{"title":"液相色谱-串联质谱联用一锅合成pH调节磁吸附剂快速简便测定安非他明类兴奋剂","authors":"Yabing Shan, Ying Chen, Jiayi Li, Xianbin Zeng, Rui Jia, Yuwei Liu, Dongmei Li, Di Chen","doi":"10.3390/jox15040102","DOIUrl":null,"url":null,"abstract":"<p><strong>Background: </strong>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.</p><p><strong>Methods: </strong>A novel Fe<sub>3</sub>O<sub>4</sub>/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.</p><p><strong>Results: </strong>The method demonstrated exceptional linearity (R<sup>2</sup> > 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.</p><p><strong>Conclusions: </strong>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.</p>","PeriodicalId":42356,"journal":{"name":"Journal of Xenobiotics","volume":"15 4","pages":""},"PeriodicalIF":4.4000,"publicationDate":"2025-07-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12286256/pdf/","citationCount":"0","resultStr":"{\"title\":\"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.\",\"authors\":\"Yabing Shan, Ying Chen, Jiayi Li, Xianbin Zeng, Rui Jia, Yuwei Liu, Dongmei Li, Di Chen\",\"doi\":\"10.3390/jox15040102\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p><strong>Background: </strong>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.</p><p><strong>Methods: </strong>A novel Fe<sub>3</sub>O<sub>4</sub>/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.</p><p><strong>Results: </strong>The method demonstrated exceptional linearity (R<sup>2</sup> > 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.</p><p><strong>Conclusions: </strong>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.</p>\",\"PeriodicalId\":42356,\"journal\":{\"name\":\"Journal of Xenobiotics\",\"volume\":\"15 4\",\"pages\":\"\"},\"PeriodicalIF\":4.4000,\"publicationDate\":\"2025-07-02\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12286256/pdf/\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of Xenobiotics\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.3390/jox15040102\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q1\",\"JCRName\":\"TOXICOLOGY\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Xenobiotics","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.3390/jox15040102","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"TOXICOLOGY","Score":null,"Total":0}
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.
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 Fe3O4/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 (R2 > 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.
期刊介绍：
The Journal of Xenobiotics publishes original studies concerning the beneficial (pharmacology) and detrimental effects (toxicology) of xenobiotics in all organisms. A xenobiotic (“stranger to life”) is defined as a chemical that is not usually found at significant concentrations or expected to reside for long periods in organisms. In addition to man-made chemicals, natural products could also be of interest if they have potent biological properties, special medicinal properties or that a given organism is at risk of exposure in the environment. Topics dealing with abiotic- and biotic-based transformations in various media (xenobiochemistry) and environmental toxicology are also of interest. Areas of interests include the identification of key physical and chemical properties of molecules that predict biological effects and persistence in the environment; the molecular mode of action of xenobiotics; biochemical and physiological interactions leading to change in organism health; pathophysiological interactions of natural and synthetic chemicals; development of biochemical indicators including new “-omics” approaches to identify biomarkers of exposure or effects for xenobiotics.
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