摘要
建立超高效液相色谱-串联质谱法同时测定玉米中4种交链孢霉毒素的分析方法。样品粉碎后经磷酸二氢钠缓冲液-甲醇-乙腈的混合液提取,固相萃取柱净化,XBridge BEH C 18色谱柱分离,以甲醇-1.0 mmol/L碳酸氢铵水溶液为流动相进行梯度洗脱,采用电喷雾离子源负模式(ESI-)结合多反应监测方法(MRM)采集数据,测定结果用基质匹配工作曲线定量。细交链孢菌酮酸(TeA)、交链孢酚(AOH)和腾毒素(TEN)在1.0~100.0μg/L、交链孢酚单甲醚(AME)在0.1~10.0μg/L范围内线性良好(r>0.999)。4种毒素的方法检出限为0.005~0.501μg/kg。TeA、AOH、TEN在4.0~100.0μg/L、AME在0.4~10.0μg/L加标水平下,回收率为78.4%~100.3%,相对标准偏差为2.2%~8.9%,表明该方法具有较好的精密度和准确度,能满足玉米中4种交链孢霉毒素的检测要求。
This study developed a method for the simultaneous determination of four Alternaria mycotoxins in maize by ultra-high performance liquid chromatography-tandem mass spectrometry.Samples were purified by solid-phase extraction column after pulverization and extraction by methanol-acetonitrile-sodium dihydrogen phosphate buffer,then separated on an XBridge BEH C 18 with gradient elution by methanol and 1.0 mmol/L ammonium bicarbonate aqueous solution,and detected by UPLC-MS/MS under negation(ESI-)electrospray ionization and MRM models.The matrix-matched external standard calibration was used for quantitation.Tenuazonic acid(TeA),alternariol(AOH),and tentoxin(TEN)showed good linearity(r>0.999)in the concentration range of 0.1-100.0μg/L,as well as alternariol methyl ether(AME)in the concentration range of 0.1-10.0μg/L.The detection limit for 4 Alternaria mycotoxins was 0.005-1.002μg/kg.The average recoveries of TeA,AOH,and TEN were 78.4%-100.3%and the relative standard deviation was 2.2%-8.9%when TeA,AOH,and TEN were 4.0-100.0μg/L,and AME was 0.4-10.0 g/L,indicating that this method had high precision and accuracy and could meet the detection requirements of the 4 kinds of Alternaria mycotoxins in maize.
作者
苏爽
张二鹏
韩月哲
张榕杰
韩华云
贺静
SU Shuang;ZHANG Erpeng;HAN Yuezhe;ZHANG Rongjie;HAN Huayun;HE Jing(College of Chemistry,Zhengzhou University,Zhengzhou 450001,China;Henan Center for the Disease Control and Prevention,Zhengzhou 450016,China)
出处
《河南工业大学学报（自然科学版）》
CAS
北大核心
2020年第3期72-77,共6页
Journal of Henan University of Technology：Natural Science Edition
基金
河南省科技攻关项目“玉米、水稻等粮食作物及其制品中交链孢霉毒素污染水平分析和膳食暴露评估研究”(172102310339)。
