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Table of Content

25 August 2014, Volume 35 Issue 16
Processing Technology
Separation and Purification of Astaxanth from Antarctic Krill Shells by Macroporous Resin
JIANG Qi-xing1, SONG Su-mei1, XIA Wen-shui1, LIU Fu-jun2, XU Yan-shun1, LIU Dong-mei2, WANG Hai-ou1,*
2014, 35(16):  1-5.  doi:10.7506/spkx1002-6630-201416001
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In the present study, the static and dynamic adsorption capacities of AB-8 macroporous resins for astaxanthin
from Antarctic krill shells were evaluated. The results showed that the maximum quantity of astaxanthin adsorbed was
476.2 μg per gram of dry AB-8. Ethyl acetate was selected as the elution solvent with a desorption rate of 98.7%. The
dynamic adsorption conditions were optimized as 2 μg/mL and 4 BV/h for astaxanthin concentration and flow rate,
respectively. Under the optimal condition, the astaxanthin in saponification solution was purified with recovery rate of
78.9% and purity of 92.4%.

Optimization of the Preparation Process for Soy Protein Isolate-Based Fat Simulant
WANG Jian-hui, JIN Na, CHENG Yuan-yuan, LIU Yong-le*, WANG Fa-xiang, LI Xiang-hong, YU Jian
2014, 35(16):  6-10.  doi:10.7506/spkx1002-6630-201416002
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This study proposes a procedure for preparation of soy protein isolate (SPI)-based fat stimulant with similar
sensory characteristics to oils and fats. The preparation conditions were investigated preliminarily by single-factor design
and optimized by Box-Behnken design (BBD) with the viscosity and emulsion stability of composite system as a function
of SPI concentration, konjac gum concentration, heating temperature, heating time and homogenization time. A composite
system containing 8% SPI and 0.08% konjac gum heated at 79.8 ℃ for 13 min followed by 40 s homogenization was found
to be optimal. The product obtained exhibited a viscosity of 45.94 mPa·s and an emulsion stability of 74.49 min, close to the
quality of commercially available vegetable oils.

Optimization of Extrusion Parameters for Improved Oligomerization of Lentinula edodes Handle Fiber
LIU Ting-ting, DAI Long, WANG Qing-qing, WANG Da-wei*
2014, 35(16):  11-17.  doi:10.7506/spkx1002-6630-201416003
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The oligomerization of Lentinula edodes handle fiber was conducted through single-screw extrusion. Viscosity
method was used to measure the degree of polymerization (DP) and molecular weight (MW) of extruded products. By using
response surface methodology, the oligomerization efficiency of extrude Lentinula edodes handle fiber was investigated
as a function of extrusion temperature, raw material particle size and liquid to solid ratio. The results showed the best
oligomerization efficiency was achieved when the fiber powder with particle size 0.147 mm (100 mesh) was extruded at
162 ℃ with a liquid to solid ratio of 1.43:1. It turned out that the DP dropped from 1 278 to 202, and the MW from 207 054
to 32 742. Scanning electron microscopy (SEM) observation showed the loose and porous structure of the extruded material,
and the original molecular structure was not significantly damaged as indicated by infrared spectroscopy, but a small part of
hemicellulose was degraded. Water-holding capacity, oil-holding capacity and expansive force of oligomerized Lentinula
edodes handle fiber were improved obviously compared with the untreated samples.

Optimizing the Extraction of Protein from Cashew Nuts
ZHONG Jun-zhen, DUN Ru-yan, HUANG Zong-lan, LIU Wei, LIU Cheng-mei*
2014, 35(16):  18-22.  doi:10.7506/spkx1002-6630-201416004
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In the present study, cashew nuts were analyzed for main chemical components. A comparative investigation of
different extraction methods for protein extraction from cashew nuts was made. The extraction process was optimized with
regard to solid-to-liquid (S/L) ratio, solvent pH, extraction temperature and time by single-factor and orthogonal array designs.
The results showed that crude fat was the most abundant component in cashew nuts with a level of 44.13%, which also
contained 22.91% carbonhydrates, 19.41% protein, 3.07% water and 2.45%. The best extraction efficiency was achieved using
alkali extraction and the best experimental conditions were found to be extraction at 35 ℃ for 1.5 h using an extraction solvent
at pH 9 with an S/L ratio of 1:40 (g/mL). Under the optimized conditions, the yield of protein was 79.0% with a purity of
86.62%. SDS-PAGE analysis showed that the major subunits of cashew nuts protein had a molecular mass of 22 and 26.2 kD,
respectively, and 14.1- and 16-kD subunits and a small amount of 67.5- and 88-kD subunits were also observed.

Response Surface Analysis for the Optimization of Extraction Process for Polysaccharides from Tricholoma matsutake and Antioxidant Activity of the Extracted Polysaccharides
CHEN Lian-hong1, YANG Li-zhu2, SUO Hua-yi3, LI Jian4,*
2014, 35(16):  23-28.  doi:10.7506/spkx1002-6630-201416005
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Objective: To develop an optimized enzymatic method for extracting polysaccharides from Tricholoma matsutake
with a combination of cellulase, pectinase and neutral protease and to evaluate the antioxidant activity in vitro of the
extracted polysaccharides. Methods: On the basis of single-factor experiments, a four-factor, three-level Box-Behnken
design was utilized for the mathematical modeling of polysaccharide yield as a function of material/water ratio, medium
pH and hydrolysis time and temperature. This was followed by response surface analysis of the developed mathematical
model. The antioxidant activity of Tricholoma matsutake polysaccharides was determined by pyrogallol autoxidation and
free radical-scavenging assay. Results: The optimum condition for the extraction of Tricholoma matsutake polysaccharides
were found to be hydrolysis at 35 ℃ for 71 min with a material/solvent ratio of 1:40 (g/mL) at pH 5. Under these conditions,
the model-predicted and experimentally measured values of polysaccharide yield were 7.06% and 6.95%, respectively,
revealing a relative error of only 1.56% between them. The Tricholoma matsutake polysaccharides had a strong capacity to
scavenge superoxide anion (IC50 = 0.565 mg/mL) and DPPH free radical (IC50 = 0.454 mg/mL). Conclusion: The proposed
extraction method is efficient, simple and applicable for the extraction of polysaccharides form Tricholoma matsutakes and
the extracted polysaccharides have significant antioxidant capacity in vitro.

Optimization of Extraction Conditions of Heme from Tilapias Blood by Enzymatic Hydrolysis
CEN Jian-wei1, LI Lai-hao1, YANG Xian-qing1, LIU Zai-jun1,2, HAO Shu-xian1, ZHOU Wan-jun1, WEI Ya1
2014, 35(16):  29-33.  doi:10.7506/spkx1002-6630-201416006
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To achieve scientific and effective utilization of tilapias blood as an abundant resource in China, the extraction
conditions of heme from tilapias blood by enzymatic hydrolysis were studied in this paper. Protamex was found as
the best enzyme catalyst for the extraction of heme from tilapias blood. By using single-factor and orthogonal array
designs, the optimum enzymatic hydrolysis conditions were determined as follows: temperature, 40 ℃; pH, 8.0; substrate
concentration, 6 g/100 mL; enzyme/substrate, 8 000 U/g; and hydrolysis time, 2 h. Under these conditions, followed by heat
treatment, acid precipitation and vacuum freeze drying, heme was obtained with a yield of 80.9% and a purity of 28.2%.
This extraction procedure is simple, practical, cost saving and suitable for industrial production of value-added products with
reduced environmental pollution.

Optimization of Spray Drying Process for the Preparation of Maca Fine Powder
ZHANG Wen-wen1, ZHENG Hua1, LI Kun1, ZHANG Hong1,*, XU Juan1, ZHANG Li2
2014, 35(16):  34-38.  doi:10.7506/spkx1002-6630-201416007
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The aim of this study was to develop a maca processing system and provide a reliable method for preparing raw
materials for high-value maca products. For the preparation of maca fine powder, maca tubers were extracted with alcohol,
and the extract was then concentrated by evaporating the ethanol before spray drying. Three operating parameters, viz., feed
concentration, air inlet temperature and airflow rate were investigated. The best spray drying conditions were established by
single-factor and orthogonal array design methods as feed concentration 5%, air inlet temperature 120 ℃ and airflow rate
0.4 m3/min. Under the optimized conditions, the contents of moisture, alkaloid, protein, vitamin C and total sugar of
maca fine powder were 2.12%, 15.87 mg/g, 1.64 mg/g, 6.03 mg/g and 554.50 mg/g, respectively. The ultrastructure and
hygroscopic properties of the maca fine powder showed that the active components of maca were preserved by the optimized
spry-drying process and the final product could be used as an excellent raw materialfor the development of maca products.

