稳定同位素稀释-超高效液相色谱-串联质谱法快速测定植物油中16种真菌毒素

A Fast Analytical Approach for Determination of 16 Kinds of Mycotoxins in Vegetable Oils Using Stable Isotope Dilution and Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了稳定同位素稀释-超高效液相色谱串联质谱法简单、快速、高效地检测植物油中16种真菌毒素的方法。植物油经乙腈-水-乙酸(84∶15∶1,V/V)提取并离心后,上清液用水1∶1(V/V)稀释,高速低温离心去除油脂,过膜后,加入稳定同位素内标补偿基质效应干扰,以五氟苯色谱柱为分离柱,用甲醇和含有0.1%(V/V)甲酸的1 mmol/L乙酸铵溶液进行梯度洗脱,超高效液相色谱-串联质谱(UPLC-MS/MS)检测,内标标准曲线法定量测定植物油中的16种真菌毒素。16种真菌毒素的线性相关系数均大于0.9994,检出限为0.1~66.7μg/kg,定量限为0.3~200.0μg/kg。4种不同植物油基质中,3个浓度水平的加标回收率为74.2%~105.6%,相对标准偏差为0.3%~13.9%。采用本方法检测了市售38个植物油样品中的真菌毒素。本方法简便、快速、可靠,可用于植物油中16种真菌毒素的快速准确检测。

A fast,simple and cost-effective UPLC-MS/MS method was established for determination of16 kinds of mycotoxins in vegetable oils with stable isotope dilution technique. Samples were extracted by acetonitrile-water-acetic acid 84∶ 15∶ 1（ V/V） and then diluted using water without any further clean-up steps.The mycotoxins were fully separated on a pentafluorophenyl column. Matrix effects were efficiently compensated by the [13 C]-labelled internal standards. The mean recoveries at three different concentration levels ranged from 74.2% to 105.6%,with RSD varied from 0. 3% to 13. 9%. Finally,the method was applied to analyze several kinds of vegetable oil samples. The method was simple,rapid,high sensitive and suitable for the determination of mycotoxins in vegetable oils.