建立了超高效液相色谱-三重四极杆质谱(UPLC-MS/MS)快速检测红枣中链格孢菌代谢产生的细交链格孢菌酮酸(TEA)、链格孢酚(AOH)、交链格孢酚单甲醚(AME)和腾毒素(TEN)4种链格孢菌毒素的方法。采用2.0%甲酸-乙腈溶液超声提取,辅以0.2 g NaCl盐析,使用BEH C18色谱柱在6 min内快速分离毒素,并采用多反应监测模式(MRM)检测红枣中的4种链格孢菌毒素。除了链格孢酚的线性范围为1.0~100 μg/L外,其他3种毒素的线性范围均为10~1 000 μg/L,线性关系(r2)均大于0.990,检出限为0.5~12.4 μg/kg。4种毒素在空白基质中的加标回收率为92.8%~116%,相对标准偏差为0.5%~11.2%,可满足红枣中链格孢菌毒素的检测要求。运用毒理学软件理论计算得到成年人对4种毒素的允许每日暴露量(PDE)为19.30~25.65 μg/d。
Abstract
A noval method was established for the detection of four alternaria mycotoxins,iealternariol,alternariol monomethyl ether,tenuazonic acid and tentoxin in jujube by ultrahigh performance liquid chromatography-tandem mass spectrometry.The sample was extracted with 2.0% formic acid-acetonitrile by sonication and auxiliarily salted out with 0.2 g NaCl.Four alternaria mycotoxins in jujube were separated on a BEH C18 column in 6 min,and dectected in multiple reaction monitoring mode(MRM).The calibration curves for 4 alternaria mycotoxins showed good linearities in the ranges of 1.0-100 μg/L for alternariol and 10-1 000 μg/L for the other three toxins,with their correlation coefficients larger than 0.990 and the detection limits of 0.5-12.4 μg/kg.The spiked recoveries for 4 toxins in blank matrix were between 92.8% and 116% with the relative standard deviations of 0.5%-11.2%,which could meet the requirements for detection of alternaria mycotoxin in jujube.Moreover,the permitted daily exposures(PDE) for adults against 4 types of toxins were obtained to be 19.30-25.65 μg/d based on the calculation of the toxicological software theory.
关键词
超高效液相色谱-串联质谱(UPLC-MS/MS)链格孢菌毒素红枣风险评估
Keywords
ultrahigh performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)alternaria mycotoxinsjujuberisk assessment
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Related Author
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Related Institution
Hunan Provincial Center for Disease Control and Prevention
China National Center for Food Safety Risk Assessment
China National Research Institute of Food and Fermentation Industries
Key Laboratory of Theoretical Chemistry of Environment,Guangdong Provincial Key Laboratory of Chemical Pollution and Environmental Safety & MOE,School of Environment,South China Normal University
Faculty of Science,Beijing University of Chemical Technology