Ultrasonic-Assisted Extraction and in vitro Antioxidant Activity of Pigment from Sorghum Flour
Lü Man-man, LIU Hang, MIAO Xiu-gang, XU Fang-yi, LI Wu-xia, WANG Min*
2014, 35(16):  39-45.  doi:10.7506/spkx1002-6630-201416008
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Objective: To explore the optimal ultrasonic-assisted extraction conditions of pigment from sorghum flour and
evaluate the antioxidant activity of the extracted pigment. Methods: Based on the single-factor designs, the ultrasonicassisted
extraction conditions of pigment from sorghum flour were optimized by response surface methodology with Box-
Behnken design in order to increase the extraction yield of pigment. Meanwhile, the in vitro antioxidant activity of pigment
from sorghum flour was also studied. Results: The optimal extraction conditions were 50.76%, 500.64 W and 1:16.72 (g/mL)
for ethanol concentration, ultrasonic power and material/liquid ratio, respectively. Under these conditions, the maximum
predicted extraction yield of pigment was 54.26%. When the ethanol concentration, ultrasonic power and material/liquid
ratio were 51%, 504 W and 1:17 (g/mL), respectively, the experimentally observed extraction yield of pigment was
(53.99 ± 0.26)%. Sorghum pigment showed significant scavenging effects on 1,1-diphenyl-2-picryl-hydrazy (DPPH·) and
hydroxyl free radicals (·OH) and excellent reducing power. Conclusion: Response surface methodology with Box-Behnken
design is applicable for the optimization of the ultrasonic-assisted extraction of pigment from sorghum flour. The pigment
from sorghum flour has strong antioxidant capacity.

Pretreatment and Hot Air Drying of Betel Nuts
LOU Zheng1, LIU Qing1,*, GUO Jing2, SHI Jian-fang1, ZHAO Yu-qiang1, GAO Xue-min1
2014, 35(16):  46-51.  doi:10.7506/spkx1002-6630-201416009
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This study explored the effects of different boiling periods (10, 20 and 30 min) and temperatures (80, 90 and 100 ℃)
for pretreatment as well as different drying temperatures (50, 55, 60 and 65 ℃) and loading weights (16, 24, 32 and 40 kg/m2)
on drying characteristics and length/diameter ratio of betel nuts. The results showed that different boiling periods had no
significant effect on water content, but different boiling temperatures had an obvious effect. The length/diameter ratio of
betel nuts was significantly changed with different boiling periods and boiling temperatures, revealing a decrease with
extended boiling time but an increase with increasing boiling temperature. The optimum pretreatment parameters were
cooking for 10 min at 100 ℃. Both drying time and loading weight had remarkable effects on the moisture content of betel
nuts. The drying rate of betel nuts became higher at elevated drying temperature, but declined with increasing loading
weight. The whole drying process was a falling-rate period. The optimum drying parameters were 60 ℃ and 24 kg/m2 for
drying temperature and loading weight, respectively.

Optimization of Ultrasonic-Assisted Aqueous Enzymatic Extraction and Fatty Acid Composition of Silkworm Pupae Oil
JIA Jun-qiang1,2, WU Qiong-ying1,2, DU Jin-juan1, HE Rong-hai3, GUI Zhong-zheng1,2, YAN Hui1,2
2014, 35(16):  52-57.  doi:10.7506/spkx1002-6630-201416010
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As a new extraction technique, ultrasonic-assisted neutral protease hydrolysis (UANPH) was used to extract oil
from silkworm pupae. On the basis of single factor experiments, effects of ultrasonic power, substrate concentration and
enzyme dosage on the extraction yield of silkworm pupae oil were studied with response surface methodology. In addition,
the fatty acid composition of silkworm pupae oil was analyzed by gas chromatography (GC). The results showed that the
the extraction yield of silkworm pupae oil was affected in decreasing order by substrate concentration, enzyme dosage and
ultrasonic power. The optimized operating parameters were as follows: substrate concentration 68.2 g/L, ultrasonic power
121.6 W and enzyme dosage 2 849.4 U/g. Experiments carried out under the optimal conditions led to an extraction yield
of (90.2 ± 0.66)%. GC analysis showed that composition and contents of fatty acids in silkworm pupae oils by UANPH
extraction and traditional solvent (n-hexane) extraction were in substantial agreement. The silkworm pupae oils were mainly
composed of palmitoleic acid, palmitic acid, linolenic acid, linoleic acid, oleic acid and stearic acid.

Aqueous Enzymatic Extraction and Oxidative Stability of Papaya Seed Oil
YE Li-hong, WANG Biao-shi*, CHENG Yi-ting, HUANG Ri-feng, GUAN Qing-hao, JIANG Min, JIN Bei, DU Jian-zhong
2014, 35(16):  58-63.  doi:10.7506/spkx1002-6630-201416011
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This study was aimed to establish the optimum conditions for the aqueous enzymatic extraction of papaya seed
oil by investigating the effects of enzymes, hydrolysis time, substrate to water ratio, enzyme dosage and temperature on oil
yield by using single-factor and orthogonal array designs. Meanwhile, the effects of temperature, light and antioxidants on
the oxidative stability of papaya seed oil as reflected by its peroxide value were also analyzed. The results showed that the
optimum parameters for extracting papaya seed oil were found to be 5 h of hydrolysis using neutral protease at a dosage of
2.5% with a substrate to water ratio of 1:7 (g/mL) at 45 ℃. Under the optimized conditions, the extraction yield of papaya
seeds oil was 85.73%. Temperature, light and oxygen caused an increase in peroxide value during storage of papaya seed oil
and TBHQ had good antioxidant effect on the oil.

Optimization by Response Surface Methodoloy of Ultrasonic Extraction of Total Flavonoids from Tartary Buckwheat Hull
ZHAO Qiang1,2, SUO You-rui1,*, LI Tian-cai1, ZHAO Hai-fu3, DONG Xiao-ning2
2014, 35(16):  64-70.  doi:10.7506/spkx1002-6630-201416012
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The ultrasonic extraction of total flavonoids from tartary buckwheat hull was optimized by response surface
analysis with Box-Behnken design, and the flavonoid extract obtained was analyzed by high performance liquid
chromatography (HPLC). The results showed that the extraction efficiency of total flavonoids was affected in decreasing
order by ethanol concentration, liquid-to-solid ratio, refluxing time and ultrasonication time, for which the optimal conditions
were 65%, 14:1 (mL/g), 1.6 h and 28 min, respectively. Under the optimized conditions, the yield of total flavonoids was
1.495 20%. The HPLC method used in this study was found to be highly repeatable.

Inhibition of Acrylamide Formation in Dried Bun Slice by Improving Baking Conditions and Adding Food Additives
DOU Kang-ning1, LUO Hai-lan1, PENG Xin-ran2, YANG Shu-zhi3, WANG Fei1,*
2014, 35(16):  71-75.  doi:10.7506/spkx1002-6630-201416013
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This paper presents a way to reduce acrylamide contents in dried bun slice by improving the baking condition
and adding food additives. The results demonstrated that the acrylamide level was reduced by 10.9% by baking at higher
temperature (230 ℃) than at lower temperature (190 ℃). A decrease of 31.7% was observed when the moisture content
in fresh bun was reduced from 41.7% to 9.6%, while the addition of 1.0% calcium sulfate and 0.04% tea polyphenols to
fresh bun led to a decrease of 56.5%. The acrylamide content of dried bun slice was decreased from 177.2 to 46.8 μg/g by
improving the baking condition and simultaneously adding food additives, indicating a reduction of 73.5%. Therefore, the
generation of acrylamide in dried bun slice could be effectively inhibited by high-temperature short-time baking, reduced
moisture content of fresh bun and addition of food additives to fresh bun.

