超高效液相色谱-三重四极杆质谱联用法同时测定粮谷类食品中的5种真菌毒素

Simultaneous determination of 5 kinds of mycotoxins in the grain by ultra performance liquid chromatography-triple quadrupole mass spectrometry

中文关键词:  超高效液相色谱-三重四极杆串联质谱法  粮谷类食品  真菌毒素  一步式净化

英文关键词:ultra performance liquid chromatography-triple quadrupole mass spectrometry  grain  mycotoxins  one-step clean-up

中文摘要:

      目的 建立一种一步式净化柱净化、超高效液相色谱-三重四极杆质谱联用法同时测定粮谷类食品中黄曲霉毒素B1、B2、G1、G2、玉米赤霉烯酮5种真菌毒素的分析方法。方法 以84%(V: V)乙腈作为提取溶剂, 样品经均质后经一步式多功能净化柱净化后进超高效液相色谱-三重四极杆质谱联用仪, 利用C18色谱柱分离, 采用电喷雾离子源(electrospray ionization, ESI)和多反应监测模式(multiple reaction monitoring mode, MRM), 在正、负离子模式下同时进行定性定量测定。结果 5种真菌毒素目标分析物在各自的质量测定浓度范围内, 线性相关系数良好(相关系数r2＞0.999), 方法定量限为0.10～4.00 μg/kg, 加标回收率为73.5%～112.5%, 相对标准偏差小于15%。结论 该方法前处理操作简便, 灵敏度高, 定性定量准确, 可满足对粮谷类产品中多种真菌毒素同时检测的要求。

英文摘要:

      Objective To establish a method for simultaneous determination of 5 mycotoxins including aflatoxin B1, B2, G1, G2 and zearalenone in the grain by ultra performance liquid chromatography-triple quadrupole mass spectrometry. Methods Grain samples were extracted by 84% (V: V) acetonitrile solution. Samples were homogenized, and then the extracts were further purified by one-step clean-up columns. Five types of mycotoxins in the samples were determined by ultra performance liquid chromatography-triple quadrupole mass spectrometry(UPLC-MS/MS) with C18 chromatographic column separation, electrospray ionization(ESI) source and multiple reaction monitoring mode (MRM) under the positive and negative ions mode at the same time. Results All of 5 types of mycotoxins had a good linear relationship (r 2＞0.999). The quantitative limit of the method was 0.104.00 μg/kg, the recoveries were from 73.5% to 112.5%, and the relative standard deviations(RSDs) were less than 15%. Conclusion The proposed method is fast, accurate and sensitive, which can be applied for the simultaneous determination of aflatoxin B1, B2, G1, G2 and zearalenone in the grain samples.