固相萃取-超高效液相色谱-串联质谱法同时测定地表水中7种双酚类似物

Qiuxu Wang, Qiyan Feng, Guan-jiu Hu, Zhanqi Gao, Xueqiang Zhu, James Epua Epri
{"title":"固相萃取-超高效液相色谱-串联质谱法同时测定地表水中7种双酚类似物","authors":"Qiuxu Wang, Qiyan Feng, Guan-jiu Hu, Zhanqi Gao, Xueqiang Zhu, James Epua Epri","doi":"10.2139/ssrn.3934341","DOIUrl":null,"url":null,"abstract":"For the simultaneous measurement of seven types of bisphenol analogues (BPs) in surface water, a method combining solid-phase extraction (SPE) with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. The extraction efficiency was improved by optimizing the parameters that affect it, including the solid phase extraction cartridge, pH, enrichment factor, flow rate, rinsing and elution volumes. On the basis of a single factor experiment, an attempt to obtain the result of optimizing by response surface method was made, and the optimal parameters were as follows: at a flow rate of 8 mL/min, 1000 mL of water sample was run through the hydrophilic-lipophilic balancing cartridge, rinsed with 10% methanol, eluted with 9 mL methanol, and concentrated with nitrogen using an automatic solid-phase extraction system. The analytes were separated on an Acquity UPLC BEH C18 column using gradient elution with a mobile phase of acetonitrile and 0.05% (v/v) ammonia, and then analyzed using UPLC-MS/MS using multiple reaction monitoring in the negative-ion mode, with an 8-minute chromatographic run time. In the range of 1-500 μg/L, seven BPs showed good linearity with correlations greater than 0.99. The recovery ranged from 82.3%-96.7%, and the range of matrix effect was 89.2% to 107%. These results indicated excellent recovery and minimal matrix effect. The limits of detection were 0.025-1.5 ng/L, the relative standard deviation ranged were 2.9%-8.5%. Using the developed method, five BPs were detected in Luoma Lake and four BPs were detected in inflow rivers. BPA and BPF were the predominant BPs, and the concentration of BPA was the highest. The method was proved to be sensitive, accurate and efficient, and it was suitable for qualitative and quantitative analysis of seven BPs in surface water.","PeriodicalId":11510,"journal":{"name":"Ecology eJournal","volume":null,"pages":null},"PeriodicalIF":0.0000,"publicationDate":"2021-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"14","resultStr":"{\"title\":\"Simultaneous Determination of Seven Bisphenol Analogues in Surface Water by Solid-Phase Extraction and Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry\",\"authors\":\"Qiuxu Wang, Qiyan Feng, Guan-jiu Hu, Zhanqi Gao, Xueqiang Zhu, James Epua Epri\",\"doi\":\"10.2139/ssrn.3934341\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"For the simultaneous measurement of seven types of bisphenol analogues (BPs) in surface water, a method combining solid-phase extraction (SPE) with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. The extraction efficiency was improved by optimizing the parameters that affect it, including the solid phase extraction cartridge, pH, enrichment factor, flow rate, rinsing and elution volumes. On the basis of a single factor experiment, an attempt to obtain the result of optimizing by response surface method was made, and the optimal parameters were as follows: at a flow rate of 8 mL/min, 1000 mL of water sample was run through the hydrophilic-lipophilic balancing cartridge, rinsed with 10% methanol, eluted with 9 mL methanol, and concentrated with nitrogen using an automatic solid-phase extraction system. The analytes were separated on an Acquity UPLC BEH C18 column using gradient elution with a mobile phase of acetonitrile and 0.05% (v/v) ammonia, and then analyzed using UPLC-MS/MS using multiple reaction monitoring in the negative-ion mode, with an 8-minute chromatographic run time. In the range of 1-500 μg/L, seven BPs showed good linearity with correlations greater than 0.99. The recovery ranged from 82.3%-96.7%, and the range of matrix effect was 89.2% to 107%. These results indicated excellent recovery and minimal matrix effect. The limits of detection were 0.025-1.5 ng/L, the relative standard deviation ranged were 2.9%-8.5%. Using the developed method, five BPs were detected in Luoma Lake and four BPs were detected in inflow rivers. BPA and BPF were the predominant BPs, and the concentration of BPA was the highest. The method was proved to be sensitive, accurate and efficient, and it was suitable for qualitative and quantitative analysis of seven BPs in surface water.\",\"PeriodicalId\":11510,\"journal\":{\"name\":\"Ecology eJournal\",\"volume\":null,\"pages\":null},\"PeriodicalIF\":0.0000,\"publicationDate\":\"2021-12-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"14\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Ecology eJournal\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.2139/ssrn.3934341\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Ecology eJournal","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.2139/ssrn.3934341","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
引用次数: 14

