods. Principal component
analysis (PCA), linear discriminant analysis (LDA) and sensor loadings analysis were used to study the sensor response
data acquired, combined with the thiobarbituric acid reactive substances (TBARS) values for a comprehensive assessment.
The results showed that grass carp muscle samples stored for different periods could be distinguished by 10 electronic nose
sensors. The sensor responses of nitrogen oxides, amines and aliphatic aromatic substances were changed dramatically during
the later periods of storage. For grass carp muscle stored for 12 h at room temperature, changes in sensor responses were
more evident for amines and aliphatic aromatic substances, which can be an important basis for freshness detection of grass
carp muscle by electronic nose. TBARS values showed an upward trend with extending storage time. Both electronic nose
and TBARS test results showed that chilled storage for 12 days followed by 12 h at room temperature were two important
time points of freshness changes of grass carp muscle. According to the correlation analysis, aliphatic-methane sensor can
be used as a detection method to judge the freshness of grass carp muscle under different storage conditions described in this
paper and therefore provide an important basis for freshness detection and control of grass carp.

Antioxidant Properties and Flavor Characteristics of Steamed Bread Fermented by Lactobacillus plantarum Isolated
from Traditional Sourdough
CHENG Xiaoyan1, SUN Yinfeng1, LIU Na1, HUANG Weining1,*, LI Ning2, FILIP Arnaut3
2015, 36(12):  87-92.  doi:10.7506/spkx1002-6630-201512016
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In this study, steamed bread (ZLPS) fermented by Lactobacillus plantarum subsp. plantarum isolated from
traditional sourdough were studied for their antioxidant property and flavor characteristics. Common wheat steamed
bread (WS) and steamed bread (LPS) fermented by Lactobacillus plantarum Biogreen 300 were used as controls. The
antioxidant properties of the three samples were evaluated by total phenolic content (TPC) and 1,1-diphenyl-2-picrylhydrazyl
(DPPH) radical-scavenging ability while the flavor characteristics were determined using solid phase mictroextraction-gas
chromatography-mass spectrometry (SPME-GC-MS). The results showed that fermentation by Lactobacillus plantarum
subsp. plantarum isolated from traditional sourdough was able to significantly inhibit the decrease of antioxidant properties
of steamed bread samples caused by steaming. Compared to WS, the TPC of steamed bread fermented by Lactobacillus
plantarum subsp. plantarum was increased by 108.70%, while its DPPH radical-scavenging capacity was 13.65 times higher
than that of WS. The total content of volatile flavor compounds was increased by 53.11% for LPS and 56.92% for ZLPS,
respectively, suggesting enhanced flavor of the steamed breads. ZLPS also produced a number of unique flavor substances
such as iso-amyl acetate, 6-methyl-5-heptene-2-one, 3-octanol, 2-ethyl-1-hexanol, and acetic acid 2-phenylethyl ester.
Furthermore ZLPS showed the highest sensory evaluation scores.

Determination of Ellagic Acid from Six Red Raspberry Cultivars Grown in Northeast China Using RP-HPLC
WANG Jinling1, LI Liangliang1, Lü Changshan2
2015, 36(12):  93-96.  doi:10.7506/spkx1002-6630-201512017
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A reversed phase high performance liquid chromatography (RP-HPLC) method was established to determine
the contents of ellagic acid in six red raspberry cultivars grown in northeast China. Meanwhile, the results were compared
with those of the blueberry fruit. A SinoChrom DS-BP C18 column (150 mm × 4.6 mm, 5 μm) was used to separate ellagic
acid; the mobile phase was a mixture of 0.3% phosphate and methanol solution (60:40, V/V) at a flow rate of 1.0 mL/min;
the column temperature was set at 30 ℃ and the UV detection wavelength was 254 nm. Our results indicated that ellagic
acid could be separated well, and a good linear relationship appeared between the content of ellagic acid in the range of 0.1–1 μg
and peak area with correlation coefficient of 0.999 3. The relative standard deviation (RSD) was 0.06% for precision, 0.09% for
reproducibility, and 0.39% for stability. The average recovery rates of ellagic acid from spiked samples were between 93.00% and
98.62% with RSD of 0.21%–0.42%. The proposed method is convenient, accurate, and repeatable. The contents of total ellagic
acid in different red raspberry cultivars varied from 39.10 to 155.98 mg/100 g, and the content of free ellagic acid was in the range
of 1.24 to 8.26 mg/100 g. Red raspberry is rich in ellagic acid, and it could be fully developed and utilized.

Effect of Synthetic Preservatives on Volatile Flavor Compounds in Caviar of Sturgeon (Huso dauricused × sturger schrenckii)
HUANG Hui1, HE Dan1,2, LI Laihao1, LIN Wanling1, WEI Ya1, YANG Xianqing1, HAO Shuxian1,*
2015, 36(12):  97-103.  doi:10.7506/spkx1002-6630-201512018
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Changes in the volatile flavor compounds of sturgeon caviar (Huso dauricused × sturger schrenckii) during cold
storage were analyzed by solid phase microextraction (SPME) coupled to gas chromatography-mass spectrometry (GCMS)
through NIST 05a.L mass spectral library search and alignment. Stugeon caviar was divided into four groups including
control group (with no additives), group A1 (with 0.5‰ potassium sorbate and 0.2‰ ascorbate), group A2 (with 0.5‰
potassium sorbate, 0.2‰ ascorbate and 0.2‰ nisin), and group A3 (with 0.5‰ potassium sorbate, 0.2‰ ascorbate and 0.2‰
L-ascorbyl palmitate). A total of 46 volatile compounds were identified in fresh sturgeon caviar. The compounds responsible
for the flavor of sturgeon carviar were mostly aldehydes, among which, hexanal, heptanal, octanal, and nonanal showed
higher levels. In addition, the unique lemony and woody aroma of fresh caviar may contribute to D-linonene, longifolene and
caryophyllene. The loss of volatile flavor compounds in sturgeon caviar was prevented by additive treatments in the present
study, and the levels of ketones and alcohols were decreased as well. The reduction reaction of aldehydes was promoted in
caviars by the addition of 0.5‰ potassium sorbate, 0.2‰ ascorbate and 0.2‰ nisin, thus leading to a substantial decrease
in aldehydes and a notable increase in esters. Finally, the changes in aldehydes caused by A1 and A3 treatments were
responsible for a stronger fishy and grassy smell of sturgeon caviar.

