SPE-UPLC-MS/MS同时检测污水中多种滥用药物及其代谢物
Simultaneous determination of illicit drugs and their metabolites in wastewater by SPE-UPLC-MS/MS
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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≥0.993 2），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。
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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
Abstract: A quantitative analysis method based on solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS) for simultaneous determination of illicit drugs and their metabolites 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 ionization (ESI) in positive ion mode, and multiple reaction monitoring mode (MRM) was adopted for quantitative analysis. All analytes had a good linear relationship (r ≥ 0.993 2) 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. -
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