Chen Huifan, Zhou Huimin, Wang Zhenguo, Hu Xialin, Yin Daqiang
{"title":"固相萃取-超高效液相色谱-串联质谱-电喷雾法同时测定地面水中7种苯并三唑类紫外稳定剂","authors":"Chen Huifan, Zhou Huimin, Wang Zhenguo, Hu Xialin, Yin Daqiang","doi":"10.1002/jssc.70200","DOIUrl":null,"url":null,"abstract":"<div>\n \n <p>Benzotriazole ultraviolet stabilizers (BUVSs) are emerging persistent pollutants, due to the weak polarity and wide log <i>K</i><sub>ow</sub> values, there is no general optimal analytical method for BUVSs. In this study, a solid-phase extraction-ultra performance liquid chromatography tandem mass spectrometry (SPE-UHPLC/MS/MS) method was developed for the simultaneous determination of seven BUVSs in the aqueous environment, based on the generalized electrospray ionization (ESI+) mode. The conditions of ESI-UHPLC-MS/MS detection and SPE were systematically optimized. A 50 mm UHPLC column at a column temperature of 40°C gave the highest response for the target BUVSs using methanol–0.1% (v/v) formic acid solution as the mobile phase. The effects of the four packed SPE cartridges (HLB, HC-C<sub>18</sub>, LC-C<sub>18</sub> and phenyl columns) and sample pH (3.0–9.0) on the SPE enrichment were comparatively analyzed, and the optimum condition was HLB cartridges at sample pH 3.0. The SPE elution solvent was optimized as 5 mL methanol + 5 mL dichloromethane (V:V = 1:1). The seven target BUVSs were quantified by isotope internal standard method, and the linear range of the standard curve was wide (0.1–50 ng∙L<sup>−1</sup>) with the correlation coefficient <i>R</i><sup>2</sup> > 0.998. The recoveries of the spiked standards for the purified water as well as the sample of Huangpu River were 80.6%–105.2% and 53.9%–103.7% (except UV-P: 141.6%–148.7%), respectively. The relative standard deviations (RSDs) of the intra-day were 4.1%–18.0%; and the RSDs of the inter-day were 3.4%–18.8%, respectively. The limits of detection of the method were in the range of 0.050–0.406 ng∙L<sup>−1</sup>. Compared with the reported studies, this method is more sensitive and stable, and the UHPLC-MS/MS instrument based on the ESI ionization source is more generalizable.</p>\n </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8000,"publicationDate":"2025-06-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Simultaneous Determination of Seven Benzotriazole UV Stabilizers in Surface Waters by Using Solid-Phase Extraction Coupled With Ultra-High-Performance Liquid Chromatography Tandem Mass Spectrometry With Electrospray Ionization\",\"authors\":\"Chen Huifan, Zhou Huimin, Wang Zhenguo, Hu Xialin, Yin Daqiang\",\"doi\":\"10.1002/jssc.70200\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div>\\n \\n <p>Benzotriazole ultraviolet stabilizers (BUVSs) are emerging persistent pollutants, due to the weak polarity and wide log <i>K</i><sub>ow</sub> values, there is no general optimal analytical method for BUVSs. In this study, a solid-phase extraction-ultra performance liquid chromatography tandem mass spectrometry (SPE-UHPLC/MS/MS) method was developed for the simultaneous determination of seven BUVSs in the aqueous environment, based on the generalized electrospray ionization (ESI+) mode. The conditions of ESI-UHPLC-MS/MS detection and SPE were systematically optimized. A 50 mm UHPLC column at a column temperature of 40°C gave the highest response for the target BUVSs using methanol–0.1% (v/v) formic acid solution as the mobile phase. The effects of the four packed SPE cartridges (HLB, HC-C<sub>18</sub>, LC-C<sub>18</sub> and phenyl columns) and sample pH (3.0–9.0) on the SPE enrichment were comparatively analyzed, and the optimum condition was HLB cartridges at sample pH 3.0. The SPE elution solvent was optimized as 5 mL methanol + 5 mL dichloromethane (V:V = 1:1). The seven target BUVSs were quantified by isotope internal standard method, and the linear range of the standard curve was wide (0.1–50 ng∙L<sup>−1</sup>) with the correlation coefficient <i>R</i><sup>2</sup> > 0.998. The recoveries of the spiked standards for the purified water as well as the sample of Huangpu River were 80.6%–105.2% and 53.9%–103.7% (except UV-P: 141.6%–148.7%), respectively. The relative standard deviations (RSDs) of the intra-day were 4.1%–18.0%; and the RSDs of the inter-day were 3.4%–18.8%, respectively. The limits of detection of the method were in the range of 0.050–0.406 ng∙L<sup>−1</sup>. Compared with the reported studies, this method is more sensitive and stable, and the UHPLC-MS/MS instrument based on the ESI ionization source is more generalizable.