Analysis of Nutrients and Heavy Metals in Tender Stem of Triarrhena lutarioriparia from the Dongting Lake Area
XIAO Junjiu1, ZHAO Lingyan1, SHI Xingbo1, NIE Can1,2, DENG Fangming1,*
2015, 36(12):  104-107.  doi:10.7506/spkx1002-6630-201512019
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This study was conceived to analyze the nutritional value and prospect of the tender stems of Triarrhena
lutarioriparia growing on the beach of Dongting Lake. The fresh samples were peeled and separated into two portions:
one was blanched before refrigerated storage, and the other was directly refrigerated. The two portions were tested for
major chemical components. The results showed the fresh and blanched tender stems to contain 91.86% and 89.82%
moisture, 3.08% and 3.72% total sugar, 1.10% and 1.86% reducing sugar, 2.90% and 3.55% protein, 31.81% and
43.67% total dietary fiber (dry basis), and 0.36% and 0.33% total ash (dry basis), respectively. The tender stems of
Triarrhena lutarioriparia was found to contain 15 amino acids and a number of elements including Ka, Na, Ca, Mg, Mn,
Zn, Cu, and Se but no Pb, Cd or Cr, as well as lower amounts of Hg and As than the national standard limits of China.

Determination of Naturally Occurring Sugars in Wine by Ion Chromatography with Integrated Pulsed Amperometric Detection
MA Jiamin1,2, CUI He1,*, ZHANG Wenhao1, LI Li3, DONG Lizhen1, LI Huixin1
2015, 36(12):  108-112.  doi:10.7506/spkx1002-6630-201512020
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We developed a method for the determination of eight naturally occurring sugars in wine by ion chromatography
with integral amperometric detection. We used potassium hydroxide (KOH) produced by eluent generator electrolysis for
gradient elution. On CarboPac PA20 anion exchange column, all eight target compounds could be separated completely in 30
minutes. The limits of detection (LODs) of these analytes by the integral amperometric detector were very low, and a wide
linear range was found. The relative standard deviations (RSDs) for six replicate determinations varied from 4.9% to 8.7%,
and the recoveries of these eight sugars from spiked samples ranged from 81.5% to 95.1%. Our method proved to be simple,
fast, sensitive and suitable for the analysis of the eight naturally occurring sugars in wine by achieving good separation
without derivatization.

Analysis of Total Selenium and Inorganic Selenium in Apostichopus japonicus from Different Regions by Hydride Generation-Atomic Fluorescence Spectrometry
LI Xiumei1,2, SUN Guohua2, YANG Jianmin2,*, REN Lihua2, MA Yuanqing2, GU Weili2, ZHANG Jian2, LIU Zhaocun3
2015, 36(12):  113-118.  doi:10.7506/spkx1002-6630-201512021
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This study aimed to explore the selenium status of Apostichopus japonicus from the Yellow Sea and the Bohai
Sea. Total selenium and inorganic selenium were detected by hydride generation-atomic fluorescence spectrometry (HGAFS).
This method had a wide linear dynamic range and good precision and accuracy, so it was suitable for the determination
of different forms of selenium in aquatic products. Selenium levels in four populations of Apostichopus japonicus from
Dalian, Dongying, Yantai, Qingdao, and Rizhao respectively were examined. Among five tissues investigated, respiratory
tree contained the highest levels of organic selenium and inorganic selenium which were averaged at (14.171 ± 3.412) and
(6.194 ± 3.829) mg/kg, respectively, and both of which followed the same decreased order of respiratory tree > digestive
tract > muscle > inner body wall > outer body wall. The proportions of organic selenium in body wall and muscle (the edible
part) were between 75.6% and 89.4%, except for Apostichopus japonicas muscle from Dongying containing the lowest level
(53.6%) of organic selenium. There were significant differences in the contents of total selenium and inorganic selenium in
the same tissues from different regions, and the contents of inorganic selenium in respiratory tree, digestive tract and muscle
were higher in Dongying population than in those from other regions.

Niacin and Zeaxanthin Contents in Different Maize Kernels
DENG Xiaojing, MEI Xiupeng, XU De, CHEN Xining, LIU Xiaoli, LIU Chaoxian, CAI Yilin*
2015, 36(12):  119-124.  doi:10.7506/spkx1002-6630-201512022
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Microbiological and spectrophotometric methods were respectively used to determine the contents of niacin and
zeaxanthin in maize kernels of 123 from 3 200 inbred lines to study the effects of maize type, kernel color and kernel type
on the contents of both phytochemicals in maize as well as their correlation. The results showed that the niacin content
of maize was in the range of 0.57–4.80 mg/100 g; the niacin content of waxy maize was much higher than that of normal
maize, the niacin content of white maize was higher than that of yellow maize, and the niacin content of purple maize was
between those of white maize and yellow maize. No significant differences in niacin contents were found among different
kernel types and among different kernel types with the same kernel color. The zeaxanthin content of maize varied from 0.35
to 4.03 mg/kg. The zeaxanthin content of waxy maize was much lower than that of normal maize, the zeaxanthin content of
white maize was lower than that of yellow maize, and the zeaxanthin content of purple maize was between those of white
maize and yellow maize. No significant differences in zeaxanthin contents existed among different kernel types and among
different kernel types with the same kernel color. These results indicated that the different maize types and kernel colors of
maize significantly affected the contents of niacin and zeaxanthin, whereas the main effect of kernel type and its interactive
effect with kernel color were not significantly different. Moreover, there was a moderate but significant negative correlation
between niacin content and zeaxanthin content in maize (r = - 0.361, P < 0.01), indicating that the higher the niacin content,
the lower the zeaxanthin content. These findings could provide a reference for the reasonable application of maize kernels
and the improvement of maize breeding.