Separation of Total Polyphenols from Akebia trifoliate Peel by Calcium Precipitation Method
OUYANG Yu-zhu, LI Xue-feng, YAO Yi-huan
2014, 35(16):  76-79.  doi:10.7506/spkx1002-6630-201416014
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A calcium precipitation method to separate total polyphenols from a 70% ethanol extract of dried powdered
Akebia trifoliate peel was proposed and optimized by response surface methodology. The yield of total polyphenols was
investigated as a function of precipitator dosage, precipitation temperature and time. The results showed that the optimum
precipitation conditions that provided maximum total polyphenol yield of 5.103 7% were obtained when 50 mL of the extract
was precipitated by adding 90 mL of clear saturated limewater at 70 ℃ for 38 min. There was a good agreement between the
predicted and experimental data for total polyphenol yield. The separated precipitate contained 84.417 4% total polyphenols.

Optimization of Combined Ultrahigh Pressure and Thermal Treatment for Production of Blunt-Snout Bream Sausage with Added Matcha and Analysis of Its Volatile Flavor Compounds
SHANG Xiao-lan, LI Cong-sheng, LU Yan-xia, JIANG Hai-qiang
2014, 35(16):  80-84.  doi:10.7506/spkx1002-6630-201416015
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Ultrahigh pressure and thermal treatment were applied jointly to treat blunt-snout bream sausage with added
matcha to improve its quality. Response surface analysis showed that treatment at 410.52 MPa and 41.07 ℃ for 14.91 min
provided good texture properties. The results of analysis by gas chromatography-mass spectrometry (GC-MS) indicated
that both traditional boiling and the combined ultrahigh pressure and thermal treatment favored the formation of aroma
compounds, while after this combined treatment further boiling gave rise to adverse effects.

Ultrasound-Assisted Extraction and Antioxidant Activity in vitro of Flavonoids from Male Tussah Moth
TIAN Ye, YUE Xi-qing*, YANG Mei
2014, 35(16):  85-90.  doi:10.7506/spkx1002-6630-201416016
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Objective: To investigate the extraction and antioxidant effects of flavonoids from male tussah moth. Methods:
Flavonoids were ultrasonically extracted from male tussah moth with ethanol. The extract was analyzed qualitatively by
UV-visible absorption spectroscopy. The optimum extraction conditions were determined by orthogonal array design.
The antioxidant activity of flavonoids from male tussah moth investigated by comparing the reducing power and radical
scavenging effects against DPPH, hydroxyl and superoxide anion radicals with those of VC and BHT in vitro. Results: The
optimum extraction conditions were as follows: ethanol concentration 60%, solid/solvent ratio 1:40, extraction time 45 min
and temperature 70 ℃. Under the optimized conditions, the yield of total flavonoids from male tussah moth was 3.72 mg/g
in one extraction cycle. The extracted flavonoids had potent radical scavenging activity in a dose-dependent manner against
DPPH, hydroxyl and superoxide anion radicals, and its IC50 was 752.4, 617.8 and 813.4 μg/mL, respectively. The hydroxyl
radical scavenging activity was stronger than that of VC and BHT, and the superoxide anion radical activity was stronger
than that of BHT. Conclusion: Flavonoids from male tussah moth had strong antioxidant effects in vitro.

Optimization of Pulsed Light Parameters for Enhanced Sterilization of E. coli on Pancake Using Response Surface Methodology
TANG Ming-li, WANG Bo, LIU He, HE Yu-tang, HUI Li-juan, MA Tao*
2014, 35(16):  91-95.  doi:10.7506/spkx1002-6630-201416017
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Pulsed light was used for surface sterilization of pancake and the effect of pulsed light parameters on the
logarithmic reduction of E. coli on pancake was explored by response surface methodology on the basis of single factor
experiments. A quadratic polynomial model for the logarithmic reduction of E. coli on pancake as a function of pulsed light
parameters was established to analyze the effects of pulse energy, number and distance, and their pairwise interactions.
E. coli on the surface of pancake could be effectively killed by using pulsed light. The pulsed light conditions were
optimized as follows: pulse energy 500 J, pulse number 40, and pulse distance 10.9 cm. Under these conditions, pulsed light
resulted in a reduction of 2.15 logarithmic units for E. coli on pancake, which in turn prolonged the shelf life and improved
the microbiological safety.

Change in Aroma Composition of “Yujinxiang” Melon during Storage at Ambient Temperature
ZHANG Na, JIANG Yu-mei*, LI Ji-xin, XU Tao
2014, 35(16):  96-100.  doi:10.7506/spkx1002-6630-201416018
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The dynamic change in the aroma composition of “Yujinxiang” melon (Cucumis melo L.) during ambient
temperature storage was analyzed by headspace solid phase micro-extraction (HS-SPME) combined with gas
chromatography-mass spectrometry (GC-MS). The results showed that 71 aroma components were identified, including
29 esters, 15 aldehydes and ketones, and 12 alcohols. Alcohols and aldehydes were the major aroma components during
the early storage period with a relative total amount of 41.9%. Among these aroma components, n-hexanal, cis-3-hexenol,
2-hexenal, (E,Z)-2,6-nonadienal, (E,Z)-3,6-nonyl dien-1-ol and (Z)-6-nonenal, mainly responsible for the delicate aroma
of the fruit, were relatively more abundant. The relative quantity of esters increased with extended storage duration and
became major aroma components. Among them, the relative quantities of ethyl acetate and acetic acid benzyl ester, which
contributed to fruity aroma, significantly increased. The relative total quantity of esters increased to 91.57% on the tenth day
of storage as major aroma components. To conclude, the volatile aroma compound composition of “Yujinxiang” melon is
significant different at different storage stages.

Analysis & Detection
Development of SPE-HPLC Method for Determination of Dehydrogenated Abietic Acid Residue in Duck Skin Tissue
ZHANG Su-zhen1,2, GENG Zhi-ming2,*, WANG Dao-ying2, ZHU Yong-zhi2, LIU Fang2, ZHANG Mu-han2, BIAN Huan2, XU Wei-min2
2014, 35(16):  101-104.  doi:10.7506/spkx1002-6630-201416019
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A high-performance liquid chromatographic (HPLC) method was established to determine dehydrogenated abietic
acid in duck skin. Dehydrogenated abietic acid in duck skin sample was extracted with acetonitrile, followed by purification
with a C18 solid-phase extraction (SPE) cartridge, and detected by HPLC-ultraviolet detector (UV). The chromatographic
conditions were as follows: column, reversed-phase C18 (250 mm × 4.6 mm, 5 μm); mobile phase, a mixture of 0.003 mol/L
phosphoric acid-methanol (13:87, V/V); flow rate, 1.0 mL/min; and detection wavelength, 212 nm. Results indicated that
the linearity ranged from 0.1 to 10.0 mg/L, and the detection limit and the quantification limit were 0.10 μg/g and 0.33 μg/g,
respectively. The recoveries of dehydrogenated abietic acid spiked at 0.5–20 μg/g were in the range of 80.8%–91.8%. The
method was successfully applied for the determination of dehydrogenated abietic acid in rosin-defeathered duck skin, and
the result indicated that content of dehydrogenated abietic acid in the duck sample could reach 10.06 μg/g. The present
method proved to be of high maneuverability and excellent sensitivity and accuracy, and could be employed to analyze
dehydrogenated abietic acid residue in duck skin tissue.

Rapid Identification of Bolete Mushrooms by UV Spectroscopy Combined with Euclidean Distance and Principal Component Analysis
YANG Tian-wei1, LI Tao2, ZHANG Ji3, LI Jie-qing1, LIU Hong-gao1, WANG Yuan-zhong3,*
2014, 35(16):  105-109.  doi:10.7506/spkx1002-6630-201416020
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In this study, an ultraviolet (UV) spectroscopic method was established for rapid identification of different species
of bolete mushrooms from different areas. For preparation of boletes extracts, the optimal extraction extraction solvent,
sample amount and extraction time were determined as 0.5 mol/L NaOH, 0.100 0 g and 40 min, respectively. The similarity
of UV spectral fingerprint of bolete samples was analyzed by included angle cosine (IAC), Euclidean distance (ED) and
principal component analysis (PCA). The results showed that, within 10 h, the RSDs of stability, repeatability and accuracy
for bolete extracts were 0.06%–2.33%, 0.09%–1.81% and 0.11%–1.92%, respectively. The difference of IAC values among
samples was small, ranging from 0.823 to 0.999. But the difference of ED values among samples was large, ranging from
31.36 to 873.17. PCA showed that the cumulative contribution rate of the first three factors was 93.626%, which could
reflect most information about the samples. These findings suggested that the ED and PCA methods can be used for rapid
identification and quality control of different specices of boletes from different areas.

