池塘底泥中合成激素的气相色谱-质谱测定

Determination of Synthetic Hormone in Sediment by Gas Chromatography-Mass Spectrometry

应用气相色谱-质谱联用技术，建立了底泥中合成激素炔雌醇、左炔诺孕酮和炔诺酮的分析方法，优化了前处理条件。样品经超声提取、层析净化、衍生化后，用气相色谱-质谱进行定性和定量分析。3种合成激素在0．5—40mg／L的质量浓度范围内具有良好的线性，检出限分别为炔雌醇0．8μg／kg、左炔诺孕酮0．6μg／kg和炔诺酮0．9μg／kg，加标回收率在68％～99％之间，相对标准偏差在1．7％-5．4％之间。

In this study, the synthetic hormones such as 17α-ethinylestriadiol, levonorgestrel and norethisterone in sediment were determined by gas chromatography -mass spectrometry （GC -MS）. The method consisted of solvent extraction, column cleanup, derivatization, and finally, detection by GC -MS. The results showed that the method could be employed to determine the synthetic hormone in pond sediment. The linear range was 0.5 -40 mg/L and the dete.ction limits were 0.8 μg/kg for 17α-ethinylestriadiol, 0.6 μg/kg for levonorgestrel and 0. 9μg/kg for norethisterone, respectively. The mean recoveries of three hormones ranged from 68% -99% and their relative standard deviations （RSD） were less than 5.4% .