Determination of Multi-Elements in Triticale by Inductively Coupled Plasma Mass Spectrometry
NIE Xidu1, FU Liang2,*, TANG Lijuan3, HUANG Jianhua4
2015, 36(12):  125-128.  doi:10.7506/spkx1002-6630-201512023
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A method for simultaneous and quantitative determination of 18 elements including B, Na, Mg, Al, K, Ca, Ti, V,
Cr, Mn, Fe, Co, Ni, Cu, Zn, Se, Cd and Pb in triticale was established. Samples were digested by using a mixture of HNO3
and H2O2 in a closed-vessel microwave system, and the 18 elements in the test solution were then detected by inductively
coupled plasma mass spectrometry (ICP-MS). The mass spectral interferences caused by polyatomic ions were corrected
by dynamic reaction cell (DRC). Sc, Ge, Rh and Bi were used as internal standard elements to correct the matrix effect
and signal drift. The linear ranges of Mg, Al, K and Ca were 0–10.00 mg/L, whereas those of the other elements were
0–50.00 μg/L. The limits of detection (LODs) of the 18 elements were in the range of 3.04–17.38 ng/L with relative standard
deviations (RSDs) between 0.95% and 12.50%. The accuracy and precision of this method were confirmed by reference
standard material (GBW 10011, wheat). The contents of B, Mg, K, Ca, Fe, Mn and Se in triticale were obviously higher than
those in normal wheat, while the content of Na in triticale was lower than that in normal wheat. The technique presented in
this study is useful for the quality control and nutritional evaluation of triticale.

Relationship between Nutrient Element Distribution and Processing Degree of Rice
QIAN Lili, SONG Chunlei, LI Zhijiang, ZHANG Dongjie*
2015, 36(12):  129-132.  doi:10.7506/spkx1002-6630-201512024
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This study was performed to examine the distribution profiles of nutrient elements in rice. Rice grains of the
cultivar Longjing 40 were processed to different grades according to the staining method in the Chinese national standard
GB/T 5502—2008. A total of 17 kinds of nutrient elements in rice with different processing levels were determined by
inductively coupled plasma mass spectrometry (ICP-MS) and quantitative analysis of the elements on the surface, near the
surface, near the core, and in the core of rice caryopsis was conducted by X-ray photoelectron spectroscopy (XPS). The
results showed that the contents of 11 kinds of elements including Na, Mg, Al, K, Ca, V, Cr, Mn, Fe, Co, Cu, Zn, Rb, Sr, Mo,
Cs and Ba differed significantly in different grades of rice (P < 0.01), and their loss rates varied across grades. The contents
of Na, K, Ca and Fe were different in different parts of rice grain, and their contents were higher on the surface than near
the core and in the core of rice caryopsis. On the other hand, the distribution of nutrient elements in the caryopsis was not
uniform, and rice processing may cause losses of the nutrient elements in different levels.

Preparation of High-Purity Chlorogenic Acid Derivatives from Purple Sweet Potato
LI Fu1, CHEN Bin1, LI Lianhong2, WANG Mingkui1
2015, 36(12):  133-137.  doi:10.7506/spkx1002-6630-201512025
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The purpose of the present study was to prepare high-purity and high-value chlorogenic acid derivatives from
purple sweet potato. Purple sweet potato slices were extracted with hot water. The extracted compounds were separated with
D72 macroporous resin, sephadex LH-20 column chromatography and preparative high performance liquid chromatography
(HPLC) to obtain high-purity chlorogenic acid analogues which were identified as isochlorogenic acid A, isochlorogenic acid
B, isochlorogenic acid C and 3,4,5-O-tricaffeoyl quinic acid, respectively, by nuclear magnetic resonance technique. HPLC
analysis suggested that the purities of these analogues were all over 98%. The developed method can be used to rapidly
obtain standard samples of chlorogenic acid derivatives from purple sweet potato, while avoiding effectively the negative
effects of the anthocyanins on product color and purity.

Analysis of Volatile Components in Leaves of Dysosma versipellis from Guizhou Province
LI Jinhui
2015, 36(12):  138-141.  doi:10.7506/spkx1002-6630-201512026
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This work presents a comparative analysis of the volatile components in the leaves of Dysosma versipellis from
Yaorenshan and Maolan nature reserve in Guizhou province of China. The volatile components were extracted from the
leaves of D. versipellis by headspace solid phase microextraction, identified by GC-MS and quantified by the peak area
normalization method. The results showed that 39 compounds were extracted from the leaves of D. versipellis grown in
Yaorenshan, among which 31 compounds were identified, together accounting for 91.22% of the total volatile components,
and the predominant components included espatulenol (22.34%), β-terpinene (20.59%), limonene (10.47%), (1S)-α-pinene
(6.56%), (+)-ledene (4.52%), γ-muurolene (4.11%) and caryophyllene (3.22%). A total of 25 compounds were extracted
from D. versipellis in Maolan reserve, among which, 23 were identified and their relative contents accounted for 87.77%
of the total volatile components. The most abundant volatile components included dodecanal (15.58%), espatulenol
(13.63%), p-cymene (6.95%), γ-muurolene (4.89%), decanal (4.67%), undecanal (4.14%), d-cadinene (3.97%), α-cubebene
(3.91%), β-eudesmol (3.40%) and γ-elemene (3.24%). Eight compounds were common to both habitats, but there were large
differences in their relative contents. The differences in volatile components of D. versipellis may be closely associated with
producing area and growing environment.

Bacterial Diversity of Daqu for Yanggaomeijiu as Determined by PCR-Mediated DGGE
LI Yan1,2, DONG Zhenling1,3, LI Jia1, MOU Dehua1,*
2015, 36(12):  142-147.  doi:10.7506/spkx1002-6630-201512027
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Purpose: To detect and analyze the bacterial diversity of Yanggaomeijiu Daqu (traditional Chinese fermentation
starter) by polymerase chain reaction-denatured gradient gelelectrophoresis (PCR-DGGE) for further understanding of the
flavor characteristics of Yanggaomeijiu. Methods: Samples of Yanggaomeijiu were processed and then extracted to obtain
total DNA for PCR amplification and the amplified DNA bands were excised from the gels for sequence analysis by DGGE.
Results: By using PCR-DGGE, the genus of Weissella, Lactobacillus, Pediococcus, Sporolactobacillus, Staphylococcus,
Thermoactinomyces and 4 unculturable bacterial strains were identified in Yanggaomeijiu Daqu. Conclusions: This work
shows that the bacterial diversity is abundant in Yanggaomeijiu Daqu among which, lactic acid bacteria constituted the
largest group.

