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使用一锅合成的具有内置pH调节功能的磁性吸附剂结合液相色谱-串联质谱法快速简便地测定苯丙胺类兴奋剂

Rapid and Simplified Determination of Amphetamine-Type Stimulants Using One-Pot Synthesized Magnetic Adsorbents with Built-In pH Regulation Coupled with Liquid Chromatography-Tandem Mass Spectrometry.

作者信息

Shan Yabing, Chen Ying, Li Jiayi, Zeng Xianbin, Jia Rui, Liu Yuwei, Li Dongmei, Chen Di

机构信息

National Narcotics Laboratory Beijing Regional Center, Beijing 100164, China.

School of Pharmaceutical Sciences, Zhengzhou University, Zhengzhou 450001, China.

出版信息

J Xenobiot. 2025 Jul 2;15(4):102. doi: 10.3390/jox15040102.

DOI:10.3390/jox15040102
PMID:40700149
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC12286256/
Abstract

BACKGROUND

Amphetamine-type stimulants (ATS) in water pose significant public health and ecological risks, necessitating reliable and efficient detection methods. Current approaches often involve time-consuming pH adjustments and post-processing steps, limiting their practicality for high-throughput analysis. This study aimed to develop a streamlined method integrating pH regulation and adsorption into a single material to simplify sample preparation and enhance analytical efficiency.

METHODS

A novel FeO/MWCNTs-OH/CaO composite adsorbent was synthesized via a one-pot grinding method, embedding pH adjustment and adsorption functionalities within a single material. This innovation enabled magnetic solid-phase extraction (MSPE) without pre-adjusting sample pH or post-desorption steps. The method was coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) for ATS detection. Optimization included evaluating adsorption/desorption conditions and validating performance in real water matrices.

RESULTS

The method demonstrated exceptional linearity (R > 0.98), low detection limits (0.020-0.060 ng/mL), and high accuracy with relative recoveries of 92.8-104.8%. Precision was robust, with intra-/inter-day relative standard deviations (RSDs) below 11.6%. Single-blind experiments confirmed practical applicability, yielding consistent recoveries (relative errors: 1-8%) for ATS-spiked samples at 0.8 and 8 ng/mL. Compared to existing techniques, the approach reduced processing time to ~5 min by eliminating external pH adjustments and post-concentration steps.

CONCLUSIONS

This work presents a rapid, reliable, and user-friendly method for ATS detection in complex environmental matrices. The integration of pH regulation and adsorption into a single adsorbent significantly simplifies workflows while maintaining high sensitivity and precision. The technique holds promise for large-scale environmental monitoring and forensic toxicology, offering a practical solution for high-throughput analysis of emerging contaminants.

摘要

背景

水中的苯丙胺类兴奋剂(ATS)对公众健康和生态构成重大风险,因此需要可靠且高效的检测方法。目前的方法通常涉及耗时的pH调节和后处理步骤,限制了它们在高通量分析中的实用性。本研究旨在开发一种将pH调节和吸附整合到单一材料中的简化方法,以简化样品制备并提高分析效率。

方法

通过一锅研磨法合成了一种新型的FeO/MWCNTs-OH/CaO复合吸附剂,将pH调节和吸附功能嵌入到单一材料中。这一创新使得无需预先调节样品pH或进行解吸后处理步骤即可进行磁性固相萃取(MSPE)。该方法与液相色谱-串联质谱(LC-MS/MS)联用用于ATS检测。优化包括评估吸附/解吸条件并在实际水样中验证性能。

结果

该方法具有出色的线性(R>0.98)、低检测限(0.020 - 0.060 ng/mL)以及92.8 - 104.8%的高相对回收率,准确性高。精密度良好,日内/日间相对标准偏差(RSD)低于11.6%。单盲实验证实了其实际适用性,对于添加了0.8和8 ng/mL ATS的样品,回收率一致(相对误差:1 - 8%)。与现有技术相比,该方法通过消除外部pH调节和浓缩后步骤,将处理时间缩短至约5分钟。

结论

本研究提出了一种用于复杂环境基质中ATS检测的快速、可靠且用户友好的方法。将pH调节和吸附整合到单一吸附剂中显著简化了工作流程,同时保持了高灵敏度和精密度。该技术在大规模环境监测和法医毒理学方面具有应用前景,为新兴污染物的高通量分析提供了实用解决方案。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8b6e/12286256/04e9fd637de5/jox-15-00102-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8b6e/12286256/b8e9da026d59/jox-15-00102-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8b6e/12286256/712771ba0fac/jox-15-00102-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8b6e/12286256/623884258ea0/jox-15-00102-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8b6e/12286256/04e9fd637de5/jox-15-00102-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8b6e/12286256/b8e9da026d59/jox-15-00102-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8b6e/12286256/712771ba0fac/jox-15-00102-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8b6e/12286256/623884258ea0/jox-15-00102-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8b6e/12286256/04e9fd637de5/jox-15-00102-g004.jpg

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