高效液相色谱串联质谱检测食用植物油中的乙基麦芽酚

Determination of Ethyl Maltol in Edible Vegetable Oil Using High Performance Liquid Chromatography Tandem Mass Spectrometry/Mass Spectrometry

为了建立食用植物油中乙基麦芽酚检测的高效液相色谱串联质谱方法,食用植物油样品与二氯甲烷混合后,以1.5%NaOH水溶液做为提取溶剂,涡旋、离心后,用磷酸将上层提取液调至4~7,调节pH后的上清液用PLS固相萃取柱进行净化除杂。采用电喷雾电离源正离子多反应监测模式进行检测,采用溶剂匹配标准曲线外标法进行定量。结果表明:该方法在6.25~100 ng/mL质量浓度范围内线性关系良好(R^(2)>0.999),方法定量限为25.0μg/kg,在3个加标水平下的平均回收率为82.9%~105.1%,相对标准偏差小于5%,重复性好。该方法准确、灵敏度高,能有效减少芝麻油的基质效应,适用于多种食用植物油中乙基麦芽酚的检测。

To establish a method for determination of ethyl maltol in edible vegetable oil by high performance chromatography tandem mass spectrometry/mass spectrometry,edible vegetable oil samples were mixed with dichloromethane in a ratio of 1∶1,and 1.5%NaOH aqueous solution was used as the extraction solvent.After eddying and centrifugation,the supernatant was adjusted to 4-7 with phosphoric acid,and the pH-adjusted supernatant was purified with a PLS solid phase extraction cartridge to remove impurities.Electron spray ionization source was used for detection in positive ion multiple reaction monitoring mode.Ethyl maltol was quantified by solvent-matched standard curve external standard method.The results indicated that the method had a good linear correlation in the range of 6.25~100 ng/mL(R^(2)>0.999),the limit of quantification was 25.0μg/kg,the average recovery at three spiked levels was 82.9%-105.1%,and the relative standard deviations were below 5%with a good repeatability.The method was accurate and sensitive,especially can effectively reduce the matrix effect of sesame oil,and was suitable for the detection of ethyl maltol in various edible vegetable oil.