高效液相色谱-串联质谱法测定白酒、配制酒中58种解热镇痛类非法添加化学药物

Determination of 58 antipyretic and analgesic drugs illegally added in liquor and prepared liquor by high performance liquid chromatography-tandem mass spectrometry

目的建立高效液相色谱-串联质谱法测定白酒、配制酒中58种解热镇痛类非法添加化学药物的方法。方法样品经甲醇超声提取后,以甲酸铵溶液-甲酸乙腈为流动相进行梯度洗脱,外标法定量,采用高效液相色谱-串联质谱法对样品进行测量。结果 58种待测化合物在相应的线性范围内呈良好的线性关系,相关系数大于0.995;定量限范围为0.1~2.5 mg/kg;在3个添加水平下, 58种待测物的平均回收率基本为85.0%~131.2%,进样精密度和重复性的相对标准偏差<12.31%(n=6)。结论该方法简单、快速、重复性好、稳定性强,适用于白酒、配制酒中清热镇痛类非法添加化学药物的检测。

Objective To establish a method for the determination of 58 antipyretic and analgesic drugs illegally added in liquor and prepared liquor by high performance liquid chromatography-tandem mass spectrometry.Methods After ultrasonic extraction with methanol,the mobile phase was ammonium formate solution acetonitrile formic acid for gradient elution.The external standard method was used for quantification.The samples were measured by high performance liquid chromatography tandem mass spectrometry.Results The 58 compounds showed good linear relationship in the corresponding linear range with all the correlation coefficient greater than 0.997.The limit of quantitation was 0.1-2.5 mg/kg;the average recoveries of 58 compounds were 85.0%-131.2%,and the relative standard deviations of injection precision and repeatability were less than 12.31%(n=6).Conclusion The method is simple,rapid,reproducible and stable,which is suitable for the detection of heat clearing and analgesic drugs illegally added in liquor and prepared liquor.