Determination of Chloramphenicol, Thiamphenicol and Florfenicol Residues in Feed, Raw Milk and Dairy Products by UPLC-MS-MS
HU Xue, LI Cui-zhi*, LIU Li-jun, KANG Kai, BAI Yan-mei, DUAN Guo-xia, ZHANG Li-jia
2014, 35(16):  110-113.  doi:10.7506/spkx1002-6630-201416021
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An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS) method for
simultaneous determination of chloramphenicol, thiamphenicol and florfenicol residues in feed, raw milk and dairy products
was developed. The extraction procedures and the UPLC-MS-MS conditions for feed, raw milk, liquid milk, fermented milk,
milk drinks, milk powder, milk tablet and frozen drinks were studied. After protein in samples was precipitated by cooling
down, the compounds were extracted into acetonitrile, which was separated into layers in the presence of added saturated
sodium chloride. The supernatant was dried under nitrogen, and then re-dissolved before the removal of fat by addition of
n-hexane. The compounds were analyzed in a negative electrospray ion multiple reaction monitoring mode with a mobile
phase composed of acetonitrile and water by means of gradient elution. The limit of quantification (LOQ) was 0.1 μg/kg
for chloramphenicol, thiamphenicol and florfenicol. The matrix effects, recovery rates, and relative standard deviation
(RSD) were 57.9%–139.2%, 64.3%–120.2% and 2.1%–10.0%, at fortification levels of 0.1–2.5 μg/kg for chloramphenicol,
thiamphenicol and florfenicol, respectively. This method is simple, convenient, fast and suitable for the quantification and
confirmation of chloramphenicol, thiamphenicol, and florfenicol in feed, milk and dairy products.

Extraction and Analysis of Volatile Components of Tangerine Peel
GAO Ting-ting, YANG Shao-xiang*, LIU Yu-ping, SUN Bao-guo
2014, 35(16):  114-119.  doi:10.7506/spkx1002-6630-201416022
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The volatile components of tangerine peel were extracted by either head-space solid-phase micro-extraction
(HS-SPME) or simultaneous distillation extraction (SDE) and analyzed by gas chromatography-mass spectrometry (GCMS).
Eighty-nine volatile constituents were identified, including 44 alkenes, 10 alcohols, 10 aldehydes, 8 phenols, 7 esters,
4 ketones and 6 other components. Thirty-four components were identified by both extraction methods. D-Limonene,
γ-terpinene, 2-thujene, α-farnesene, p-cymene and α-pinene made greater contributions to the odor characteristics of
tangerine peel.

Analysis of the Volatile Components in Polyphenol Compounds Extracted from Dendrocalamus latiflorus Shoots
REN Wang1, YE Xiu-juan1, LI Ting-ting1, ZHENG Jiong1,2,*
2014, 35(16):  120-123.  doi:10.7506/spkx1002-6630-201416023
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This research was focus on the extraction of polyphenol compounds from Dendrocalamus latiflorus shoots with
four different solvents, and the volatile compounds in polyphenol extracts were identified and quantitatively evaluated
by GC-MS. The results showed that total phenol contents in methanol, ethanol, acetone, and ethyl acetate extracts were
4.94, 4.85, 4.47 and 2.22 mg/g, respectively. Totally 24 volatile compounds were identified from the four polyphenol
extracts. Among them, the most abundant compounds were 4-hydroxybenzaldehyde, 4-hydroxybenzyl cyanide, acetic acid,
1,2,3,5-cyclohexanetetrol, 2,3-dihydro-3,5-dihydroxy-6-methyl-4-pyran and pyruvic alcohol. The major volatile phenols in
the extracts were pyrocatechol and 3-methylcatechol.

Isolation, Purification and Detection of Anthraquinone Compounds from the Root of Actinidia arguta Sieb. et Zucc.
YANG Yu-hong1,2, LI Xin3, YANG Jian2, LIU Chang-jiang3, KANG Zong-li2,*
2014, 35(16):  124-127.  doi:10.7506/spkx1002-6630-201416024
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Anthraquinones from the root of Actinidia arguta Sieb. et Zucc. were isolated and purified by polyamide column
chromatography and silica gel column chromatography and were determined by high performance liquid chromatography
(HPLC). The results showed that the optimum silica gel column chromatographic conditions were selected as 200 mesh silica
gel, column dimensions φ 1.1 cm × 100 cm, flow rate 1.5 mL/min and mobile phase composed of a mixture of methanol
and water (90:10, V/V). The detection wavelength for anthraquinones was 254 nm. Emodin and chrysophanol as the major
anthraquinones were detected in the root of Actinidia arguta Sieb. et Zucc. at levels of 46 and 157.5 μg/g, respectively.

Headspace Solid Phase Microextraction for Analysis of Volatile Components in Chinese Steamed Bread Made with Four Starter Cultures
MA Kai1, HUA Wei2, GONG Ping1, CHEN Er-ning2, BAI Yu2, LIU Jie2, WANG Yan-sheng3, LI Tai-hua3, GAO Li-juan2,*
2014, 35(16):  128-132.  doi:10.7506/spkx1002-6630-201416025
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In this work, the composition of volatile components in Chinese steamed bread fermented with traditional mixed
starters (QJ and ZZ) and commercial dry yeast starters (AQ and YS) was determined by headspace-solid phase microextraction
(HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS). According to the NIST 08.L MS spectral
library and reference data, 59, 51, 47 and 43 volatile compounds in Chinese steamed bread fermented with QJ, ZZ, AQ and
YS were identified, respectively. These volatile components included alcohols, hydrocarbons, esters, aldehydes, ketones, aromatics
and other compounds. The results showed fermentation with the traditional mixed starters could result in the production of more
components in different relative quantities in Chinese steamed bread than the dry yeast starters. This may be the main reason why
Chinese steamed bread fermented with the same wheat flour and different starters have distinct volatile components.

Analysis of Lipid and Fatty Acid Composition in Different Tissues of Adult Female and Male Takifugu flavidus
XU Jia-bo, SHI Yong-hai*, ZHANG Gen-yu, LIU Yong-shi, ZHANG Hai-ming, LU Gen-hai, DENG Ping-ping, ZHANG Zong-feng
2014, 35(16):  133-137.  doi:10.7506/spkx1002-6630-201416026
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In this paper, the moisture content, lipid contents, and fatty acid composition of liver, gonad, muscle, and derma
from adult Takifugu flavidus were investigated. The male was in stage Ⅲ of ovary development, and the female was in
stage Ⅳ of spermary development. The results indicated that there was a significant difference in moisture content among
different tissues (P < 0.05). For the female, the highest moisture content was observed in muscle and the lowest moisture
content in liver; for the male, the highest moisture content was observed in spermary and the lowest moisture content in
liver. Meanwhile, the total lipid contents in liver, gonad, muscle, and derma of the female were (48.87 ± 7.75)%, (11.77 ±
1.44)%, (0.50 ± 0.00)%, and (0.13 ± 0.06)%, respectively. The total lipid contents in liver, gonad, muscle, and derma
of the male were (63.13 ± 3.07)%, (1.70 ± 0.10)%, (0.43 ± 0.12)%, and (0.30 ± 0.20)%, respectively. There was a
significant difference in total lipid content among different tissues for the female and male (P < 0.05), and the highest lipid
content was detected in liver, followed by gonad, and the lowest lipid content in derma. In addition, the highest relative
contents of saturated fatty acids (SFA) were shown in muscle for the female and male. The relative content of C16:0 in muscle
was significant higher than in liver, ovary, and derma. Monounsaturated fatty acids (MUFA) as the most abundant fatty
acids in liver were (46.4 ± 0.5)% and (45.7 ± 0.9)% in the female and male, respectively, higher than in gonad, muscle
and derma. The most abundant fatty acids in gonad were polyunsaturated fatty acids (PUFA) at levels of (28.6 ± 1.4)%
and (33.8 ± 1.9)% in the female and male, respectively. The relative content of ΣPUFA in ovary was significantly higher
than in liver and muscle (P < 0.05), while no significant difference was found between ovary and derma (P > 0.05). The
relative content of ΣPUFA in spermary was significantly higher than in liver, muscle, and derma (P < 0.05). The absolute
content of fatty acids in liver was 8.75% and 10.57% in the female and male, respectively, significantly higher than in gonad, muscle, and derma (P < 0.05). This research shows that Takifugu flavidus is nutritional and delicious. The liver can
be used for the development of fish oil. The liver is rich in PUFA, which can provide the basic material for the development
of cardiovascular drugs.

