固相萃取-液相色谱串联质谱法测定食品中的麻黄碱、芬氟拉明、西布曲明和酚酞
张志刚,郑向华,陈燕,吴敏,林建忠,徐敦明,林立毅
厦门海关技术中心,福建厦门 361013
Determination of ephedrine, fenfluramine, sibutramine and phenolphthalein in food by solid phase extraction-high performance liquid chromatography tandem mass spectrometry
张志刚,郑向华,陈燕,吴敏,林建忠,徐敦明,林立毅
Xiamen Customs Technical Center, Xiamen 361013, China
摘要:摘要建立固相萃取-高效液相色谱串联质谱法同时检测食品中可能非法添加的4种违禁添加药物(麻黄碱、芬氟拉明、西布曲明、酚酞)的分析方法。样品经0.1 mol/L盐酸水溶液提取后,经过Oasis HLB柱净化,采用电喷雾(ESI)离子源电离,正离子多反应监测(MRM)模式检测,以保留时间和子离子比进行定性分析,外标法定量分析。结果表明, 4种违禁药的质量浓度在2.0~200μg/L范围内与色谱峰面积的线性关系良好,线性相关系数均大于0.998,方法的检出限为2.5μg/kg,定量限为8μg/kg。各待测物在不同添加水平的回收率为71.0%~99.5%,测定结果的相对标准偏差为2.1%~8.2%(n=6)。该方法可用于食品中麻黄碱、芬氟拉明、西布曲明和酚酞4种非法添加物的同时且快速检测。
Abstract:A method for simultaneous determination of four illegal drugs(ephedrine, fen ?uramine, sibutramine and phenolphthalein) in food by solid phase extraction-high performance liquid chromatography tandem mass spectrometry was established. Samples were extracted by 0.1 mol/L hydrochloric acid solution, puri?ed by Oasis HLB column, ionized by electrospray(ESI) ion source, and detected by positive ion multiple reaction monitoring(MRM) mode. Qualitative analysis was carried out with retention time and daughter ion ratio, and external standard method was used for quantitative analysis. The results showed that the mass concentrations of the four banned drugs had good linear relationships with chromatographic peak areas in the range of 2.0-200μg/L, the linear correlation coef ?cients were more than 0.998, and the detection limits of the method were 2.5μg/kg, limits of quanti ?cation were 8μg/kg. The recoveries of the tested substances at different addition levels were 71.0%-99.5%, and the relative standard deviations of the determination results was 2.1%-8.2%(n=6). The method can be used for the simultaneous and rapid detection of ephedrine, fenfluramine, sibutramine and phenolphthalein in food.
关键词:关键词固相萃取;高效液相色谱串联质谱法;食品;麻黄碱;芬氟拉明;西布曲明;酚酞
Keywords:solid phase extraction; high performance liquid chromatography tandem mass spectrometry; food;ephedrine; fen?uramine; sibutramine; phenolphthalein
基金:福建省社会发展引导性(重点)项目(2018Y0075)
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张志刚,郑向华,陈燕,等.固相萃取-高效液相色谱串联质谱法测定食品中麻黄碱、芬氟拉明、西布曲明和酚酞[J].化学分析计量,2022,31(2):16.ZHANG Zhigang,ZHENG Xianghua,CHEN Yan,et al. Determination of ephedrine,fen?uramine,sibutramine and phenolphthalein in food by solid phase extraction-high performance liquid chromatography tandem mass spectrometry[J]. Chemical Analysis and Meterage,2022,31(2):16.
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