同位素内标-高效液相色谱-串联质谱法同时测定小麦和玉米中19种真菌毒素

Simultaneous Determination of Isotope Internal Standard-High Performance Liquid Chromatography-Tandem Mass Spectrometry 19 Mycotoxins in Wheat and Corn

建立高效液相色谱-串联质谱法测定小麦和玉米中19种真菌毒素的检测方法。样品经乙腈∶水∶甲酸(80∶18∶2)溶液提取、离心、浓缩后,以C18色谱柱分离,甲醇-甲酸水溶液为流动相梯度洗脱,采用电喷雾正负离子(ESI+、ESI-)同时电离,多反应监测模式检测,同位素内标法定量。19种真菌毒素在一定含量范围内均具有良好的线性关系(R^(2)≥0.992),定量限范围为0.12~30μg/kg,在低、中、高3个添加浓度水平下的回收率范围为61%~117%,相对标准偏差小于15%(n=6),满足日常检测方法性能要求。本方法操作简便、灵敏度高、重现性好,适用于小麦、玉米等粮食中多种真菌毒素的同时测定。

A method for the determination of 19 mycotoxins in wheat and corn by high performance liquid chromatography-tandem mass spectrometry was established.After the sample was extracted with acetonitrile:water:formic acid(80∶18∶2)solution,centrifuged,and concentrated,it was separated on a C18 chromatographic column,methanol-formic acid aqueous solution was used as mobile phase gradient elution,and electrospray positive and negative ions(ESI+,ESI-)were used.Simultaneous ionization,multi-reaction monitoring mode detection,and isotope internal standard method for quantification.All the 19 mycotoxins had a good linear relationship within a certain content range(R^(2)≥0.992),the limit of quantification was 0.12~30μg/kg,and the recovery rate was 61%~117%,under the three levels of low,medium and high additive concentration,the relative standard deviation was less than 15%(n=6),which met the performance requirements of daily testing methods.This method was easy to operate,had a high sensitivity and a good reproducibility,and was suitable for the simultaneous determination of multiple mycotoxins in wheat,corn and other grains.