摘要

为同时测定地表水中7种双酚类似物(bp),建立了固相萃取(SPE)与超高效液相色谱-串联质谱(UPLC-MS/MS)相结合的方法。通过优化固相萃取筒、pH、富集因子、流速、漂洗和洗脱体积等影响萃取效率的参数,提高了萃取效率。在单因素实验的基础上,尝试用响应面法获得优化结果,最佳参数为:以8 mL/min的流速,取1000ml水样通过亲水-亲脂平衡筒,用10%甲醇冲洗,用9ml甲醇洗脱,用自动固相萃取系统用氮气浓缩。色谱柱为Acquity UPLC BEH C18,流动相为乙腈- 0.05% (v/v)氨气,梯度洗脱,采用UPLC-MS/MS,负离子模式下多反应监测,色谱运行时间为8分钟。在1 ~ 500 μg/L范围内,7个bp具有良好的线性关系,相关系数均大于0.99。加样回收率为82.3% ~ 96.7%,基质效应为89.2% ~ 107%。结果表明,该方法回收率高,基质效应小。检出限为0.025 ~ 1.5 ng/L,相对标准偏差为2.9% ~ 8.5%。利用该方法,骆马湖共检测到5个bp,入流河流共检测到4个bp。BPA和BPF是主要的bp,其中BPA的浓度最高。结果表明,该方法灵敏、准确、高效,适用于地表水中7种bp的定性和定量分析。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Simultaneous Determination of Seven Bisphenol Analogues in Surface Water by Solid-Phase Extraction and Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry
For the simultaneous measurement of seven types of bisphenol analogues (BPs) in surface water, a method combining solid-phase extraction (SPE) with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. The extraction efficiency was improved by optimizing the parameters that affect it, including the solid phase extraction cartridge, pH, enrichment factor, flow rate, rinsing and elution volumes. On the basis of a single factor experiment, an attempt to obtain the result of optimizing by response surface method was made, and the optimal parameters were as follows: at a flow rate of 8 mL/min, 1000 mL of water sample was run through the hydrophilic-lipophilic balancing cartridge, rinsed with 10% methanol, eluted with 9 mL methanol, and concentrated with nitrogen using an automatic solid-phase extraction system. The analytes were separated on an Acquity UPLC BEH C18 column using gradient elution with a mobile phase of acetonitrile and 0.05% (v/v) ammonia, and then analyzed using UPLC-MS/MS using multiple reaction monitoring in the negative-ion mode, with an 8-minute chromatographic run time. In the range of 1-500 μg/L, seven BPs showed good linearity with correlations greater than 0.99. The recovery ranged from 82.3%-96.7%, and the range of matrix effect was 89.2% to 107%. These results indicated excellent recovery and minimal matrix effect. The limits of detection were 0.025-1.5 ng/L, the relative standard deviation ranged were 2.9%-8.5%. Using the developed method, five BPs were detected in Luoma Lake and four BPs were detected in inflow rivers. BPA and BPF were the predominant BPs, and the concentration of BPA was the highest. The method was proved to be sensitive, accurate and efficient, and it was suitable for qualitative and quantitative analysis of seven BPs in surface water.
求助全文
通过发布文献求助,成功后即可免费获取论文全文。 去求助
来源期刊
自引率
0.00%
发文量
0
×
引用
GB/T 7714-2015
复制
MLA
复制
APA
复制
导出至
BibTeX EndNote RefMan NoteFirst NoteExpress
×
提示
您的信息不完整,为了账户安全,请先补充。
现在去补充
×
提示
您因"违规操作"
具体请查看互助需知
我知道了
×
提示
确定
请完成安全验证×
copy
已复制链接
快去分享给好友吧!
我知道了
右上角分享
点击右上角分享
0
联系我们:info@booksci.cn Book学术提供免费学术资源搜索服务,方便国内外学者检索中英文文献。致力于提供最便捷和优质的服务体验。 Copyright © 2023 布克学术 All rights reserved.
京ICP备2023020795号-1
ghs 京公网安备 11010802042870号
Book学术文献互助
Book学术文献互助群
群 号:481959085
Book学术官方微信