水环境中26种类固醇激素的分析方法研究

Research on the Analysis Method of 26 Steroid Hormones in Water Environment

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。

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.