【摘要】 目的建立电喷雾-离子迁移谱(electrospray ionization-ion mobility spectrometry,ESI-IMS)技术快速筛查改善睡眠类保健食品和中成药中非法添加地西泮、咪达唑仑、硝西泮、阿普唑仑、巴比妥等5种化学药物的分析方法。方法样品用乙腈超声提取,90%乙腈水溶液稀释后ESI-IMS直接测定。在正离子模式下检测地西泮和咪达唑仑,在负离子模式下检测硝西泮、阿普唑仑、巴比妥,基质外标法定量。结果 5种化合物在各自浓度范围内线性关系良好,相关系数均大于0.99。地西泮、咪达唑仑、巴比妥、硝西泮、阿普唑仑的检出限分别为0.20、0.50、2.00、8.00、8.00mg/L,平均回收率为78.7%~113.8%,相对标准偏差(RSD,n=6)小于10%,与液相色谱-串联质谱(1iquid chromatography-tandem mass spectrometryLC-MS/MS)检测结果一致。结论本方法快速准确,可实际应用于改善睡眠类健康产品中非法添加地西泮、咪达唑仑、硝西泮、阿普唑仑、巴比妥等5种违禁药物的筛查。更多还原

【Abstract】 Objective To establish a method for rapid screening of diazepam,midazolam,barbital,nitrazepam and alprazolam in health foods and traditional Chinese medicines by electrospray ionization-ion mobility spectrometry(ESI-IMS).Methods The samples were extracted by ultrasound with acetonitrile and the supernatant was diluted by 90%acetonitrile,and then detected by IMS with ESI~+ mode for diazepam and midazolam,with ESI~-mode for barbital,nitrazepam and alprazolam.The matrix-matched external standard method was used for quantification.Results Good linearities of 5 kinds of compounds were obtained(r>0.99) and the detection limits of diazepam,midazolam,barbital,nitrazepam and alprazolam were 0.20,0.50,2.00,8.00,8.00 mg/L,respectively.The recoveries were 78.7%~113.8%with the relative standard deviations below 10%(n=6).The results were in accordance with liquid chromatography-tandem mass spectrometry(LC-MS/MS).Conclusion The established method is rapid and accurate,and can be applied in detection of illegal drugs for improving sleep products of diazepam,midazolam,barbital,nitrazepam and alprazolam.更多还原