引用本文:孙娟,何青青,徐荣,宋祖华.水环境中26种类固醇激素的分析方法研究[J].环境监控与预警,2019,11(6):18-23
SUN Juan,HE Qing-qing,XU Rong,SONG Zu-hua.Research on the Analysis Method of 26 Steroid Hormones in Water Environment[J].Environmental Monitoring and Forewarning,2019,11(6):18-23
【打印本页】   【HTML】   【下载PDF全文】   查看/发表评论  【EndNote】   【RefMan】   【BibTex】
←前一篇|后一篇→ 过刊浏览    高级检索
本文已被:浏览 26次   下载 5 本文二维码信息
码上扫一扫!
分享到: 微信 更多
水环境中26种类固醇激素的分析方法研究
孙娟,何青青,徐荣,宋祖华
江苏省南京环境监测中心,江苏 南京 210013
摘要:
建立了固相萃取-超高效液相-串联质谱法同时测定水环境中26种类固醇激素的分析方法。明确了取样体积为500 mL,Cleanert PEP为富集柱,乙酸乙酯为洗脱剂,甲醇为溶剂进行提取操作。选择了正离子模式,以0.1%甲酸/甲醇-水为流动相,负离子模式以0.1%氨水/乙腈-水为流动相,试样经AcquityTMUPLC BEH C18色谱柱分离后,选用质谱检测模式进行定性、定量分析。通过方法验证,26种类固醇激素的方法检出限为0.3~1.5 ng/L,测定下限为1.2~6.0 ng/L,代表性样品测定结果的相对标准偏差为2.6%~13.7%(n=6),加标回收率为71.2%~121%。该方法操作便捷,灵敏度高,精密度和准确度良好,可适用于水环境中多种痕量、超痕量类固醇激素的定性定量分析。
关键词:  水环境  类固醇激素  固相萃取  超高效液相色谱  串联质谱
DOI:
分类号:X832; O657.63
文献标识码:B
基金项目:2018年南京环保科研基金资助项目(201801)
Research on the Analysis Method of 26 Steroid Hormones in Water Environment
SUN Juan,HE Qing-qing,XU Rong,SONG Zu-hua
Jiangsu Nanjing Environmental Monitoring Center,Nanjing,Jiangsu 210013,China
Abstract:
In this paper,an analytical method was developed for simultaneous determination of 26 kinds of steroid hormones in water environment by solid phase extraction-ultra performance liquid chromatography-triple quadrupole mass spectrometry. A 500 mL sample was extracted by passing it through a Cleanert PEP column, target analytes were eluted from the SPE column by ethyl acetate. A solvent exchange is necessary to avoid incompatible with solid phase, so methanol was used as the final solvent. The target analytes were separated by AcquityTMUPLC BEH C18 chromatographic column and the matched mass spectrometry detection mode was selected for qualitative and quantitative analysis.Positive ion mode was selected with methanol-water as mobile phase and negative ion mode with acetonitrile-water as mobile phase.Method validation results showed that the detection limits of 26 kinds of steroid hormones were between 0.3~1.5 ng/L, the lower limits were between 1.2~6.0 ng/L, the relative standard deviations of representative samples were between 2.6%~13.7% (n=6), and the standard recovery rates were between 71.2%~121%. The results indicated that this method was convenient, sensitive, precise and accurate. So it could be used for qualitative and quantitative analysis of steroid hormones in water environment.
Key words:  Water environment  Steroid hormones  Solid phase extraction  Ultra performance liquid chromatography  Tandem mass spectrometry