新型脱脂前处理净化-UPLC-MS/MS法测定食用油中6种真菌毒素

Simultaneous Determination of 6 Kinds of Mycotoxin in Oil by Enhanced Matrix Removal-Lipid-High Performance Liquid Chromatography-Tandem Mass Spectrometry

研究建立了一种采用新型脱脂前处理(EMR-Lipid)净化技术-高效液相色谱-串联质谱法同时测定食用油中黄曲霉毒素(AFB_(1)、AFB_(2)、AFG_(1)、AFG_(2))、赭曲霉毒素A(OTA)和玉米赤霉烯酮(ZEN)的方法。样品用含1%的乙酸乙腈溶液提取,通过EMR-Lipid净化剂净化后,以C_(18)色谱柱分离,用乙腈:甲醇(1:1)-5 mmol/L乙酸铵溶液进行梯度洗脱,采用高效液相色谱-串联质谱法测定,多反应监测(MRM)模式和同位素内标法定量。6种真菌毒素在一定质量浓度范围内线性良好,相关系数大于0.99,检出限为0.04~0.40μg/kg,定量限为0.12~1.20μg/kg,平均回收率为91.2%~119.8%,相对标准偏差(RSD)为2.9%~9.1%。该方法简单快速、灵敏可靠,适用于食用油中6种真菌毒素的快速准确检测。

To develop a method for the simultaneous determination of aflatoxin(AFB_1,AFB_2,AFG_1,AFG_2),ochratoxin A(OTA) and zearalanone(ZEN) in edible oil by enhanced matrix removal-lipid(EMR-Lipid)-high performance liquid chromatography-tandem mass spectrometry.The oil sample was extracted with 1% acetic acid-acetonitrile solution,purified by EMR-Lipid sorbent,separated by C_(18) chromatographic column with acetonitrile:methanol(1:1)-5 mmol/L ammonium acetate as mobile phase,the analyte was determined by high performance liquid chromatography-tandem mass spectrometry,and quantified by multiple reaction monitoring mode with internal standard method.The method had good linear relationship in the range of certain mass concentrations with correlation coefficients above 0.99,the limits of detection were 0.04-0.40 μg/kg,and the limits of quantitation were and 0.12-1.20 μg/kg,the recoveries and the relative standard deviations were in the range of 91.2%-119.8% and 2.9%-9.1%.This method is simple and fast,stable and reliable,and suitable for the simultaneous determination of 6 kinds of mycotoxin in oil.