Determination of Metal Elements Profile and Regional Distribution in Peach Fruit from Fenghua City
WU Dajun1, LIN Qingwu2, WU Xiaoyi2, CAI Yan2,*, YANG Zhenfeng2, HE Xiaoyu3
2015, 36(12):  148-152.  doi:10.7506/spkx1002-6630-201512028
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In this study, microwave digestion-inductively coupled plasma-atomic emission spectrometry (ICP-AES)
was applied to determine metal elements in peaches (the Hujingmilu and Yulu cultivars). The effects of acid system
and best spectral line on the determination of metal elements were examined to optimize the two conditions. Under the
optimum experimental conditions, the accuracy of the method was validated with recoveries ranging from 82.82%–118.3%
and relative standard deviation (RSD) of 2.28%–18.4%, and limits of detection (LOD) of 0.1–1 μg/L. Peaches from
different areas in Fenghua contained several macro elements including K, Ca, Mg, and Fe, and four trace elements including
Cu, Mn, Se, and Zn as analyzed by the proposed method. There existed differences in the regional distribution of these
elements in peaches.

Optimization of Supercritical CO2 Extraction of Abalone Visceral Oil by Response Surface Methodology and Analysis of Fatty Acid Composition
TANG Peng1, DUAN Haixia2, XIA Jinmei3,*, WENG Wuyin1, LI Qian3, XU Jianzhong3, LIN Yi3, XU Chen3
2015, 36(12):  153-159.  doi:10.7506/spkx1002-6630-201512029
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Supercritical CO2 was used to extract abalone visceral oil. To optimize the extraction conditions, the statistical
software SAS 9.2 was applied to design the experiment with response surface methodology. The impacts of pressure,
temperature, and time on extractability were investigated. It was found that the optimum extraction pressure, temperature
and time were 31.2 MPa, 42.3 ℃ and 9.4 min, respectively. The extraction rate was 75.23% under the optimized conditions.
Ultra performance liquid chromatography-quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF-MS) was then
used to analyze the extracted oil. A total of 39 fatty acids with different lengths of carbon chain and numbers of double
bonds were detected, including 9 kinds of saturated fatty acids, 8 kinds of monounsaturated fatty acids and 22 kinds of
polyunsaturated fatty acids.

GC-MS Analysis of Arom Chemical Composition of Red Raspberry Wines Fermented with Three Different Yeast Strains
LIU Yana1, YANG Hua2, GUO Dejun1,*
2015, 36(12):  160-165.  doi:10.7506/spkx1002-6630-201512030
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The aroma components of red raspberry wines fermented with three different wine yeast strains, D254, 71B and
D15, were extracted with headspace-solid phase micro extraction (HS-SPME) and then separated and identified by gas
chromatography-mass spectrometry (GC-MS) through mass spectral library search. Total ion current (TIC) peak area
normalization method was used to determine the relative contents of aroma components. A total of 105 flavor components
were detected, among which 35, 48 and 57 compounds were detected in red raspberry wines fermented with D254, 71B
and D15, respectively, with 8 being common to these three samples. The main aromatic compound in red raspberry wine
fermented with D254 was 1-buten-ol-3-methyl (54.39%) while those in the wine fermented with 71B were 2-propenoic
acid octyl ester (12.41%), demecolcine (12.06%) and ethyl caprate (8.21%), and were glycerol tricaprylate (11.06%) and
amfepramone (8.81%) in the wine fermented with D15. Overall, GC-MS analysis and sensory evaluation suggested that red
raspberry wine fermented by 71B contains more aroma substances and is suitable for the pubic taste. Thus, 71B could be the
best yeast strain for the production of red raspberry wine.

Development of Squalene Certified Reference Material
CHEN Weizhu1,2, JIN Wenhui1, FANG Hua1, XIE Quanling1, ZHANG Yiping1, HONG Zhuan1,*
2015, 36(12):  166-170.  doi:10.7506/spkx1002-6630-201512031
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Squalene certified reference material was developed by purification of crude squalene. The structure of the
certified reference material was confirmed by infrared spectroscopy (IR), high resolution mass spectrometry (HRMS) and
nuclear magnetic resonance (NRM) and squalene was divided into 150 aliquots. The homogeneity and stability tests and
quantitative analysis were carried out by gas chromatography-flame ionization detection (GC-FID). Fifteen randomly
selected aliquots showed good homogeneity as indicated by F-test analysis at a 95% confidence interval. The test samples
were stable at −18 ℃ for 24 months. A cooperative certification was conducted with 8 qualified laboratories. The certified
purity value of the reference material was 99.57% with a relatively expanded uncertainty of 0.30% (k = 1.96). The reference
material can conform to the technical requirement of the certified reference material. This material was intended for use in
the method validation and quality control regarding squalene.

Safety Detection
Detecting Hollowness of White Radish Based on Hyperspectral Imaging
HU Pengcheng1, SUN Ye1, WU Hailun1, GU Xinzhe1, TU Kang1, ZHENG Jian2, PAN Leiqing1,*
2015, 36(12):  171-176.  doi:10.7506/spkx1002-6630-201512032
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Hollowness is a common defect found in radish postharvest storage. In the present study, a prototype hyperspectral
imaging system was designed for evaluating the internal quality of white radish. Three different detection models including
semi-transmittance, reflectance and transmittance were evaluated and used to extract the hyperspectral imaging data of
white radish, partial least squares discriminant analysis (PLS-DA), support vector machine (SVM), and artificial neural
network (ANN) algorithms were then used to establish the hollowness model for radish identification and the recognition
accuracy was calculated. The prediction accuracies based on PLS-DA, SVM, and ANN were 72.5%, 72.5% and 83.3% in
semi-transmittance mode, 82.5%, 82.5% and 92.3% in reflectance mode, and 90.0%, 90.0% and 94.3% in transmittance
mode, respectively. The results showed that hyperspectral transmittance imaging achieved the best prediction results among
the three different detection models, ANN algorithm was the optimal algorithm to build hollowness discrimination model.
Hyperspectral transmittance imaging in the combination with ANN gave the best results with a prediction accuracy of 94.3%
for detecting the internal hollowness of white radish. Therefore, it was feasible to use hyperspectral transmittance imaging
system for detecting the hollowness of white radish in postharvest storage.

