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猪粪中典型类固醇雌激素的固相萃取/GC-MS检测
引用本文:刘 敏,岳 波,尹平河,黄泽春,王 琪,黄启飞,何 洁.猪粪中典型类固醇雌激素的固相萃取/GC-MS检测[J].环境科学研究,2011,24(7):763-768.
作者姓名:刘 敏  岳 波  尹平河  黄泽春  王 琪  黄启飞  何 洁
作者单位:1.暨南大学化学系, 广东 广州 510632;中国环境科学研究院固体废物污染控制技术研究所, 北京 100012
基金项目:国家环保公益性行业科研专项
摘    要:以猪粪中常见且具有较大潜在危害的E1(雌酮),17α-E2(17α-雌二醇),17β-E2(17β-雌二醇)和E3(雌三醇)为研究对象,建立了猪粪中这4种典型类固醇雌激素的GC-MS(气相色谱-质谱)分析检测方法.着重优化了样品的前处理方法,包括对超声提取剂、超声提取时间、固相萃取淋洗剂、衍生化温度和时间的优化选择.结果表明:在优化的试验条件下,猪粪中的典型雌激素E1,17α-E2,17β-E2和E3检出限分别为8.0,2.5,5.1和3.3 μg/kg,平均加标回收率在92.3%~137.4%之间. 

关 键 词:猪粪    雌激素    超声提取    固相萃取    衍生化    GC-MS
收稿时间:2010/10/17 0:00:00
修稿时间:2011/1/7 0:00:00

Analysis of Typical Steroid Estrogens in Pig Manure by Solid Phase Extraction/GC-MS
LIU Min,YUE Bo,YIN Ping-he,HUANG Ze-chun,WANG Qi,HUANG Qi-fei and HE Jie.Analysis of Typical Steroid Estrogens in Pig Manure by Solid Phase Extraction/GC-MS[J].Research of Environmental Sciences,2011,24(7):763-768.
Authors:LIU Min  YUE Bo  YIN Ping-he  HUANG Ze-chun  WANG Qi  HUANG Qi-fei and HE Jie
Institution:1.Department of Chemistry,Jinan University,Guangzhou 510632,China 2.Research Institute of Solid Waste Management,Chinese Research Academy of Environmental Sciences,Beijing 100012,China
Abstract:Great potential harm from livestock manure is commonly found in estrone(E1),17α-E2(17α-estradiol),17β-E2(17β-estradiol) and E3(estriol).Gas chromatography/mass spectrometry(GC-MS) method was developed for the analysis and quantification of the four typical steroid estrogens in pig manure samples.The pre-treatment method was carefully optimized,including the options for the ultrasonic extraction solvent,extraction time,solid phase extraction eluent,derivatization temperature and time.The results showed that the detection limits for E1,17α-E2,17β-E2 and E3 in pig manure were 8.0,2.5,5.1 and 3.3 μg/kg under the optimal experimental conditions.The average spiked recoveries were in the range of 92.3% to 137.4%.
Keywords:pig manure  estrogens  ultrasonic extraction  solid phase extraction  derivatization  GC-MS
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