高效液相色谱-串联质谱法测定杂粮豆类中11种真菌毒素

Simultaneous Determination of 11 Mycotoxins in Minor Food Legumes by High Performance Liquid Chromatography-Tandem Mass Spectrometry(HPLC-MS/MS)

利用高效液相色谱-串联质谱建立杂粮豆类中11种真菌毒素(包括黄曲霉毒素B_1、B_2、G_1、G_2、赭曲霉毒素A、T-2毒素、脱氧雪腐镰刀菌烯醇、伏马毒素B1、B2和B3、玉米赤霉烯酮)同时检测的方法。实验对提取溶剂、提取时间和净化方式等进行优化,建立双体系联合提取方法,首先采用甲醇-水(70∶30,V/V)体系提取,再以乙腈-水(84∶16,V/V)体系二次提取,提取时间3 min,在此基础上采用C18吸附剂进行净化处理。结果表明,11种毒素的线性范围良好,相关系数大于0.999,添加回收率为70.0%～108%,相对标准偏差为1.3%～8.6%。所建方法简单、快速、灵敏度高、重复性好,可满足杂粮豆类中11种真菌毒素的同时检测需要。

A method was developed for the simultaneous determination of 11 mycotoxins in minor food legumes, including aflatoxins B1, B2, G1, G2, ochratoxins A, T-2, deoxynivalenol, fumonisins B1, B2 and B3 and zearalenone. Sample extraction and purification conditions were optimized. Samples were extracted with methanol-water(70:30, V/V) and acetonitrilewater(84:16, V/V) consecutively(the extraction process took 3 min), and then the extract was purified using C18 sorbent.The results showed that the calibration curves for all mycotoxins were linear with correlation coefficients above 0.999. The average recoveries of spiked samples ranged from 70.0% to 108%, with relative standard deviations(RSDs) from 1.3%to 8.6%. The method was simple and rapid with high sensitivity and repeatability, and it was suitable for simultaneous detection of 11 mycotoxins in minor food legumes.