Determination of three ephedrine psychoactive substances in sewage using solid-phase extraction–ultra-performance liquid chromatography–tandem mass spectrometry

IF 1.8 3区化学 Q4 BIOCHEMICAL RESEARCH METHODS

Rapid Communications in Mass Spectrometry Pub Date : 2024-08-26 DOI:10.1002/rcm.9877

Yiqin Xu, Fang Yang, Hong Ye, Qingqiang Tang, Yanwen Chen, Zhigang Gao, Shuhua Wang, Fang Zhang, Xiaojing Li

{"title":"Determination of three ephedrine psychoactive substances in sewage using solid-phase extraction–ultra-performance liquid chromatography–tandem mass spectrometry","authors":"Yiqin Xu, Fang Yang, Hong Ye, Qingqiang Tang, Yanwen Chen, Zhigang Gao, Shuhua Wang, Fang Zhang, Xiaojing Li","doi":"10.1002/rcm.9877","DOIUrl":null,"url":null,"abstract":"<div>\n \n <section>\n \n <h3> Rationale</h3>\n \n <p>In recent years, ephedrine psychoactive substances have attracted much attention due to their prevalence in water bodies and potential threat to aquatic ecosystems. Psychoactive substances have been considered as a new type of environmental pollutant due to their unpredictable potential risks to the behavior and nervous system of non-target organisms. A rapid, sensitive, selective, and robust method for the quantification of three ephedrine psychoactive substances in sewage is needed.</p>\n </section>\n \n <section>\n \n <h3> Methods</h3>\n \n <p>An ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the simultaneous determination of three ephedrine psychoactive substances in water. The optimal processing conditions were determined by optimizing the chromatography—mass spectrometry and solid-phase extraction (SPE) conditions (e.g., the SPE column, sample pH, washing, and elution), and the treatment conditions were determined; this was achieved via positive ion scanning in multiple reaction monitoring mode. Poly-Sery MCX was selected as the extraction column, with samples loaded at pH 3. And 4-mL solution of 2% formic acid (FA) aqueous solution was used as the eluent; the target compounds were eluted with 5 mL of 5% NH<sub>4</sub>OH in acetonitrile (ACN) solution. The best results were obtained when the residue was resolubulization in ACN after nitrogen evaporation.</p>\n </section>\n \n <section>\n \n <h3> Results</h3>\n \n <p>The developed UPLC-MS/MS showed a good linear relationship in the range of 0–50.00 μg/L, with determination coefficients (<i>R</i><sup>2</sup>) greater than 0.9990. The detection limit and quantitation limit were 0.05–0.10 and 0.20–0.50 μg/L, respectively. Recovery rates of the target compounds in blank sewage at three different concentrations ranged from 92.37% to 106.31%, with relative standard deviations (RSDs) of 0.77%–4.83% (n = 7).</p>\n </section>\n \n <section>\n \n <h3> Conclusions</h3>\n \n <p>This method has been successfully applied to the analysis of surface water and domestic sewage, and the samples were processed stably, indicating that the method is practical for the determination of ephedrine psychoactive drugs in water bodies.</p>\n </section>\n </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"38 20","pages":""},"PeriodicalIF":1.8000,"publicationDate":"2024-08-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Rapid Communications in Mass Spectrometry","FirstCategoryId":"92","ListUrlMain":"https://onlinelibrary.wiley.com/doi/10.1002/rcm.9877","RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"BIOCHEMICAL RESEARCH METHODS","Score":null,"Total":0}

引用次数: 0

Abstract

Rationale

In recent years, ephedrine psychoactive substances have attracted much attention due to their prevalence in water bodies and potential threat to aquatic ecosystems. Psychoactive substances have been considered as a new type of environmental pollutant due to their unpredictable potential risks to the behavior and nervous system of non-target organisms. A rapid, sensitive, selective, and robust method for the quantification of three ephedrine psychoactive substances in sewage is needed.

