液液萃取-超高效液相色谱-串联质谱法定量测定污水中10种毒品
Quantitative determination of 10 illicit drugs in wastewater by liquid-liquid extraction-ultra performance liquid chromatography-tandem mass spectrometry
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摘要: 建立一种基于液液萃取-超高效液相色谱-串联质谱法（LLE-UPLC-MS/MS）同时测定污水中10种毒品的氘代内标定量分析方法。污水样品经二氯甲烷-乙酸乙酯（1∶1）液液萃取浓缩，采用C18色谱柱，流动相为0.1%甲酸-5 mmol/L甲酸铵水溶液和乙腈，线性梯度洗脱分离，ESI正离子化多反应监测进行定量分析。10种待测物在各自的标准曲线范围内线性关系良好（r≥0.995 7），定量限为1 ng/L（除苯丙胺为2.5 ng/L），相对回收率范围为96.36% ~ 106.43%，日内与日间精密度均小于4.70%。该方法准确可靠、重复性好，适用于污水中10种毒品的定量检测，对影响固相萃取富集的复杂基质污水同样适用，为实时监测药品滥用提供了新的分析手段。
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关键词:
- 毒品 /
- 污水 /
- 液液萃取 /
- 超高效液相色谱-串联质谱法 /
- 含量测定
Abstract: A deuterated internal standard quantitative analysis method based on liquid-liquid extraction-ultra performance liquid chromatography-tandem mass spectrometry (LLE-UPLC-MS/MS) for simultaneous determination of 10 illicit drugs in wastewater was established.Wastewater samples were concentrated by liquid-liquid extraction with dichloromethane: ethyl acetate (1∶1), and separated by a linear gradient of 0.1% formic acid-5 mmol/L ammonium formate aqueous solution and acetonitrile on a C18 column. The samples were then detected by ESI positive ion mode and multiple reaction monitoring mode (MRM) for quantitative analysis.All analytes had a good linear relationship (r ≥ 0.995 7) within the range of their respective standard curves; the limit of quantification was 1 ng/L (except amphetamine at 2.5 ng/L); the relative recovery rate ranged from 96.36% to 106.43%, and the intra- and inter-day precisions were less than 4.70%.This method is accurate, reliable and reproducible, and is suitable for the quantitative determination of 10 illicit drugs in wastewater.It is also suitable for wastewater with complex matrixes that affect solid phase extraction and enrichment.It provides a new analytical method for real-time monitoring of drug abuse. -
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