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Zhang X.Y.,Institute of Physical and Chemical Inspection
Zhonghua yu fang yi xue za zhi [Chinese journal of preventive medicine] | Year: 2013

To develop a rapid hilic ultra performance liquid chromatography (UPLC)-mass spectrum (MS)/MS method for determination of tetrodotoxin in seafood. The sample of muscle and liver of puffer fish and nassarius were extracted with aqueous solution containing 0.2% (V/V) acetic acid (the extract of liver must be purified through HLB cartridge), and then cleanup of extract was accomplished by solid-phase extraction with a graphitized carbon black cartridge. The analysis of tetrodotoxin was carried out on a chromatographic column (Acquity UPLC BEH Amide, 100 mm×2.1 mm×1.7 μm) with gradient elution of 95% (V/V) acetonitrile-H2O both containing 0.1% (V/V) formic acid and 2.0 mmol/L ammonium formate, and detected by positive electrospray ionization tandem mass spectrometry in the multiple reaction monitoring (MRM) mode, and quantified by matrix-match standard solution. The calibration curves were linear in the range of 30 - 10 000, 50 - 10 000 and 30 - 10 000 μg/kg of tetradotoxin in muscle and liver of puffer fish and in muscle of nassarius, respectively. The correlation coefficients were within 0.9963 - 0.9990. The limits of detection were 10, 20 and 10 μg/kg, and that of quantitation were 30, 50 and 30 μg/kg for muscle and liver of puffer fish and muscle of nassarius, respectively. The average recoveries were 81.5% - 93.1%, 82.3% - 106.0% and 83.5% - 95.2% for tetrodotoxin spiked in muscle and liver of puffer fish and in muscle of nassarius, respectively, with relative standard deviation (RSD) of 2.3% - 11%, 4.3% - 14.0% and 3.5% - 13.0% (n = 6). The method was simple, accurate and sensitive, and could be successfully applied to the measurement of tetrodotoxin in puffer fish and nassarius. Source


Liu Y.,Institute of Physical and Chemical Inspection | Lu Y.,Institute of Physical and Chemical Inspection | Wang L.,Institute of Physical and Chemical Inspection | Chang F.,Institute of Physical and Chemical Inspection | And 2 more authors.
Food Additives and Contaminants: Part B Surveillance | Year: 2015

A survey of 11 mycotoxins in 348 wheat flour samples marketed in Hebei province of China were analysed by liquid chromatography-tandem mass spectrometry, was carried out. The selected mycotoxins consisted of four aflatoxins (AFs: AFB1, AFB2, AFG1 and AFG2) and seven Fusarium toxins, i.e. deoxynivalenol (DON), nivalenol, 3-acetyldeoxynivalenol and 15-acetyldeoxynivalenol, zearalenone, Fusarenon-X and deoxynivalenol-3-glucoside. Results indicated that most of the wheat samples analysed were contaminated with mycotoxins. Wheat was most susceptible to DON (91.4% contamination), with a mean level of 240 μg kg−1. On average the probable daily intake (PDI, expressed as µg kg−1 body weight day−1) of mycotoxins was within the provisional maximum tolerable daily intake (PMTDI, 2.0 µg kg−1 of body weight day−1) as set by the Joint FAO/WHO Expert Committee on Food Additives. Nevertheless, exposure assessment revealed that the maximum PDI of mycotoxins was 4.06 µg kg−1 body weight day−1, which was twice the PMTDI value. Thus, consistent monitoring is recommended, as to keep the contamination level under control. © 2015 Taylor & Francis. Source


Liu Y.,Institute of Physical and Chemical Inspection | Lu Y.,Institute of Physical and Chemical Inspection | Wang L.,Institute of Physical and Chemical Inspection | Chang F.,Institute of Physical and Chemical Inspection | Yang L.,Beijing Institute of Control Engineering
Food Additives and Contaminants: Part B Surveillance | Year: 2015