Assessment of Fresh Pork Quality by LF-NMR: Parameter Optimization
WANG Zhiyong, WANG Xin*, XIA Yimiao, HUANG Yuanfen, LIU Baolin
2015, 36(12):  177-184.  doi:10.7506/spkx1002-6630-201512033
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Information about water mobility and distribution in meat can be provided by proton nuclear magnetic resonance
(NMR) relaxometry. The suitable measurement parameters of low-field proton nuclear magnetic resonance (LF-NMR)
relaxometry will not only be helpful for the reliability of experiment data, which reflect accurately the information on the
sample, but also be beneficial for enhancing the detection efficiency. In this study, using fresh lean pork from the hind
legs, the effects of LF-NMR parameters on the accuracy, stability and reproducibility of the experimental results were
investigated. No significant changes in experimental data (P > 0.05) were observed when the tR (repetition delay) and Echo
Count (sampling data number) were set as more than 4 500 ms and more than 3 000, respectively. The optimal conditions
were determine as follows: τ value (time between 90 degree pulse and 180 degree pulse) of 200 μs, N of 8 and SW value
(receiver bandwidth) of 250 kHz during the test. Good stability and reproducibility could be guaranteed when the sample
was cut into lumps (about 4–5 g), incubated in a water bath at 32 ℃, and subsequently transferred to the probe before the
measurement. These results can provide appropriate detection conditions for applications of LF-NMR for quality assessment
of fresh lean pork and other meats.

Optimization of Headspace Solid Phase Micro-Extraction Conditions for GC-MS Analysis of  Volatile Metabolites from Staphylococcus aureus
SHI Hui, TANG Junni, CHEN Juan*, WANG Qiong
2015, 36(12):  185-190.  doi:10.7506/spkx1002-6630-201512034
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Volatile metabolites from Staphylococcus aureus cultured with tryptone soy broth (TSB) were extracted under
different conditions namely three types of fiber (65 μm PDMS/DVB fiber, 75 μm CAR/PDMS fiber and 50/30 μm DVB/
CAR/PDMS fiber), three extraction times (20, 30 and 40 min) and three extraction temperatures (50, 65 and 80 ℃),
respectively. The extracts were detected by gas chromatography-mass spectroscopy (GC-MS). The optimal extraction
conditions were determined. The results indicated that 50/30 μm DVB/CAR/PDMS fiber was suitable for the extraction of
various components and more comprehensive information was obtained using this fiber. Abundant amounts and response
intensities of bacterial volatile metabolites were extracted at 80 ℃ for 30 min. Accordingly the optimal extraction conditions
for volatile metabolites from S. aureus were obtained. Using the established extraction method, the main volatile compounds
produced by S. aureus cultured in TSB were detected to be alcohol, 1-decanol, 3-hydroxy-2-butanone, acetone, acetic acid,
benzyl alcohol, 3-methyl-1-butanol, indole, 1-octanol and octanoic acid. This extraction method can provide a valuable tool
for the analysis of bacterial volatile metabolites.

Stable Isotope Distribution of Carbon, Nitrogen and Hydrogen in Yak Meat from Different Regions
XIANG Yang, HAO Lizhuang, NIU Jianzhang, ZHANG Xiaowei, CHAI Shatuo*
2015, 36(12):  191-195.  doi:10.7506/spkx1002-6630-201512035
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This study aimed to confirm the possible traceability of yak meat samples from different regions using stable
isotopes. The δ13C, δ15N, and δ2H values of yak meat samples (muscle crude fat and de-fatted muscle) from Henan county
and Datong county of Qinghai province, and Hongyuan county and Jiulong county of Sichuan province were tested using
isotope ratio mass spectrometry (IRMS). The composition characteristics of δ13C, δ15N, and δ2H of yak meat samples were
compared and analyzed. The results demonstrated that the δ13C, δ15N, and δ2H differed significantly among meat samples
from different yak tissues (P < 0.05 or P < 0.01). The distinguishing capacity for de-fatted muscle was better than for muscle
crude. When the indicators of stable isotope were taken into comprehensive consideration, yak meat samples from different
places was better distinguished as compared to the individual indicators, and the combined analysis of stable nitrogen and
hydrogen isotopes provided potential indicators for tracing the origin of yak meat samples with an accuracy up to 85%. It is
a promising approach to classify yak meat based on δ13C, δ15N and δ2H combined with multivariate statistical methods.

Analysis of Chemical Contaminants and Risk Assessment of Pesticide Residues in Carambola (Averrhoa carambola) Fruit
DUAN Yun1, GUAN Ni2, DENG Aini1, LUO Jinhui1
2015, 36(12):  196-200.  doi:10.7506/spkx1002-6630-201512036
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Chemical contaminant residues in carambola (Averrhoa carambola) fruits collected from Guangdong, Guangxi,
Hainan and Fujian provinces were assayed. The results showed that the frequency of occurrence of pesticide residues in
wholesales and open markets were low whereas the largest number of pesticide residues in sample collection spots near
cultivation base was detected. Samples contaminated with pesticide residues exceeding the maximum residue levels (MRLs)
existed mainly in the collection spots. Three pesticides detected at the highest concentrations were beta-cypermethrin,
carbendazim and chlorbenzuron. Based on deterministic method for risk assessment of pesticides, the potential health risk of
21 other pesticide residues in carambola was low. However, the potential risk of dicofol was high. The semi-probabilistic approach
was applied to analyze the potential risk of dicofol. Results showed that at a 99.5% confidence level (P99.5) exposure levels in
2- to 10-year-old subgroups were over the value of allowable daily intake (ADI). There existed potential risk from dicofol for
these age groups. Thus, we should put more emphasis on monitoring samples collected from near cultivation base, modifying and
establishing MRLs for dicofol, carbendazim and chlorbenzuron and formulating alternative pesticides.

