色谱2012，Vol.30Issue(7)：665-671,7.DOI:10.3724/SP.J.1123.2012.02028
分散固相萃取-超快速液相色谱-串联质谱法测定牛蛙全血中6种酚类环境雌激素
Analysis of six phenolic environmental estrogens in bullfrog blood by using dispersive solid-phase extraction and ultrafast liquid chromatographytandem mass spectrometry
摘要
Abstract
A rapid, sensitive and accurate method for the simultaneous determination of six phenolic environmental estrogens, i. e. , bisphenol A ( BPA), dtethylstilbestrol ( DES ), dienestrol(DE) , hexestrol (HEX), 4-( tert-octyl)-phenol (4-tOP) and 4-nonylphenol (4-NP) in bullfrog blood by dispersive solid-phase extraction-ultrafast liquid chromatography-tandem mass spectrometry ( dSPE-UFLC-MS/MS) was established. After protein precipitation, bullfrog blood samples were cleaned-up by dSPE method with ethylenediamine-functionalized Fe3O4 magnetic polymers (EDA-MPs) as adsorbent. The effects of precipitation solvents, adsorption time and the amount of EDA-MPs used on the recoveries of six phenolic environmental estrogens were investigated in detail. Chromatographic separation was performed on a Shim-pack XR-ODS II analytical column (100 mm x2. 0 mm, 2..2μm). The mass spectrometer was operated by using electrospray ion (ESI) source in the multiple reaction monitoring (MRM) mode. The results showed that the linearities were in the range of 0. 5 - 100. 0 |xg/L with correlation coefficients (r2) not less than 0. 999 6 for all the six phenolic environmental estrogens. The limits of quantification (LOQs) (S/N > 10) in bullfrog blood samples were between 0.075μg/L and 0.40μg/L. The recoveries were between 95.0% and 110.0% at three spiked levels. The precision values expressed as relative standard deviations (RSDs) were in the range of 0. 6% -6. 3%. The developed method can be applied to the routine analysis of the six phenolic environmental estrogens in bullfrog blood samples.关键词
分散固相萃取/超快速液相色谱-串联质谱法/多反应监测/氨基功能化Fe3O4磁性高分子复合微粒/酚类环境雌激素/全血Key words
dispersive solid-phase extraction (dSPE)/ultrafast liquid chromatography-tandem mass spectrometry ( UFLC-MS/MS)/multiple reaction monitoring ( MRM)/ethylenediaminefunctionalized Fe,O4 magnetic polymers (EDA-MPs)/phenolic environmental estrogens/blood分类
化学化工引用本文复制引用
赵永纲,陈晓红,姚珊珊,李小平,金米聪..分散固相萃取-超快速液相色谱-串联质谱法测定牛蛙全血中6种酚类环境雌激素[J].色谱,2012,30(7):665-671,7.基金项目
宁波市农业与社会发展项目(2011C50058)、浙江省公益性技术应用研究计划项目(201207002)、浙江省自然科学基金项目(LY12H26003)、浙江省医药卫生平台研究计划骨干人才项目(2011RCB033)和宁波市农业与社会发展重大(重点)择优委托项目(2011C11021). （2011C50058）