A survey of 11 mycotoxins in 348 wheat flour samples marketed in Hebei province of China were analysed by liquid chromatography-tandem mass spectrometry, was carried out. The selected mycotoxins consisted of four aflatoxins (AFs: AFB1, AFB2, AFG1 and AFG2) and seven Fusarium toxins, i.e. deoxynivalenol (DON), nivalenol, 3-acetyldeoxynivalenol and 15-acetyldeoxynivalenol, zearalenone, Fusarenon-X and deoxynivalenol-3-glucoside. Results indicated that most of the wheat samples analysed were contaminated with mycotoxins. Wheat was most susceptible to DON (91.4% contamination), with a mean level of 240 μg kg−1. On average the probable daily intake (PDI, expressed as µg kg−1 body weight day−1) of mycotoxins was within the provisional maximum tolerable daily intake (PMTDI, 2.0 µg kg−1 of body weight day−1) as set by the Joint FAO/WHO Expert Committee on Food Additives. Nevertheless, exposure assessment revealed that the maximum PDI of mycotoxins was 4.06 µg kg−1 body weight day−1, which was twice the PMTDI value. Thus, consistent monitoring is recommended, as to keep the contamination level under control. © 2015 Taylor & Francis Source


Liu Y.P.,Institute of Physical and Chemical Inspection | Dong B.,Institute of Physical and Chemical Inspection | Qin Z.S.,Institute of Physical and Chemical Inspection | Yang N.J.,Institute of Physical and Chemical Inspection | And 4 more authors.
Food Additives and Contaminants: Part B Surveillance | Year: 2011

Ethyl carbamate (EC) in wine, grain spirits and wine sauce (145 samples) was analysed using solid-phase extraction and stable isotope dilution GC/MS. Samples were obtained from markets in eight areas (Shijiazhuang, Baoding, Handan, Qinhuangdao, Langfang, Zhangjiakou, Xingtai and Cangzhou) of Hebei Province, China. The method had a limit of detection of 2μgkg-1, with recoveries varying from 95.7 to 102% and RSD ranging 2.3-5.6%. The average concentrations of ethyl carbamate in wines, grain spirits and wine sauce were 14.7 (52.0-44.5) μgkg-1, 33.8 (2.9-129) μgkg-1 and 8.7 (52.0-63.3) μgkg-1, respectively. The results led to the development of limit standards that can be used to predict the concentration of ethyl carbamate in Chinese fermented wines. © 2011 Taylor & Francis. Source


Shen X.,Institute of Physical and Chemical Inspection
Zhonghua yu fang yi xue za zhi [Chinese journal of preventive medicine] | Year: 2013

OBJECTIVE: To understand the content status of ethyl carbamate (EC) in yellow rice wine and the changes in storage period and shelf life in Zhejiang province.METHODS: A total of 475 samples of yellow rice wine purchased randomly from supermarkets and food stores in Zhejiang province during 2008-2012, and 49 samples collected from manufacturers were measured for EC content. The sample collected from manufacturers by filter sterilization was placed at 4 °C, room temperature and 37 °C for 400 d, respectively;a bottled wine and a wine in bag were bought from market were placed for 400 d in room temperature to conduct shelf life storage test, and measure the content in every point in 2011. The EC of the samples was determinated by gas chromatography-mass spectrometry after the samples were diluted with D5-EC isotope dilution technique, and purified by alkaline diatomite solid phase extraction column.RESULTS: The overall detection rate of EC was 99% (472/475) in yellow rice wine of Zhejiang province in 2008-2012, the median value was 70-112 µg/kg, the 90th percentile was 190-333 µg/kg, the 95th percentile was 214-393 µg/kg, and the maximum value was 430-515 µg/kg. The content of EC was increased gradually along with the increasing of storage age in commercially yellow rice wine, and the average content of EC were positively correlated with storage age(r = 0.988). The contents of EC in yellow rice wine after sterilization increased from 74 µg/kg to 86 µg/kg, 127 µg/kg and 509 µg/kg at 4 °C, room temperature and 37°C, respectively for 400 d storage, the differences had statistical significance (F = 14.73, P < 0.01). The content of EC in yellow rice wines in shelf life, which stored in room temperature with bottle and bag package, was decreased slightly with increasing storage time in the beginning, from 215 to 184 µg/kg and 196 to 158 µg/kg, respectively, and increased again with increasing storage time after 250 d, with 252 µg/kg and 210 µg/kg in bottle and bag package after 400 d, respectively, the differences had statistical significance (Z = 2.37, P < 0.05).CONCLUSION: EC is widespread in rice wine, the content of EC was correlated with storage time and temperature. Source

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