摘要
建立一种基于固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)同时检测污水中多种滥用药物及其代谢物的定量分析方法。样品在pH 2条件下过滤后加入内标,利用Oasis Prime MCX固相萃取柱、甲醇淋洗溶剂4 mL、5%氨水-乙腈洗脱溶剂4 mL和0.1%甲酸水溶液复溶溶剂进行固相萃取,采用色谱柱ZORBAX Eclipse Plus C18进行色谱分析,流动相0.1%甲酸水溶液和乙腈进行梯度洗脱;采用ESI离子源正离子方式,多反应监测模式(MRM)进行定量分析。所有待测物在各自的标准曲线范围内线性关系良好(r≥0.9932),定量限为1 ng/L(除苯丙胺为2.5 ng/L),提取回收率范围为82.13%~99.96%,日内与日间精密度均小于9.43%。该方法准确可靠、重复性好,适用于污水中多种滥用药物及其代谢物的定量检测,为实时监测药品滥用提供了分析手段。
A quantitative analysis method based on solid phase extraction-ultra performance liquid chromatographytandem mass spectrometry(SPE-UPLC-MS/MS)for simultaneous determination of illicit drugs and their metabo⁃lites in wastewater was established.Samples filtered at pH of 2 and spiked with internal standard were loaded to Oasis Prime MCX cartridges for solid-phase extraction.The samples were washed with 4 mL of methanol and eluted with 4 mL of 5%ammonia in acetonitrile before reconstituting with 0.1%formic acid/water solution.ZORBAX Eclipse Plus C18 column was used for chromatography,and gradient elution was performed with 0.1%formic acid/water solution and acetonitrile as mobile phase.The samples were then detected by electrospray ion⁃ization(ESI)in positive ion mode,and multiple reaction monitoring mode(MRM)was adopted for quantitative analysis.All analytes had a good linear relationship(r≥0.9932)within the range of their respective standard curve;the limit of quantification was 1 ng/L(except amphetamine at 2.5 ng/L);the extraction recovery ranged from 82.13%to 99.96%;and the intra-and inter-day precisions were less than 9.43%.The method is accurate,reliable and reproducible,and is suitable for the quantitative determination of illicit drugs and their metabolites in wastewater and can provide an analytical method for real-time monitoring of drug abuse.
作者
王婧媛
侯臣之
花镇东
张婷婷
苏梦翔
徐慧
王优美
狄斌
WANG Jingyuan;HOU Chenzhi;HUA Zhendong;ZHANG Tingting;SU Mengxiang;XU Hui;WANG Youmei;DI Bin(Department of Pharmaceutical Analysis,China Pharmaceutical University,Nanjing210009;China National Narcotics Control Commission-China Pharmaceutical University Joint Laboratory on Key Technologies of Narcotics Control,Nanjing 210009;Drug Control Information and Technology Center of Ministry of Public Security of the People's Republic of China,Beijing 100741,China)
出处
《中国药科大学学报》
CAS
CSCD
北大核心
2020年第3期305-312,共8页
Journal of China Pharmaceutical University
基金
国家重点研发计划资助项目(No.2018YFC0807402)。
关键词
滥用药物
污水
固相萃取
超高效液相色谱-串联质谱
含量测定
illicit drugs
wastewater
solid phase extraction(SPE)
ultra performance liquid chromatographytandem mass spectrometry(UPLC-MS/MS)
content determination
作者简介
通信作者:王优美,E-mail:youmei_626@163.com;通信作者:狄斌,Tel:025-83271269,E-mail:dibin@cpu.edu.cn。
