电喷雾-离子迁移谱法快速筛查保健品和中成药中5种违禁化学药物  

Rapid screening of 5 kinds of illegal drugs in improving sleep health foods and traditional Chinese medicines by electrospray ionization-ion mobility spectrometry

作　　者：叶雅真 骆和东[1,2] 张璨雯 黄三发[1,2] 蔡伟鹏[2] 

机构地区：[1]厦门市食品药品质量检验研究院,厦门361012 [2]厦门市疾病预防控制中心,厦门361021 [3]集美大学生物与工程学院,厦门361021

出　　处：《食品安全质量检测学报》2016年第10期4050-4058,共9页Journal of Food Safety and Quality

基　　金：福建省自然科学基金面上项目(2014D005)~~

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。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（r0.99） 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.

关 键 词：电喷雾-离子迁移谱法 改善睡眠功能保健食品 非法添加 快速检测 

分 类 号：R286.0[医药卫生—中药学] TS218[医药卫生—中医学]