Investigation on Laser-Assisted Thermal Infrared Imaging Method for Detection of Food Spoilage
JIN Chao1, BI Zhongyuan1, SHENG Lei1,*, LIU Jing1,2,*
2015, 36(12):  201-204.  doi:10.7506/spkx1002-6630-201512037
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Monitoring food spoilage (FS) has been one of the important tasks in the food industry. Exploring a fast and highsensitivity
detection method for FS is extremely important. This study aimed to explore the relationship between temperature
and the degree of FS during the process of FS. Fresh pork was used as samples and laser was used as the external heat
source to enhance the differences in thermal expression. An infrared camera was used to detect the temperature variation
rate of the samples. The pH values of the samples were measured and used as the monitoring indicator of FS degree. The
thermophysical parameters of both fresh and spoiled samples were measured using differential scanning calorimetry. The
variations in the surface temperature of samples were simulated using the numerical method according to the heat transfer
equation. Finally, the relationship between the FS degrees and temperature variation rates of samples was modeled. The
results of this study can be useful in exploiting a convenient and low-cost FS detection technique.

Quantitative Identification of Added Water in Buffalo Milk Based on Multi Statistical Analysis
HUANG Li, LI Ling, FENG Ling, ZENG Qingkun*, LIN Bo, TANG Yan, NONG Haoru, YAN Pan
2015, 36(12):  205-208.  doi:10.7506/spkx1002-6630-201512038
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Seven main quality indicators of buffalo milk added with different volume ratios of water were measured by
conventional methods based on one-way analysis of variance analysis (ANOVA), principle component analysis (PCA),
and multiple linear regression for quantitative identification of added water in buffalo milk. One-way ANOVA was used to
determine the significant differences in the main quality indicators of different samples with added water to obtain a limit of
detection (LOD) of 7%. According to the PCA, the contribution rate of the first PC was 85.464%, and it included most of the
sample information. There was a significant linear relationship between the scores of the first PC and the content of added
water. Four quantitative model equations were built by multiple linear regression, with correlation coefficients (R2) of 0.965,
0.982, 0.986 and 0.989 and mean absolute errors of −0.23%, −2.40%, 0.23% and 1.28%, respectively, which could be used
for quantitative identification of added water in buffalo milk.

Determination of Sudan Ⅰ by Chemiluminescent Enzyme Immunoassay
FAN Yan, MENG Wei, ZHU Lixin, LIU Renrong*, XU Long, QIU Xuemei, YANG Fanfan
2015, 36(12):  209-212.  doi:10.7506/spkx1002-6630-201512039
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An indirect competitive chemiluminescent enzyme immunoassay (CLEIA) was developed for the detection of
Sudan Ⅰ in food products. The CLEIA conditions including molar ratio of coating antigen to carrier, antigen concentration,
and dilution ratio of antibody were optimized. In the standard curve of the optimized CLEIA, the linear range was 0.156–
5 ng/mL, the half maximal inhibitory concentration (IC50) was 0.679 ng/mL and the limit of detection (LOD) was
0.078 9 ng/mL. The CLEIA showed good recoveries with spiked chili powder ranging from 75.08% to 112.18%. Compared
with ELISA method, the IC50 values of CLEIA was reduced by 30%. The proposed method has a high sensitivity.

Rapid Determination of Residues of Prochloraz and Its Metabolite 2,4,6-Trichlorophenol in Fruits Using Gas Chromatography with Tandem Mass Spectrometry
LU Junwen, LI Rong*, YANG Fang, HUANG Siyun, CHEN Lisi
2015, 36(12):  213-217.  doi:10.7506/spkx1002-6630-201512040
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Purpose: To develop a rapid method for the determination of residues of prochloraz and its metabolite,
2,4,6-trichlorophenol, in fruits using matrix dispersive solid-phase extraction and gas chromatography with tandem mass
spectrometry (GC-MS-MS). Methods: Samples were extracted with acetonitrile, cleaned by matrix dispersive solid-phase
extraction using PSA and C18, detected by GC-MS-MS under multiple reaction monitoring mode, and quantified by an
external standard method using matrix-match standard solution. Results: In the linear range of 0.004-0.400 mg/kg, the
correlation coefficients for prochloraz and 2,4,6-trichlorophenol were 0.999 4 and 0.999 2, respectively. Their average
recoveries at spiked levels of 0.01, 0.02 and 0.10 mg/kg were 80.1%–101.5% and 79.0%-97.4% with relative standard
deviations of 2.8%–6.8% and 2.0%–6.0%, respectively, and their limits of quantification (LOQ) (RSN = 10) were 0.004 and
0.005 mg/kg, respectively. Conclusions: The proposed method is simple and sensitive with a wide range of measurement,
and can be suitable for the analysis of prochloraz and 2,4,6-trichlorophenol residues in fruits.

Determination of Triptolide and Wilforine in Honey by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
LEI Meikang1, PENG Fang1, ZHU Zitong1, DING Tao2, XU Jiawen1, WU Xiaoqin1
2015, 36(12):  218-220.  doi:10.7506/spkx1002-6630-201512041
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A method based on ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS) has
been proposed for the determination of triptolide and wilforine residues in honey. The samples were dissolved in water and
extracted with acetonitril, separated on a Hypersil GOLD C18 column (50 mm × 2.1 mm, 1.9 μm) with gradient elution. The
determination was carried out with electrospray ion source under the positive mode and multiple reaction monitoring (SRM)
mode. The concentrations of triptolide and wilforine in the range of 0.01–20 ng/mL were linearly correlated to the peak area,
with correlation coefficients greater than 0.997. The limits of quantification (RSN > 10)for both triptolide and wilforine
were 0.05 μg/kg. The recoveries of triptolide and wilforine were 69.9%–101.5%, respectively, at spiked concentrations of
0.05 μg/kg and 1.0 μg/kg, with relative standard deviations (RSD, n = 6) lower than 10%. Our results indicate that the developed
method is rapid, sensitive and accurate for the qualitative and quantitative analysis of triptolide and wilforine in honey.