</p>\\n </div>\",\"PeriodicalId\":17098,\"journal\":{\"name\":\"Journal of separation science\",\"volume\":\"48 7\",\"pages\":\"\"},\"PeriodicalIF\":2.8000,\"publicationDate\":\"2025-06-30\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of separation science\",\"FirstCategoryId\":\"5\",\"ListUrlMain\":\"https://onlinelibrary.wiley.com/doi/10.1002/jssc.70200\",\"RegionNum\":3,\"RegionCategory\":\"工程技术\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q2\",\"JCRName\":\"CHEMISTRY, ANALYTICAL\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of separation science","FirstCategoryId":"5","ListUrlMain":"https://onlinelibrary.wiley.com/doi/10.1002/jssc.70200","RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"CHEMISTRY, ANALYTICAL","Score":null,"Total":0}
Simultaneous Determination of Seven Benzotriazole UV Stabilizers in Surface Waters by Using Solid-Phase Extraction Coupled With Ultra-High-Performance Liquid Chromatography Tandem Mass Spectrometry With Electrospray Ionization
Benzotriazole ultraviolet stabilizers (BUVSs) are emerging persistent pollutants, due to the weak polarity and wide log Kow values, there is no general optimal analytical method for BUVSs. In this study, a solid-phase extraction-ultra performance liquid chromatography tandem mass spectrometry (SPE-UHPLC/MS/MS) method was developed for the simultaneous determination of seven BUVSs in the aqueous environment, based on the generalized electrospray ionization (ESI+) mode. The conditions of ESI-UHPLC-MS/MS detection and SPE were systematically optimized. A 50 mm UHPLC column at a column temperature of 40°C gave the highest response for the target BUVSs using methanol–0.1% (v/v) formic acid solution as the mobile phase. The effects of the four packed SPE cartridges (HLB, HC-C18, LC-C18 and phenyl columns) and sample pH (3.0–9.0) on the SPE enrichment were comparatively analyzed, and the optimum condition was HLB cartridges at sample pH 3.0. The SPE elution solvent was optimized as 5 mL methanol + 5 mL dichloromethane (V:V = 1:1). The seven target BUVSs were quantified by isotope internal standard method, and the linear range of the standard curve was wide (0.1–50 ng∙L−1) with the correlation coefficient R2 > 0.998. The recoveries of the spiked standards for the purified water as well as the sample of Huangpu River were 80.6%–105.2% and 53.9%–103.7% (except UV-P: 141.6%–148.7%), respectively. The relative standard deviations (RSDs) of the intra-day were 4.1%–18.0%; and the RSDs of the inter-day were 3.4%–18.8%, respectively. The limits of detection of the method were in the range of 0.050–0.406 ng∙L−1. Compared with the reported studies, this method is more sensitive and stable, and the UHPLC-MS/MS instrument based on the ESI ionization source is more generalizable.
期刊介绍:
The Journal of Separation Science (JSS) is the most comprehensive source in separation science, since it covers all areas of chromatographic and electrophoretic separation methods in theory and practice, both in the analytical and in the preparative mode, solid phase extraction, sample preparation, and related techniques. Manuscripts on methodological or instrumental developments, including detection aspects, in particular mass spectrometry, as well as on innovative applications will also be published. Manuscripts on hyphenation, automation, and miniaturization are particularly welcome. Pre- and post-separation facets of a total analysis may be covered as well as the underlying logic of the development or application of a method.