Methods

An ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the simultaneous determination of three ephedrine psychoactive substances in water. The optimal processing conditions were determined by optimizing the chromatography—mass spectrometry and solid-phase extraction (SPE) conditions (e.g., the SPE column, sample pH, washing, and elution), and the treatment conditions were determined; this was achieved via positive ion scanning in multiple reaction monitoring mode. Poly-Sery MCX was selected as the extraction column, with samples loaded at pH 3. And 4-mL solution of 2% formic acid (FA) aqueous solution was used as the eluent; the target compounds were eluted with 5 mL of 5% NH₄OH in acetonitrile (ACN) solution. The best results were obtained when the residue was resolubulization in ACN after nitrogen evaporation.

Results

The developed UPLC-MS/MS showed a good linear relationship in the range of 0–50.00 μg/L, with determination coefficients (R²) greater than 0.9990. The detection limit and quantitation limit were 0.05–0.10 and 0.20–0.50 μg/L, respectively. Recovery rates of the target compounds in blank sewage at three different concentrations ranged from 92.37% to 106.31%, with relative standard deviations (RSDs) of 0.77%–4.83% (n = 7).

Conclusions

This method has been successfully applied to the analysis of surface water and domestic sewage, and the samples were processed stably, indicating that the method is practical for the determination of ephedrine psychoactive drugs in water bodies.

查看原文本刊更多论文

利用固相萃取-超高效液相色谱-串联质谱法测定污水中的三种麻黄碱类精神活性物质。

理由：近年来，麻黄碱类精神活性物质因其在水体中的普遍存在以及对水生生态系统的潜在威胁而备受关注。精神活性物质对非目标生物的行为和神经系统具有不可预测的潜在风险，因此被视为一种新型环境污染物。需要一种快速、灵敏、选择性强且稳健的方法来定量检测污水中的三种麻黄碱类精神活性物质：方法：建立了一种超高效液相色谱-串联质谱（UPLC-MS/MS）同时测定水中三种麻黄碱类精神活性物质的方法。通过优化色谱-质谱和固相萃取（SPE）条件（如固相萃取柱、样品 pH 值、洗涤和洗脱）确定了最佳处理条件，并通过多反应监测模式下的正离子扫描确定了处理条件。选择 Poly-Sery MCX 作为萃取柱，在 pH 值为 3 的条件下装载样品；使用 4 毫升的 2% 甲酸（FA）水溶液作为洗脱液；目标化合物用 5 毫升的 5%NH4OH-乙腈（ACN）溶液洗脱。氮气蒸发后，残留物在 ACN 中再溶解，可获得最佳结果：所开发的 UPLC-MS/MS 在 0-50.00 μg/L 范围内线性关系良好，测定系数 (R2) 大于 0.9990。检测限和定量限分别为 0.05-0.10 和 0.20-0.50 μg/L。空白污水中三种不同浓度目标化合物的回收率为92.37%～106.31%，相对标准偏差（RSD）为0.77%～4.83%（n = 7）：该方法成功地应用于地表水和生活污水的分析，样品处理稳定，表明该方法适用于水体中麻黄碱类精神活性药物的测定。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

求助全文

约1分钟内获得全文求助全文

来源期刊

Rapid Communications in Mass Spectrometry 化学-分析化学

CiteScore

4.10

自引率

5.00%

发文量

219

审稿时长

2.6 months

期刊介绍： Rapid Communications in Mass Spectrometry is a journal whose aim is the rapid publication of original research results and ideas on all aspects of the science of gas-phase ions; it covers all the associated scientific disciplines. There is no formal limit on paper length ("rapid" is not synonymous with "brief"), but papers should be of a length that is commensurate with the importance and complexity of the results being reported. Contributions may be theoretical or practical in nature; they may deal with methods, techniques and applications, or with the interpretation of results; they may cover any area in science that depends directly on measurements made upon gaseous ions or that is associated with such measurements.