Rapid Determination of Pesticide Multi-Residues in Rice by QuEChERS and GC-MS
QIU Weifen1, ZHANG Changjuan1, WEN Liang2, FANG Yong1, HU Qiuhui1
2015, 36(12):  221-225.  doi:10.7506/spkx1002-6630-201512042
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The combination of QuEChERS and gas chromatography-mass spectrometry (GC-MS) was employed to establish
a new method for the rapid screening 17 pesticide residues in rice, including dichlorvos, molinate, omethoate, quintozene,
propanil, chlorpyrifos-methyl, fenitrothion, pirimiphos-methyl, malathion, chlorpyrifos, phenthoate, procymidone, butachlor,
isoprothiolane, triazophos, bifenthrin and deltamethrin. Samples were extracted with a mixture of acetonitrile/acetic acid (99:1,
V/V) and salted out with anhydrous MgSO4 and NaCl. After the incorporation of N-propyl ethylenediamine (PSA) and C18 sorbent
for the purification process, GC-MS and NAGINATA™ software were used for the detection and analysis, respectively. The results
showed that the limits of detection (LOD) of the 17 pesticide residues using the established method were in the range of 0.002–
0.050 mg/kg, and their average recovery rates in a blank sample were 80%–110% with relative standard deviations (RSDs) of
1.7%–12.3%. This method was sensitive without the need for any complicated pre-treatments or expensive equipment and was
suitable for the fast screening of pesticide residues in rice. Finally, we adopted the new method to detect pesticide residues in
25 rice samples. The results showed that 3 pesticides including chlorpyrifos, triazophos and isoprothiolane were analyzed, and their
levels were lower than the MRL stipulated by the national standard of China (GB 2763—2014).

Immunomagnetic Capture PCR for Rapid Detection of Listeria monocytogenes
LI Jingheng1, GUO Huiqin2, GAO Xiaoqiang3, LIU Fang3, QIU Shi1, LI Jianwu1, ZENG Haijuan1, LIU Lan2, SONG Chunmei1, LIU Qing1,*
2015, 36(12):  226-229.  doi:10.7506/spkx1002-6630-201512043
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This experiment was conducted using immunomagnetic enrichment followed by amplification with polymerase
chain reaction (PCR) for rapid detection of Listeria monocytogenes. The best coating conditions were achieved by shaking
the prepared immunomagnetic beads at 37 ℃ for 1 h, and the amount of antibody conjugated to the immunomagnetic beads
was 100 μg/mg, leading to a capture rate of 45%. The immunomagnetic capture PCR assay was able to detect as low as
104 CFU/mL Listeria monocytogenes with 10 times higher sensitivity than direct PCR showing a limit of detection of
105 CFU/mL. This PCR assay can provide a new method for the enrichment and rapid detection of pathogenic bacteria.

Fast Simultaneous Determination of Sixteen Novel Amide Fungicides in Vegetables and Fruits by Liquid Chromatography-Tandem Mass Spectrometry
SUN Yami, Lü Yan, WU Yinliang*
2015, 36(12):  230-236.  doi:10.7506/spkx1002-6630-201512044
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A fast method was developed for simultaneously determining 16 novel amide fungicides in fruits and vegetables
using liquid chromatography tandem mass spectrometry (LC-MS-MS). Samples were extracted with acetonitrile and saltedout
by sodium chloride to partition amide fungicides into the upper acetonitrile layer. The upper supernatant was then
directly diluted with 0.1% formic acid solution before being analyzed by LC-MS-MS on an Acquity BEH C18 column with
a mixture of 0.10% formic acid solution (A) and acetonitrile (B) as the mobile phase under gradient elution conditions. The
mass spectrometer was operated in the positive ion mode using multiple-reaction monitoring (MRM). The target analytes
were quantified by matrix-matched external standard calibration. There was a good linear correlation with calibration
coefficients all above 0.994 9 between the peak areas and concentrations of the amide fungicides in the range of 2.5 × 10−4 to
0.25 mg/L. The average recoveries of the 16 compounds in cabbage, celery, strawberry and grape were 85.7%–103.9%,
and the intra-assay relative standard deviations (RSDs) were between 2.6% and 5.2%. The limits of quantification (LOQs)
of these fungicides varied from 3.0 × 10−4 to 0.01 mg/kg. The proposed method was demonstrated to be suitable for the
determination of the 16 amide fungicides in vegetables and fruits.

Packaging & Storage
Effects of Orange Oil Treatment on Structural Materials of Orange Peel Tissue
XU Jiani, CUI Wenjing, DENG Lili, ZENG Kaifang*
2015, 36(12):  237-242.  doi:10.7506/spkx1002-6630-201512045
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The effects of oleocellosis induced by orange oil on the structural materials of Navel orange peel tissue were
studied based on collapse index, color index, cell membrane and cell wall-related index. Results showed that the oil
treatment could induce oleocellosis on Navel orange and the disease was more notable as the storage time was prolonged.
Orange oil could result in a rise in lipoxygenase (LOX) activity and superoxide anion production rate of peel tissue, in
turn accelerating the degradation of the cell membrane, increasing dramatically the cell membrane permeability and the
content of malondialdehyde (MDA). During the early storage period, the contents of cell wall-related materials such as
lignin and cellulose of the oil-treated peel tissue increased quickly and the activities of pectin methylesterase (PME) and
polygalacturonase (PG) were inhibited. Thus, the cell wall could be thickened to some degree. This study can provide a
theoretical reference for exploring the mechanisms and control strategies of oleocellosis.

Effects of Freeze on the Microstructure and Texture of Crisp Grass Carp and Grass Carp Muscle
RONG Jianhua, ZHANG Liangzi, XIE Shuli, XIONG Shi, XIONG Shanbai
2015, 36(12):  243-248.  doi:10.7506/spkx1002-6630-201512046
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The microstructure and texture of crisp grass carp and grass carp muscle frozen under -18 ℃ for three days were
examined by optical microscope, scanning electron microscope and texture analyzer. The results showed that ice crystals
were formed during freezing, resulting in damage of the cell membrane and juice loss. The cooking weight loss rates of both
fishes were increased, and the cooking weight loss rate of crisp grass carp muscle was higher than that of grass carp muscle.
The texture of crisp grass carp and grass carp muscle was significantly influenced by freezing, and the effect on grass carp
muscle was more significant than that on crisp grass carp muscle. Elasticity, resilience and chewiness of the muscle of the
two fishes were decreased significantly. The shear force, hardness and adhesiveness of grass carp muscle were decreased
significantly, while those of crisp grass carp muscle remained almost unchanged. It was also observed that the differences in
texture between the frozen and fresh fish muscle after cooking were not significant.

