%0 Journal Article %T 水环境中26种类固醇激素的分析方法研究 %T Research on the Analysis Method of 26 Steroid Hormones in Water Environment %A 孙娟,何青青,徐荣,宋祖华 %A SUN,Juan %A HE,Qing qing %A XU,Rong %A SONG,Zu hua %J 环境监控与预警 %@ 1674-6732 %V 11 %N 6 %D 2019 %P 18-23 %K 水环境;类固醇激素;固相萃取;超高效液相色谱;串联质谱 %K Water environment; Steroid hormones;Solid phase extraction;Ultra performance liquid chromatography; Tandem mass spectrometry %X 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。 %X 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. %R %U http://www.hjjkyyj.com/hjjkyyj/ch/reader/view_abstract.aspx %1 JIS Version 3.0.0