Determination of Free Fatty Acids in Goat Milk by Gas Chromatography without Derivatization
YAN Hui-li1, ZHANG Fu-xin1,*, LI Yan-hua2, JIA Run-fang1, LI Long-zhu1, AI Dui1, YANG Ji-ni1
2014, 35(16):  138-142.  doi:10.7506/spkx1002-6630-201416027
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A method was developed for the determination of free fatty acids (FFAs) in goat milk by gas chromatography (GC)
without derivatization. The process includes three parts: the extraction of goat milk lipids, the separation of FFAs and the
determination by gas chromatography. Firstly, the milk lipids were extracted with ethanol/ether/n-heptane, and then FFAs
were isolated on an aminopropyl column. Finally, the FFAs were identified and determined by gas chromatography. The
external standard method was applied to determine the recoveries of FFAs in the goat milk, which acted as the calibration
coefficients of FFAs. The results showed that the recoveries of long chain FFAs were higher than those of short chain FFAs,
especially for C2︰0 and C4︰0 with values of 23.9% and 78.5%, respectively. The recoveries were stable with relative standard
deviations blew 0.04%.

Analysis of Free Amino Acids in Flower Buds of Hemerocallis Genus Plants by RP-HPLC
YANG Li1,2, LI Xiao-dong2, LIU Shu-ying1, SUN Guo-feng2, LIN Qin-wen2, LIU Hong-zhang1,*, ZHANG Jin-zheng2
2014, 35(16):  143-147.  doi:10.7506/spkx1002-6630-201416028
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Objective: To analyze the composition of free amino acids in flower buds of plants from 8 wild species and 25
cultivated species of the genus Hemerocallis. Methods: A high performance liquid chromatography (HPLC) method to
determine free amino acids in flower buds of Hemerocallis genus plants was proposed using on-line precolumn derivatization
with o-phthalaldehyde. Comprehensive evaluation of these Hemerocallis species based on free amino acid composition was
performed by principal component analysis. Results: The results showed that the total amount of free amino acids varied
from 6.864 to 21.219 mg/g in flower buds of the 33 Hemerocallis species tested;14–16 kinds of free amino acids were
detected and their contents differed among different Hemerocallis species. All the investigated samples were richest in
asparagine, glycine, serine and glutamic acid among the flavor amino acids identified. Based on comprehensive evaluation
index, the edible species of Hemerocallis, Hemerocallis citrine, Hemerocallis minor, Hemerocallis lilioasphodelus and
Hemerocallis bearing white flowers, had the best quality followed by Hemerocallis ‘Stella Deoro’ and Hemerocallis ‘First
Spring’, whereas Hemerocallis ‘Xinkou’ and Hemerocallis ‘Yinguangfurong’ showed the poorest quality.

Rapid Screening for Gutter Oil Adulteration in Vegetable Oil Based on Fatty Acid Methyl Esters
ZHAO Hai-xiang1, REN He-ling2, XU Xiu-li2, ZHANG Feng-xia2, DING Gang-dou2, YUE Fen-peng2, MA Xiao-ning2, ZHONG Wei-ke2,*
2014, 35(16):  148-152.  doi:10.7506/spkx1002-6630-201416029
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A rapid screening method for adulteration of gutter oil in vegetable oils based on different forms of fatty acid
esters detected in samples was developed. The major forms of fatty acids were triglycerides in vegetable oils and fatty acid
methyl esters (FAMEs) in gutter oil. Using gas chromatography-mass spectrometry (GC-MS) in a full-scanning detection
mode, 37 kinds of fatty acid methyl esters were determined by searching against the NIST 05 standard mass spectral library.
The fatty acid methyl esters of samples were determined by direct dilution with n-hexane and GC-MS with full-scanning
analysis. Fatty acid methyl esters were not detected in 100 vegetable oil samples. Meanwhile, 14 kinds of fatty acid methyl
esters were detected in 13 (65%) out of 20 gutter oil samples, mainly including methyl myristate (C14∶0), methyl palmitate
(C16∶0) and methyl stearate (C18∶0). In addition, 70% of the 13 gutter samples were detected to simultaneously contain many
kinds of fatty acid methyl esters at higher levels. Thus, vegetable oil sample detected to contain more fatty acid methyl esters
at higher contents can be confirmed to be adulterated with gutter oil. In the case of lower or undetectable levels of fatty acid
methyl esters, other indicators or methods are needed. In conclusion, fatty acid methyl esters can be used an indicator for
rapid screening for gutter oil adulteration in vegetable oils.

Determination of Nitrofuran Metabolite Residues in Aquatic Fingerlings by High Performance Liquid Chromatography-Mass Spectrometry with Dispersive Solid Phase Extraction
YAN Zhong-yong1,2, ZHANG Xiao-jun1,2,*, MEI Guang-ming1,2, LI Pei-pei1,2, LONG Ju1,2, ZHU Yin1,2, WANG Jian3
2014, 35(16):  153-159.  doi:10.7506/spkx1002-6630-201416030
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A method has been developed for the determination of four metabolites of nitrofuran, i.e. semicarbazide (SEM),
3-amino-5-morpholinomethyl-2-oxazolidineone (AMOZ), 3-amino-2-oxazolidinone (AOZ) and 1-aminohydantoin
hydrochloride (AHD) in aquatic fingerlings, by high performance liquid chromatography-mass spectrometry with dispersive
solid phase extraction. Samples were washed with a mixture of methanol-water (8:1, V/V), subjected to HCl acidolysis and
derivatized using 2-nitrobenzaldehyde. The derivative was extracted with ethyl acetate, then concentrated and cleaned up by
dispersive solid phase extraction. The analysis was carried out in the multi-reaction monitoring (MRM) mode and internal
standard isotope dilution method was used for quantification. Good linearity was obtained in the correlations between the
peak areas and concentrations of the four metabolites of nitrofuran antibiotics over the concentration range from 0.5 to
20.0 μg/L, with correlation coefficients above 0.997. The limits of detection (LODs) for the four compounds were all 0.1 μg/kg.
The range of average recoveries was between 90.5% and 104.5%, with relative standard deviations (RSDs) between 1.56%
and 8.08%. The efficient and simple method could be used to identify and quantify the metabolites of nitrofuran antibiotics
in aquatic fingerlings with satisfactory sensitivity and repeatability.

Quality Analysis of Flax Lecithin Based on High Performance Thin Layer Chromatography
GUZAILINUER·Aerken, LIU Ran, HOU Jun-feng, AISANJIANG·Aihaiti, GUAN Ming*
2014, 35(16):  160-164.  doi:10.7506/spkx1002-6630-201416031
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Objective: To establish a method for the quality analysis of lecithin extracted from flax by high performance
thin layer chromatography (HPTLC). Methods: Test samples of lecithin and phosphatidylcholine standard were dissolved
separately in chloroform-methanol (3:2, V/V) before analysis by HPTLC. The developing system consisted of chloroform,
methanol and water (65:25:4, V/V). The effects of chromogenic agents, developing systems, amounts of spotted sample,
thin layer chromatography plates, temperature and relative humidity on the separation of each component in sample were
investigated. Under the best chromatography condition, the lecithin in the sample and the standard were developed, and
the peak area of phosphatidylcholine was scanned. A standard curve was established and phosphatidylcholine in sample
was quantified by an external standard method. Results: The separation of each component in sample was suitable for
qualitative analysis. The average content of phosphatidylcholine in lecithin sample was 63.33% with plate-to-plate and
within-plate precision (relative standard deviation, RSD) of 1.82% and 3.73%, respectively, and stability (RSD) of 1.60%,
and the average recovery was 98.5%. Conclusion: The method is rapid, accurate and reproducible, which can provide a new
technical reference for the quality analysis of lecithin.

