固相萃取-超高效液相色谱-串联质谱法同时测定地表水中9种性激素

建立了地表水中9种性激素的固相萃取-超高效液相色谱-串联质谱检测方法。利用HLB固相萃取柱富集水体中痕量性激素,用甲醇洗脱并浓缩,再以1 mmol/L氟化铵-乙腈为流动相,经C_(18)柱分离,采用电喷雾离子源、质谱多反应监测模式,内标法定量,实现了地表水中9种性激素的同时检测。方法检出限为0. 1～1. 8 ng/L,在低、中、高3个加标水平下,性激素的平均回收率为69. 6%～115. 0%,相对标准偏差为3. 2%～17. 7%。该方法灵敏度高,定性准确,操作简单高效,适用于地表水中9种性激素的定性定量分析。

Simultaneous Determination of 9 Hormones in Surface Water by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with Solid-Phase Extraction

An analytical method was developed for simultaneous determination of 9 hormones in surface water samples by solid-phase extraction and ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS). The sample was enriched by Oasis HLB solid phase extraction cartridge, extracted with methanol and concentrated by nitrogen. After chromatographic separation on an C₁₈ column with 1 mmol/L NH₄F aqueous-acetonitrile as the mobile phase, the target compounds were analyzed under the multiple reaction monitoring(MRM) mode and quantitated by internal standard method. The limits of detection for 9 hormones were in the range of 0.1-1.8 ng/L. The mean recoveries at three spiked levels ranged from 69.6% to 115.0%, with relative standard deviations of 3.2%-17.7%. The method was proved to be sensitive, accurate and efficient, and it was suitable for qualitative and quantitative analysis of 9 hormones in surface water.