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液相色谱质谱法测定水体及土壤中的类固醇激素
引用本文:王坤,方敏,吴辰熙,宁增平,万赟. 液相色谱质谱法测定水体及土壤中的类固醇激素[J]. 地球与环境, 2015, 43(3): 369-374
作者姓名:王坤  方敏  吴辰熙  宁增平  万赟
作者单位:1. 中煤平朔集团有限公司,山西朔州,036006
2. 中国科学院水生生物研究所,武汉,430072
3. 中国科学院地球化学研究所,贵阳,550002
基金项目:国家自然科学基金项目(41103064);国家水体污染控制与治理科技重大专项(2012ZX07104002)
摘    要:
建立了水体和土壤中类固醇激素的液相色谱质谱分析方法。水样采用固相萃取方法富集,土壤样经加速溶剂萃取后由固相萃取净化和富集。处理好的样品经丹磺酰衍生化后上仪器分析。结果表明,类固醇激素在水体和土壤中的检出限分别为0.01~0.6ng/L和0.01~0.19ng/g,回收率分别为77%~97%和62%~119%,RSD小于6.04%和15.5%。该方法具有较高的准确度和精密度,适用于环境水体及土壤中类固醇激素残留的分析。

关 键 词:类固醇激素  液相色谱质谱  衍生化  固相萃取  加速溶剂萃取
收稿时间:2014-06-23
修稿时间:2014-08-13

Analysis of Steroid Hormones in Water and Soil Using Liquid Chromatography Mass Spectrometry
WANG Kun,FANG Min,WU Chenxi,NING Zengping,WAN Yun. Analysis of Steroid Hormones in Water and Soil Using Liquid Chromatography Mass Spectrometry[J]. Earth and Environment, 2015, 43(3): 369-374
Authors:WANG Kun  FANG Min  WU Chenxi  NING Zengping  WAN Yun
Affiliation:WANG Kun;FANG Min;WU Chenxi;NING Zengping;WAN Yun;China coal Pingshuo Corporation,Shuonan Development and Construction Headquarters;Institute of Hydrobiology,Chinese Academy of Sciences;Institute of Geochemistry,Chinese Academy of Sciences;
Abstract:
Method for the analysis of steroid hormones in water and soil using liquid chromatography mass spectrometry (LC-MS) was established. Water samples were concentrated using solid phase extraction (SPE) while soil samples were first extracted using accelerated solvent extraction (ASE) and then purified and concentrated using SPE. Results show that the method detection limits were 0.01-0.6 ng/L and 0.01-0.19 ng/g, the recoveries were 77%-97% and 62%-119%,and the RSD are lower than 6.04% and 15.5%, respectively for the analysis of steroid hormones in water and soil. This method is accurate and precise and suitable for determining the residues of steroid hormones in water and soil.
Keywords:steroid hormone  LC-MS/MS  derivatization  solid phase extraction  accelerated solvent extraction
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