液相微萃取辅助表面增强拉曼光谱法：犯罪现场复杂样品中苯丙胺类兴奋剂的现场定量检测

摘要(中文译文)

苯丙胺类兴奋剂（ATS）的广泛滥用对公共安全和健康构成严重威胁，需要快速准确地现场检测ATS，特别是在犯罪现场进行刑事侦查和非法药物管制。然而，由于基质效应，通过表面增强拉曼散射（SERS）在犯罪现场检测复杂样品仍然是一个挑战。基于平膜的液相微萃取（FM-LPME）能够实现高效分离和充分的样品净化。FM-LPME用于克服SERS的基质效应，并开发了FM-LPME-SERS传感平台，用于快速准确地检测ATS。研究了关键操作因素对FM-LPME性能的影响。ENB和NPOE被确定为有效的支撑液膜溶剂。对于SERS，柠檬酸钠还原合成的银纳米粒子在SERS信号方面表现出优异的增强效果，溴化钠可以进一步改善ATS的SERS信号。最后，建立了一个基于偏最小二乘回归的定量模型来分析FM-LPME-SERS传感数据，该模型对血斑、尿液和废水样本的分析性能令人满意，检测限可接受（0.011-0.570μg mL-1），重复性高（RSD≤13%），准确度令人满意（90-114%）。该方法已成功应用于分析XX省公安局提供的药品生产现场的废水样本。因此，FM-LPME-SERS是现场检测复杂样本中ATS的有力工具，对法医学和公共安全具有重要意义。我们相信这项工作将扩大SERS对复杂样品的适用性。

Abstract

The widespread abuse of amphetamine-type stimulants (ATS) poses severe threats to public security and health, necessitating rapid and accurate on-site detection of ATS specially at crime scenes for criminal detection and illicit drug control. However, detection of complex samples at crime scenes by surface-enhanced Raman scattering (SERS) is still a challenge because of the matrix effect. Flat membrane-based liquid-phase microextraction (FM-LPME) enables efficient separation and sufficient sample clean-up. FM-LPME was used to overcome the matrix effect on SERS, and a sensing platform of FM-LPME-SERS was developed for rapid and accurate detection of ATS. The effect of key operation factors on FM-LPME performance was investigated. ENB and NPOE were identified as efficient supported liquid membrane solvent. For SERS, silver nanoparticles synthesized by sodium citrate reduction displayed superior enhancement in SERS signal, and the SERS signal for ATS could be further improved by sodium bromide. Finally, a quantitative model based on partial least squares regression was established to analyze the FM-LPME-SERS sensing data, which displayed satisfactory analytical performance for blood spot, urine, and wastewater samples with acceptable detection limit (0.011-0.570 μg mL), high repeatability (RSD ≤13%), and satisfactory accuracy (90-114%). This method was successfully applied to analyze wastewater samples from a drug production site provided by the Public Security Bureau in XX Province. Therefore, FM-LPME-SERS is a powerful tool for on-site detecting ATS in complex samples, which is of great importance for forensic science and public security. We believe this work will expand the applicability of SERS for complex samples.

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