杂质吸附固相萃取–液相色谱串联质谱法同时测定粮食中15种真菌毒素

Simultaneous Determination of 15 Mycotoxins in Grains by Solid Phase Extraction with Impurity Adsorption and UPLC/MSMS

建立了同步检测粮食中15种真菌毒素的杂质吸附固相萃取–超高效液相色谱串联质谱方法。样品经0.1%酸化84%乙腈水溶液提取,杂质吸附柱Prime-HLB净化后,加入稳定同位素内标补偿基质效应干扰,选择Phenomenon Kinetex Bipheny l100A作为分离柱,采用梯度洗脱,超高效液相色谱–串联质谱(UPLC-MS/MS)检测,内标法定量。结果表明,15种真菌毒素的线性相关系数均大于0.996,检出限为0.2~15μg/kg,定量限为0.8~30μg/kg;三种基质3个添加水平的回收率为76.9%~116.1%,相对标准偏差(RSD)为1.4%~10%;对玉米基质标准物质进行检测验证,表明8种真菌毒素的检测值均在标示范围内;采用本方法检测了市售粮食135批次,共有97批样品检出真菌毒素,检出率为71%,多毒素同时污染现象较为普遍。方法可用于粮食及其制品中真菌毒素的快速检测。

To establish a method for the simultaneous determination of 15 mycotoxins in grains by ultra performance liquid chromatography tandem mass spectrometry(UPLC/MSMS).Samples were extracted by acidified acetonitrile solution,purified by impurity adsorption column prime HLB,and compensated for matrix effect interference by adding stable isotope internal standard.Phenomenon Kinetex Bipheny l100A column was used as separation column,gradient elution,UPLC-MS/MS for detection and internal standard method for quantification.The results showed that the linear correlation coefficient of 15 mycotoxins was greater than 0.996,the detection limit was 0.2-15μg/kg,the quantitative limit was 0.8-30μg/kg,the recovery of three levels of three kinds of matrixes was 76.9%-116.1%and the RSD was 1.4%-10%.The certified reference materials of corn matrix were The results from test and verification of corn matrix reference materials showed that the detection values of 8 mycotoxins were in the marked range.This method has been used to detect 135 batches of food sold in the market,97 batches of samples were detected have mycotoxin with a detection rate of 71%,multi toxin simultaneous pollution was common.The method is simple,rapid and reliable,and can be used for the rapid and accurate detection of 15 mycotoxins in grains.