高效液相色谱-串联质谱法测定乳及乳制品中17种真菌毒素

Determination of 17 Mycotoxins in Milk and Dairy Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry

基于高效液相色谱-串联质谱技术建立同时检测乳及乳制品中17种真菌毒素的方法。样品称量后加入定量同位素内标溶液,经20 mL乙腈-水-甲酸溶液(70∶29∶1,V/V)涡旋振荡提取,加入0.3 g氯化钠盐析,高速离心后上清液过0.22μm滤膜,用三重四极杆质谱在多反应监测模式下测定,通过同位素内标法定量。结果表明:在优化后的色谱及质谱条件下,17种真菌毒素线性范围良好,相关系数(r)均大于0.99,检出限为0.05~6.20μg/kg,定量限为0.2~20.0μg/kg,对低、中、高3个添加水平均具有良好的回收率和精密度,平均加标回收率为78.9%~119.5%,相对标准偏差为0.2%~8.4%。该方法操作便捷、稳定可靠、灵敏度高,能满足乳及乳制品中17种真菌毒素的定性定量分析要求,适用于实验室对乳及乳制品中17种真菌毒素的污染监测。

To establish a method for simultaneous detection of 17 mycotoxins in milk and dairy products based on high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Samples(5.0000 g)were added to 20μL of a mixed solution of isotope-labeled internal standards,extracted with 20 mL of acetonitrile-water-formic acid solution(70:29:1,V/V)by vortex shaking,salted out with 0.3 g of sodium chloride,and then centrifuged at high speed.The supernatant was passed through a 0.22μm membrane filter,detected by triple quadrupole mass spectrometry in the multi-reaction detection mode and quantified by an internal standard method.Results:Under the optimized instrumental conditions,good linearity was observed for the 17 mycotoxins in the tested concentration ranges,with correlation coefficient(r)greater than 0.99.The limit of detection(LOD)was 0.05-6.20μg/kg,and the limit of quantitation(LOQ)was 0.2-20.0μg/kg.Good average recoveries(78.9%-119.5%)and precision(relative standard deviations(RSDs)0.2%–8.4%)were achieved at three spiked levels.The method is convenient,stable,reliable and sensitive,can meet the requirements of qualitative and quantitative analysis of the 17 mycotoxins in milk and dairy products,and is suitable for laboratory monitoring of the contamination of these mycotoxins in milk and dairy products.