Sensitive determination of illicit drugs in wastewater using enrichment bag-based liquid-phase microextraction and liquid-chromatography tandem mass spectrometry
Sensitive determination of illicit drugs in wastewater using enrichment bag-based liquid-phase microextraction and liquid-chromatography tandem mass spectrometry
复制标题
使用基于富集袋的液相微萃取和液相色谱串联质谱法灵敏测定废水中的非法药物
DOI：
10.1016/j.chroma.2021.462684
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发表时间：
2022
影响因子：
4.1
通讯作者：
Chuixiu Huang
中科院分区：
文献类型：
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作者：
Shifan Wu;Ying Dong;Bin Lin;Xiantao Shen;Ping Xiang;Chuixiu Huang
为了浓缩复杂废水中痕量的分析物，在仪器分析之前，样品制备是必要的。因此，本研究首次提出了一种富集袋式液相微萃取（EB-LPME）系统，用于从废水中分离富集苯丙胺、甲基苯丙胺、3，4-亚甲二氧基甲基苯丙胺（MDMA）、氯胺酮、可待因和芬太尼等违禁药物。在最佳的EB-LPME条件下，模型药物的回收率为40-93%，富集因子高达93。在支撑液膜厚度、有效支撑液膜面积、萃取回收率和传质通量等方面与中空纤维-液相微萃取（HF-LPME）进行了比较。与HF-LPME相比，EB-LPME具有更大的有效SLM面积和更高的萃取回收率。此外，EB-LPME提供了更大的传质通量比HF-LPME，这主要是由于SLM厚度的差异。因此，SLM的厚度被确定为主要的传质通量的决定因素实验。采用液相色谱-串联质谱法（LC-MS/MS）评价了EB-LPME的基质效应，并证实了良好的样品净化效果。采用EB-LPME-LC-MS/MS方法进行了验证，结果令人满意，方法的检出限为0.3-8.7 ng/L。最后，采用标准加入法，将EB-LPME-LC-MS/MS成功应用于武汉某医院废水中模型药物的测定。本研究清楚地表明，EB-LPME显示出巨大的潜力，作为一个有效的样品制备方法的分离和富集的药物/污染物从复杂的环境样品的废水为基础的流行病学在不久的将来。
To concentrate trace level of analytes in complex wastewater, sample preparation is necessary prior to instrumental analysis. In this work, an enrichment bag-based liquid-phase microextraction (EB-LPME) system was therefore proposed for the first time to isolate and enrich the illicit drugs (amphetamine, methamphetamine, 3,4-methylenedioxymethamphetamine (MDMA), ketamine, codeine and fentanyl) from wastewater. Under the optimum EB-LPME conditions, the recoveries of the model illicit drugs were 40–93% with enrichment factors up to 93. The optimized EB-LPME was compared to hollow fiber-LPME (HF-LPME) in terms of the thickness of the supported liquid membrane (SLM), the effective SLM area, extraction recovery and mass transfer flux. Compared with HF-LPME, EB-LPME possesses larger effective SLM area, and provided higher extraction recovery. In addition, EB-LPME provided larger mass transfer flux than HF-LPME, which was mainly due to the differences in SLM thickness. Therefore, SLM thickness was identified as the main mass transfer flux-determining factor experimentally. The matrix effect of EB-LPME was evaluated using liquid chromatography-tandem mass spectrometry (LC-MS/MS), and excellent sample clean-up was confirmed. Subsequently, EB-LPME-LC-MS/MS was validated with satisfactory results, and the detection of limit of the proposed method was in the range of 0.3–8.7 ng/L. Finally, with standard addition method, EB-LPME-LC-MS/MS was successfully applied for the determination of the model drugs in a local hospital wastewater from Wuhan, China. This study clearly showed that EB-LPME displayed great potential as an efficient sample preparation method for isolation and enrichment of the drugs/pollutants from complex environmental samples for wastewater-based epidemiology in the near future.