超高效液相色谱串联质谱法检测谷物中8种真菌毒素.pdfVIP

2017 年第 30 卷第 2 期 粮食与油脂 97 超高效液相色谱串联质谱法检测 谷物中8 种真菌毒素 陈慧菲，郁海菲，秦施奇，黄鑫彦 （上海市粮食科学研究所，　上海　200333 ） 摘　要：建立了液质联用法同时测定脱氧雪腐镰刀菌烯醇、3– 乙酰基脱氧雪腐镰刀菌烯醇、15– 乙酰基脱氧雪腐镰刀菌烯醇、黄曲霉毒素B 、B 、G 、G 、玉米赤霉烯酮共8 种真菌毒素谷物中 1 2 1 2 的含量。样品经乙腈– 水溶液提取，通过多功能净化柱净化、Waters Acquity UPLC® BEH C18 色 谱柱分离、超高效液相色谱串联质谱系统测定，脱氧雪腐镰刀菌烯醇及其衍生物同位素内标法定 量，黄曲霉毒素和玉米赤霉烯酮外标法定量。结果表明，8 种真菌毒素在线性范围内线性相关性 2 R ≥0.999 ，检出限在0.3~1.0 μg/kg 之间，加标回收率在72.2%~101.7% 之间，相对标准偏差在 1.22%~9.69% 之间。该方法操作简单、灵敏度高、回收率好，适用于谷物及其制品中多种真菌毒 素的同时检测。 关键字：超高效液相色谱；真菌毒素；多功能净化柱 Determination of 8 mycotoxins in cereal with ultra performance liquid chromatographytandem mass spectrometry CHEN Hui-fei ，YU Hai-fei ，QING Shi-qi ，HUANG Xin-yan （Shanghai Cereal Science Research Institute ，Shanghai 200333 ，China ） Abstract ：A method （UPLC–MS/MS ）was developed to detect the content of 8 mycotoxins in the cereal ，including deoxynivalenol ，3–acety deoxynivalenol ，15–acety deoxynivalenol ，aflatoxin B ， 1 B ，G ，G and zearalenone. After the extraction by acetonitrile solution ，the sample was purified by 2 1 2 multifunctional purifiedcolumn ，then separated by waters acquity UPLC® BEH C 18 column ，and determined by the UPLS–MS/MS. Deoxynivalenol and its ramification were measured by isotopically internal standard method ，the aflatoxin and zearalenone were measured by external standard method. The results showed that 8 kinds of mycotoxins had a great linear relation with the correlation coefficients all above 0.999 ，meanwhile the limits of quantification （LOQs ）were 0.3– 1.0 μg/kg ，and the recovery o