Combination of Pichia membranaefaciens with Fungicides for Control of Postharvest Diseases of Citrus Fruit
FENG Jirui1,2, ZHOU Yahan1, ZENG Kaifang1,*
2015, 36(12):  249-254.  doi:10.7506/spkx1002-6630-201512047
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In order to reduce the dosage of fungicides and find an effective control method for postharvest diseases of citrus,
the effect of Pichia membranefaciens in combination with low-dose fungicides (carbendazim and thiophanate-methyl) on
the control of postharvest citrus diseases was studied. Fungicides which could be well combined with P. membranaefaciens
were selected and the sensitivity of common citrus pathogens to the selected fungicides was verified. The postharvest fruits
were then used to validate the controlling effect of P. membranefaciens combined with fungicides on their diseases. The in
vitro experiments showed that neither carbendazim nor thiophanate-methyl inhibited the growth of P. membranaefaciens.
However, Penicillium italicum, Penicillium digitatum and Colletotrichum gloeosporioides showed different sensitivities
to the two fungicides, but the EC50 values were all lower than 1% of the recommended dosage. The in vivo experiments
showed that the treatment with P. membranefaciens in combination with either carbendazim or thiophanate-methyl had a
better control efficacy on blue mold and green mold than the individual treatments. However, the anthracnose rot in Valencia
orange was not well controlled by Pichia membranefaciens combined with thiophanate-methyl. The combined treatments
had a synergistic control effect on the incidence of Valencia orange diseases and an additive effect on that of Jincheng, which
could be an effective strategy to maintain good commercial rates of Valencia orange and Jincheng.

Effects of UV-C Treatment on Quality and Phenylpropanoid Metabolism of Postharvest Chinese Bayberry Fruit
YU Xuan, JIANG Lulu, WANG Huanyu, JIN Peng, ZHENG Yonghua*
2015, 36(12):  255-259.  doi:10.7506/spkx1002-6630-201512048
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The effects of UV-C treatment at different dosages on postharvest quality, antioxidant activity, phenylpropane
metabolite contents, and related enzymes activities in Chinese bayberry fruit (cv. Dongkui)were investigated. The fruit were
treated with 0, 1.5, 3.0, 4.5 and 6.0 kJ/m2 of UV-C and then stored at 5 ℃ for up to 12 days. The results indicated that UV-C
treatment at 3.0 kJ/m2 had the most significant inhibitory effect on fruit decay. The decreases of fruit firmness and vitamin C
content were retarded and thus fruit quality was maintained. Meanwhile, this UV-C treatment significantly enhanced the
activities of phenyalanine ammonialyase, 4-coumarate-CoA ligase, chalcone isomerase and cinnamate 4-hydroxylase, and
maintained high levels of total phenolics, anthocyanin, carotenoids and flavonoid and high antioxidant activity during the
storage. These results suggest that UV-C treatment has a promising application prospect in quality maintenance of harvested
Chinese bayberry fruit.

Effect of Repeated Freezing and Thawing on Fatty Acid Profile Changes during Processing of Chansi Cured Rabbit
SU Yan1, XIA Yangyi1,2,*
2015, 36(12):  260-263.  doi:10.7506/spkx1002-6630-201512049
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Rabbit meat subjected to repeated cycles of freezing and thawing was use to produce Chansi cured rabbit, a
unique Chinese cured meat product. Changes in the fatty acid composition were monitored during the processing of Chansi
cured rabbit. The results showed that the fat contents of raw (frozen and thawed), cured and roasted rabbit meat significantly
decreased with increasing number of freeze-thaw cycles, and thiobarbituric acid reactive substances (TBARS) values
significantly increased when compared to those of fresh rabbit meat (P < 0.05). Palmitic acid (C16:0) and linoleic acid (C18:2)
were detected in frozen and thawed rabbit meat. The degradation of fat produced oleic acid (C18:1), during the processing of
Chansi cured rabbit. The fatty acid composition also significantly changed in the raw rabbit meat after being cured and baked
(P < 0.05). The lowest fat content of 0.023 8% and the highest TBARS value of 0.216 8 mg/kg were found in Chansi cured
rabbit with 5 repeated freeze-thaw cycles. This study has shown that repeated freezing and thawing has a significant effect on
the fatty acid composition of Chansi cured rabbit.

Effect of Surfactant on Chitosan-WPI-Nano TiO2 Composite Film on Preservative Performance
WANG Qi1,2, CHEN Jiwang1,2,*, CHEN Yue1, SONG Guangsen3, XIA Wenshui1,4
2015, 36(12):  264-269.  doi:10.7506/spkx1002-6630-201512050
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The objective of this study was to examine the influence of surfactant on the preservative effect of chitosan-WPInano
TiO2 composite film (CWTF) on vegetables and fruits. The surfactants tween 20 (TW20), TW60, TW80 and TW85
were added to the CWTF film-forming solution, respectively. The tensile strength, elongation at break, transparency and
water permeability of the prepared composite membranes were then detected and the effects of the above surfactants on
CWTF properties were analyzed. Fresh-cut bamboo shoots were coated with CWTF coating solution added with different
surfactants and the weight loss was measured during subsequent storage. Results showed that after adding surfactants,
different levels of deterioration on the smoothness of CWTF surface were observed, and the rank according to film
mechanical properties and water permeability from high to low was as follows: CWTF > CWTF-TW20 > CWTF-TW85 >
CWTF-TW80 > CWTF-TW60. The results of coating experiments showed that weight loss of fresh-cut bamboo shoots with
coating was lower than that of those without coating, and was negatively correlated with membrane properties. TW20 was
selected as the appropriate surfactant and its appropriate dosage was 0.1%.