Yiqin Xu, Fang Yang, Hong Ye, Qingqiang Tang, Yanwen Chen, Zhigang Gao, Shuhua Wang, Fang Zhang, Xiaojing Li
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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":"{\"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. 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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. 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Determination of three ephedrine psychoactive substances in sewage using solid-phase extraction–ultra-performance liquid chromatography–tandem mass spectrometry
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.
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.
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