Determination of Bisphenol A in Paper Food Containers by Ultra Performance Liquid Chromatography and Tandem Mass Spectrometry
MA Xiao-fei1, SONG Wei2, LIANG Tian-zuo1, JIA Zhen-guo1, ZHANG Yan1,*
2014, 35(16):  165-169.  doi:10.7506/spkx1002-6630-201416032
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A method for the determination of bisphenol A in paper food containers by ultra performance liquid
chromatography and tandem mass spectrometry (UPLC-MS-MS) after microwave-assisted extraction was developed.
Sample extracts were purification on a Sep-Pak C18 column. The target compound was separated on a Kinetex C18 (2.1 mm ×
100 mm, 2.6 μm) column using methanol-water (containing 0.05% ammonia water) as the mobile phase with gradient
elution, and detected by MS with electrospray ionization (ESI) under a multiple reaction-monitoring mode. In the range of
1.0 to 100.0 μg/L, the calibration curve developed showed good linearity with correlation coefficients (r²) of 0.999 7. The
recoveries for spiked samples were 90.5%–98.6% at three levels of 5, 10 and 50 μg/kg, and the relative standard deviations
were less than 5.6%. The limit of detection was 2.5 μg/kg. The method proved to be easy to use, timesaving, sensitive and
suitable for the determination of bisphenol A residues in food paper containers.

Mineral Contents and Leaching Characteristics in Green Tea from Hanzhong, Shaanxi
DANG Ya1,2, LIU Shui-ying1
2014, 35(16):  170-174.  doi:10.7506/spkx1002-6630-201416033
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The contents of six mineral elements including Mn, Zn, Fe, Cu, Ni and Cr in the digested solutions and infusions
of seven kinds of green tea from the main tea-growing region of Hanzhong, Shaanxi province were determined by atomic
absorption spectroscopy (AAS). The quality evaluation of green tea from Hanzhong was carried out with respect to mineral
contents and leaching rates. The recoveries for six metal elements were between 92.70% and 102.55% with relative standard
deviations less than 10%. The results showed that AAS enabled simple, rapid and accurate determination of mineral contents
in green tea and its infusion. Based on the mineral contents and leaching rates, the quality of organic zinc and seleniumenriched
tea, Pengxiang tea powder, Hangzhong Xianhao and Hanzhong green tea was better than that of other green tea
samples tested.

Changes in Volatile Flavor Compounds in Sufu during Fermentation
LU Jing, LIU Ping, ZHANG Li-zhu, CHE Zhen-ming*
2014, 35(16):  175-179.  doi:10.7506/spkx1002-6630-201416034
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Volatile compounds in samples collected at different stages during the fermentation of sufu were extracted and
analyzed by solid phase micro-extraction (SPME) combined with gas chromatography-mass spectrometry (GC-MS). The
results showed that 110 volatile compounds were isolated and identified, which included 41 esters, 19 aldehydes, 12 ketones,
12 alcohols, 9 acids, 9 hydrocarbons and 8 other compounds. Volatile composition differed significantly across various
processing stages. More volatile compounds were detected as the fermentation proceeded. The relative contents of aldehydes
were decreased significantly after Mucor fermentation, whereas the relative contents and kinds of esters and alcohols were
increased. As the post-fermentation proceeded, the relative contents of aldehydes, acids and esters were increased gradually.
Among these volatile compounds, caproaldehyde, 2-phenylethanale, nonanal, dipentene, ethyl caproate, ethyl phenylacetate,
ethyl valerate, ethyl octanoate, 2-amylfuran and allyl methyl disulphide had an important contribution to the flavor of sufu
during the fermentation process.

Analysis of Volatile Components of Pixian Broad-Bean Sauce with Different Post-Ripening Fermentation Times
LI Zhi-hua1,2, HUANG Chi2, WANG Zi-peng2, YAO Ying-zheng2, DONG Ling2, LI Pu2, XIE Jiang2, CHEN Fu-sheng1,*
2014, 35(16):  180-184.  doi:10.7506/spkx1002-6630-201416035
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In this study, the volatile compounds in three different post-ripening fermented Pixian broad-bean sauces were
analyzed with an electronic nose and headspace solid-phase microextraction (HS-SPME) coupled to gas chromatographymass
spectrometry (GC-MS). Differences were observed by applying principal component analysis (PCA) to electronic nose
data sets. The three samples showed apparent groupings and the best combination of sensors was S1S4S7S10. A total of 44
volatile components were identified by HS-SPME-GC-MS. Nineteen volatile compounds were common to the three samples
mainly including 4-ethyl-2-methoxy-phenol, phenylethyl alcohol, 2-ethyl-phenol, benzaldehyde, benzeneacetaldehyde,
2-hydroxy-methyl benzoic acid ester, 1-heptanol, and the one, two, three-year post-ripening fermented samples were
identified to contain 36, 30, and 28 volatile compounds which accounted for 81.8%, 68.2%, and 63.6% of the total volatile
compounds, respectively. Sensory analysis showed that the 1-year post-ripening fermented sample was different in color,
aroma, and other aspects from the 2 and 3-year fermented samples, which, however, were not obviously different as a whole.

Analysis of Components and Flavor Substances during Guizhou Bacon Processing
ZHU Jian-jun1,2, WANG Xiao-yu1, HU Ping1,2,*, SONG Zhu-yu1,2
2014, 35(16):  185-189.  doi:10.7506/spkx1002-6630-201416036
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The changes in components and flavor substances were studied during Guizhou bacon processing in this paper.
Results showed a decrease in water content from 70.75% to 45.06%, an increase in acid value from 0.84 mg KOH/g to
2.31 mg KOH/g and in peroxide value from 0.48 meq/kg to 2.00 meq/kg, and a reduction in pH from 6.03 to 5.80 due to fat
hydrolysis and the production of small fatty acids. Non-protein nitrogen and volatile basic nitrogen contents tended to rise;
total free amino acid content increased from 441.55 mg/100 g to 1 060.79 mg/100 g, with semi-cystine showing the largest
increase (112.17 mg/100 g), followed by alanine (94.79 mg/100 g), leucine (94.15 mg/100 g), glutamic acid (89.67 mg/100 g)
and phenylalanine (60.68 mg/100 g). In Guizhou bacon, 55 volatile flavor compounds were obtained throughout the whole
production process, and major flavor compounds were phenols, carbonyls, esters alcohols and hydrocarbons.

Simultaneous Screening for 14 Mycotoxin Contaminants in Foods by QuEChERS-LC-MS-MS
SHI Na1,2, HOU Cai-yun1,*, LU Yong2, JIANG Jie2, ZHANG Xue-liang3
2014, 35(16):  190-196.  doi:10.7506/spkx1002-6630-201416037
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This paper presents a QuEChERS-liquid chromatography-tandem mass chromatography (LC-MS-MS) method
for the simultaneous screening for 14 mycotoxin contaminants (deoxynivalenol, penicillic acid, aflatoxin M1, aflatoxin G2,
citrinin, aflatoxin B1, aflatoxin B2, aflatoxin G1, zearalenone, ochratoxin A, sterigmatocystin, HT-2 toxin, T-2 toxin and
podophyllotoxin) in foods. The homogenized samples were extracted with 1% acetic acid in acetonitrile. The separation
was performed on an ACQUITU UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm) by gradient elution after purification
by dispersive-solid-phase extraction (d-SPE). The 14 mycotoxin contaminants in foods analyzed by LC-MS-MS-ESI in
the positive ionization, multiple-reaction monitoring (MRM) mode. The minimum detection limit was 0.5–1 μg/kg. The
developed method proved to be simple, rapid, highly selective and sensitive, and suitable for the analysis of mycotoxin
contaminants in food safety incidents.

