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

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

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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