Analysis of Volatile Components in Hot Pepper Juice during Fermentation
TANG Xin1,2, XIA Yan-bin1,2,*, WU Can1
2014, 35(16):  197-201.  doi:10.7506/spkx1002-6630-201416038
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Solid-phase micro-extraction (SPME) and gas chromatography-mass spectrometry (GC-MS) were adopted to separate and identify the volatile components of fermented hot pepper juice. The quantification was performed by area normalization method. The results indicated that 106 volatile components were identified including esters, acids, alcohols, olefins, alkenes, aldehydes and ketones. Totally 65, 78, 83 and 86 volatile components were identified in hot pepper juices fermented for 0, 1, 2 and 3 days, respectively. Fifty-three volatile compounds were common to the four samples. The amounts of alkenes and esters were increased as the fermentation process progressed, terpeniods were newly detected, and there was an increase in the number of volatile compounds. The 3 d fermented juice had the best flavor. Therefore, fermentation can improve the flavor of hot pepper juice, and even produce unique flavor, indicating its application potential. Key words: fermented hot pepper juice; volatile component; solid-phase micro-extraction (SPME); gas chromatographymass spectrometry (GC-MS)

Analysis of Aroma Composition of Purple Sweet Potato and Rice Wine Fermented With Different Yeast Starters
LI Ji-tao, JIANG Yi-ming, SHU Jun-xia, CHENG Li-ping, YANG Meng-hua, JIANG He-ti*
2014, 35(16):  202-207.  doi:10.7506/spkx1002-6630-201416039
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This study analyze the aroma components of purple sweet potato and rice wine fermented with three different
yeast starters, alcohol active dry yeast and Saccharomyces cerevisiae 1383 and 1596. The analysis was carried out using
automatic static headspace-solid phase micro-extraction-gas chromatography-mass spectrometry. Moreover, the effect
of mass ratio between purple sweet potato pulp and sacchrified sticky rice pulp on wine quality was studied. The results
showed that the best mass ratio between purple sweet potato pulp and sacchrified sticky rice pulp was in the range of
3:2–1:1; the aroma of purple sweet potato and rice wine was composed mainly of esters, alcohols, aldehydes, ketones, and
alkyl vinyl. Totally 73 aroma components were identified, including 55, 54 and 55 components individually observed in the
wines fermented with alcohol active dry yeast, and Saccharomyces cerevisiae 1383 and 1596, respectively, and 38 aroma
components were common to the three wines. The most predominant aroma compound in these three wines was pentanol
with relative contents of 17.67%, 17.84% and 18.63%, respectively.

Direct Determination of Vitamin C by Ultra Performance Convergence Chromatography
LIU Qian-qian1, ZHOU Wei1,2,3,*, WANG Bo2, WANG Li-ting3, YANG Sheng-xin3
2014, 35(16):  208-211.  doi:10.7506/spkx1002-6630-201416040
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A new method was developed for the determination of vitamin C in foods by ultra performance convergence
chromatography (UPC2). The mobile phase was a mixture of supercritical CO2 and methanol (containing 0.05% H3PO4) at a
flow rate of 0.6 mL/min. A Waters CSH Fluoro-Phenyl column (3.0 mm × 100 mm, 1.7 μm) was used, and the UV detector
was set at 245 nm. The limit of detection (LOD) was 1.5 mg/kg, and the calibration linear range was between 5 and 200 mg/L.
The spiked recoveries of vitamin C were 96.05%–101.15%, with relative standard deviation (RSD) ranging from 0.52% to
0.76%. The method is efficient, rapid, simple, sensitive, accurate, repeatable and low-cost with a low limit of detection. It
can be applied for the determination of vitamin C in foods.

Quantitative Analysis of Fatty Acids and Water in Vegetable Oils by Nuclear Magnetic Resonance
LI Tian-bao, WU Yue, LUO Jing
2014, 35(16):  212-216.  doi:10.7506/spkx1002-6630-201416041
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The main characteristic peaks of linolenic, linoleic, oleic acid, saturated fatty acids and water in vegetable oils
were analyzed by 1H-NMR spectroscopy. Benzoic acid was selected as an internal standard to quantify the contents of
linolenic, linoleic, oleic acid, saturated fatty acids and water in vegetable oils by this method without any pretreatment. The
recoveries were 98%–102% with RSD of 0.11%, 0.12%, 0.68%, 0.70% and 2.65% for linolenic, linoleic, oleic acid, total
saturated fatty acids and water, respectively. The contents of linolenic, linoleic, oleic acid, total saturated fatty acids and
water can be determined directly and accurately with less sample consumption and without using expensive standards. This
new method is simple and applicable for studying quality standards for vegetable oils.

Simultaneous Determination of Veterinary Drug Residues in Aquatic Products by Liquid Chromatography-Tandem Mass Spectrometry (LC-MS-MS)
LI Zhong-chao1,2
2014, 35(16):  217-221.  doi:10.7506/spkx1002-6630-201416042
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A method for the simultaneous determination of 78 veterinary drugs in aquatic products (fish, shrimp and
shellfish) was established using liquid chromatography tandem mass spectrometry (LC-MS-MS). Effects of experimental
conditions such as extraction solvents and Na2EDTA adding on extraction efficiency were investigated. Under the optimized
conditions, recoveries of 78 target drugs calculated from matrix match calibration curve at spiked level of 4 and 20 μg/kg
were 40.8%–125.6% for fish, 42.9%–131.9% for shrimp and 43.5%–136.4% for shellfish with RSD (n = 4) of 0.1%–16.0%,
0.1%–14.0% and 0.3%–15.8%, respectively. The detection limits drugs ranged from 0.1 to 0.5 μg/kg. The method is
sensitive, accurate and fast and can be successfully applied in the analysis of residual veterinary drugs in shrimp samples
from the aquatic farming areas of Zhangzhou, Fujian province.

Uncertainty Evaluation for the Determination of n-Hexane Evaporation Residues of Silicone Rubber Seals Contacting with Foodstuffs
DU Run-feng, ZHU Wen-liang, LU Shan
2014, 35(16):  222-226.  doi:10.7506/spkx1002-6630-201416043
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n-Hexane evaporation residue refers to the total amount of chemical potentially released when an analog sample is
in contact with oil. According to the Chinese national standard GB 4806.1—1994 Food Hygiene Standards Rubber Products,
two analytical methods, area and mass methods were used to analyze the uncertainty in the determination of n-hexane
evaporation residues of silicone rubber seals in pressure cookers and establish an appropriate mathematical model. By
analyzing the various sources of uncertainty and calculating the uncertainty components, the amount of n-hexane evaporation
residue of silicone rubber seals was 375.8 mg/L with relative standard uncertainty of 4.138 8 mg/L and expanded uncertainty
of 8.267 6 mg/L (k = 2) when the mass method was used, while the amount of n-hexane evaporation residue of silicone
rubber seals was 497.15 mg/L with relative standard uncertainty of 6.164 7 mg/L and expansion uncertainty of 12.329 4 mg/L
(k = 2) when the area method was used. In conclusion, the area method is closer to practical applications and helpful for
enterprises to conduct internal quality control. Therefore, we recommend that the area method should be applied with priority
to test n-hexane evaporation residues of silicone rubber seals.

Packaging & Storage
Induction of Disease Resistances in Loquat Fruit by Postharvest Hot Air Treatment
WANG Hua-dong, WANG Hui-qian, ZHENG Cong, WANG Jing, ZHENG Yong-hua*
2014, 35(16):  227-231.  doi:10.7506/spkx1002-6630-201416044
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The effects of hot air treatment on fruit decay and the activities and gene expression of defense-related enzymes in
postharvest loquat fruit were investigated. Freshly harvested loquat fruits were treated with hot air at 43 ℃ for 3 h, challenged
by being inoculated with Colletotrichum acutatum, and then stored at 20 ℃ for 8 d. The results showed that the fruit treated
with hot air had significantly lower natural disease incidence and smaller lesion diameter than the control fruit did. The hot air
treatment remarkably enhanced the activities of phenylalanine ammonia-lyase (PAL), chitinase, β-1,3-glucanase and polyphenol
oxidase(PPO). This hot air treatment also induced the expression of defense-related genes encoding PAL, PPO, peroxidase (POD)
and heat shock protein (HSP) 70. Meanwhile, this treatment did not significantly affect fruit firmness, titratable acidity and total
soluble solids, but enhanced the accumulation of carotenoids. These results suggest that hot air treatment can enhance disease
resistance of loquat fruit by inducing the activity and gene expression of defense-related enzymes.

Effect of Nitric Oxide Fumigation on Lignification of Loquat Fruits during Cold Storage
ZHANG Mei-zi, WU Guang-bin, CHEN Fa-he*
2014, 35(16):  232-237.  doi:10.7506/spkx1002-6630-201416045
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The present study was designed to explore the effect of exogenous nitric oxide (NO) on lignification of loquat
(Eriobotrya japonica Lindl. cv. Jiefangzhong) fruits during cold storage. The fruits were fumigated with (0, 5, 15, 25, 35
and 45 μL/L) NO gas. Fruit firmness, juice percentage, total soluble sugar, titratable acid and lignin content, and the enzyme
activities related to lignin metabolism were analyzed during cold storage (5 ℃) of loquat fruits. The results indicated that
nitric oxide treatments delayed the decline of total soluble sugar and titratable acid content. Meanwhile, NO fumigation
inhibited the increase of fruit firmness and the decrease of juice percentage, thereby maintaining better commercial quality
of loquat fruits. Nitric oxide treatments significantly inhibited the activities of phenylalanine ammonialyase (PAL) and
cinnamylalcohol dehydrogenase (CAD), delayed the reduction of total soluble sugar, and inhibited the increase of lignin
content, thus postponing the development of lignification of loquat fruits during cold storage. The treatments with nitric
oxide at 15 and 25 μL/L were more effective.

Establishment of a Mathematical Model for Treatment of Gynura bicolor DC. by Nano-Packaging in Combination with Controlled Atmosphere
JIANG Li1, FENG Li1, HOU Tian-ying2, YU Zhi-fang1
2014, 35(16):  238-243.  doi:10.7506/spkx1002-6630-201416046
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The effects of nano-packaging (NP) in combination with controlled atmosphere (CA) on the preservation and
nutritional quality of fresh Gynura bicolor DC (G. bicolor). were investigated during storage at 0 ℃. The nutrition and
quality indices including decay index, respiration rate, as well as the contents of anthocyanin, chlorophyll, amino acid,
protein, total carbohydrate and reducing sugar were tested every 5 days. The combined treatment (CA+NP) improved the
nutritional quality of G. bicolor compared with polyethylene packaging in CA or NP in a modified atmosphere alone. After
20-day storage, CA + NP treatment significantly inhibited respiration intensity and maintained higher contents of total
soluble solids, anthocyanin, chlorophyll, amino acids, protein, total sugar, and reducing sugar. The simplified regression
model: Decay index/%=24.605 - 0.020X7 + 1.122X4 - 0.162X5 (where, X4: reducing sugar content, X5: anthocyanin content,
X7: chlorophyll content) revealed satisfactory goodness of fit (R2 > 0.9). Hence, this model can be applied in practice.

Effects of High Hydrostatic Pressure Processing on the Flavor and Quality of Cultured Yellow Croaker (Pseudosciaena crocea)
YANG Hua1,2,3, LU Sen-chao1, ZHANG Hui-en1, LIU Li-jun1, QI Xiang-yang1
2014, 35(16):  244-249.  doi:10.7506/spkx1002-6630-201416047
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In this paper, cultured Pseudosciaena crocea muscle was examined for changes in nutritional components, flavor,
color difference, texture and microstructure after ultra high pressure (UHP) treatment. The results showed that the water
activity was reduced after UHP treatment, the moisture content was increased firstly and then decreased. The protein content
was also increased and the crude fat content was changed significantly (P < 0.05). In terms of nutritional components,
400 MPa (10 min) was the optimal treatment condition. The UHP treatment had little effect on the volatile composition
of the fish. The color was influenced by all pressure, dwelling time and storage time. After 10 min of UHP treatment at
300 MPa, no significant change in color difference was observed compared to the untreated control (P > 0.05). The
hardness, cohesiveness, elasticity and chewing of the fish was positively dependent on pressure. Scanning electron
microscopic (SEM) observation confirmed that the structure of cultured Pseudosciaena crocea muscle with high pressure
treatment differed significantly from that of the control.

Effect of Pretreatment with Ethanol on Bioactive Compounds and Antioxidant Activity in Fresh-Cut Broccoli Florets
WANG Hui-qian, ZHENG Cong, WANG Hua-dong, WANG Jing, ZHENG Yong-hua*
2014, 35(16):  250-254.  doi:10.7506/spkx1002-6630-201416048
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The effect of ethanol vapor treatment on bioactive compounds, such as total phenols, flavonoids, total
glucosinolates and sulforaphane, and antioxidant activity of fresh-cut broccoli florets was investigated. The broccoli heads
were pretreated with 2%, 5%, 10% or 20% ethanol vapor at 20 ℃ for 6 h, then cut into small florets and stored at 10 ℃
for 10 days. The results showed that pretreatment with 10% ethanol significantly prolonged the shelf life of fresh-cut
broccoli, increased the contents of total phenols and flavonoids, delayed the decrease in the contents of total glucosinolates
and sulforaphane. This treatment also effectively maintained higher DPPH (1,1-diphenyl-2-picrylhydrazyl) free radical
scavenging activity and reducing power, improved superoxide anion and hydroxyl free radical scavenging ability, thereby
delaying postharvest senescence and maintaining higher antioxidant activity of fresh-cut broccoli florets. Meanwhile, it
was found that there was a significant positive relationship between the contents of total phenols, flavonoids, glucosinolates
and DPPH free radical scavenging activity. These results demonstrate that ethanol treatment may be a promising method to
extend the shelflife and maintain the nutritional quality of fresh-cut broccoli.

Effects of Soaking Treatments with Citric Acid, Sodium Chloride and Apple Polyphenols on Microbial Populations and Shelf Life of Fresh Truffles
MIAO Yu-zhi1, CHEN Cui-ping2, LI Wei1, GE Fang-lan1
2014, 35(16):  255-160.  doi:10.7506/spkx1002-6630-201416049
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The effects of soaking treatments with citric acid (CTA), sodium chloride (NaCl) and apple polyphenols (APP) on
the populations of bacteria, moulds and yeasts, sensory quality and shelf life of fresh truffles were investigated. Fresh truffles
were soaked with CTA, NaCl and APP alone or in combination for 30 min at 45 ℃, and the total bacterial counts, and mold
and yeast counts were assayed. In addition, the sensory quality was judged and the shelf-life of un-soaked and soaked truffles
of storage in vacuum packaging at 4 ℃ was evaluated. There were noticeable reductions in the populations of bacteria, molds
and yeasts in soaked truffles with the individual agents; the combined treatments had marked synergistic antimicrobial effects
compared with the summation of the effects of each individual treatment. Taking into account 32 as a threshold value for
sensory acceptability, the optimal concentrations f individual treatments were 2.5% CTA, 5.0% NaCl and 2.0% APP. The
optimal concentrations for combined treatments were 2.0% APP + 2.5% CTA, 5.0% NaCl + 2.0% CTA and 2.0% APP + 5.0%
NaCl, respectively. Based on the experimental results from the combinations, the optimal concentration of CTA + NaCl +
APP was 2.0% + 5.0% + 2.0%; the shelf-life of fresh truffles was prolonged to 49 days by this combined treatment.

Technology Application
Comparison of Quality Characteristics of Lotus Root Pork Rib Soups from Electric Pressure Cooker and Clay Cooker
ZHANG Jing-yan1, XU Feng1, SHI Yun2, WANG Ke-xing1, WANG Lu-feng1,*
2014, 35(16):  261-266.  doi:10.7506/spkx1002-6630-201416050
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The conditions for cooking lotus root pork rib soup with an electric pressure cooker were optimized using single
factor and orthogonal array design methods. This study also compared sensory and texture characteristics of lotus root pork
rib soups cooked with the electric pressure cooker and a clay cooker. The optimum cooking conditions using the electric
pressure cooker were obtained as follows: rib to water ratio 1:3, and 70 kPa for 20 min and then 20 kPa for additional 45 min.
The resulting product contained 81.74 mg/mL soluble protein and showed highly similar sensory and texture characteristics
with the soup cooked with the clay cooker. Furthermore, the cooking time was shortened by 85 min under the optimized
pressurized cooking conditions as compared to clay pot cooking.

Application of Fuzzy Evaluation and Response Surface Methodology for the Formulation of Walnut Paste Nutritious Breakfast
LI Rong1, YI Xin2, MA Li1, XING Ya-ge1, RAO Yu1, CHE Zhen-ming1,*
2014, 35(16):  267-272.  doi:10.7506/spkx1002-6630-201416051
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This work was carried out to optimize walnut paste nutritious breakfast formulations by using response surface analysis
with comprehensive sensory evaluation results obtained from fuzzy mathematics as a response variable. Results indicated that the
addition of walnut protein, skim milk powder, puffed rice flour, white sugar and peanut powder had significant influences on the
fuzzy sensory score (P < 0.01). The best formulation of the walnut paste breakfast was composed of walnut protein 11.9 g, skim
milk powder 8.4 g, puffed rice flour 4.6 g, white sugar 4.0 g and peanut powder 2.0 g. Moreover, high significance of the regression
model between the fuzzy sensory score and the addition levels of walnut protein, skim milk powder, puffed rice flour, white sugar
and peanut powder was also observed from the results of multiple regressions.