摘要
目的:建立一种快速、灵敏、准确的牛蛙全血样品中双酚A、4-叔辛基酚和4-壬基酚的超快速液相色谱-串联质谱(UFLC-MS/MS)测定方法。方法:牛蛙全血样品采用蛋白质沉淀法进行净化处理,在Shim-pack XR-ODSⅡ(100 mm×2.0 mm i.d.,2.2μm)反相液相色谱柱上进行分离,采用电喷雾离子源(ESI)以高纯氮气(>99.999%)为碰撞气在多反应监测(MRM)模式下进行检测。结果:3种酚类环境雌激素在0.5μg/L～100.0μg/L范围内具有良好的线性(R2>0.999),检出限在0.07μg/L～0.15μg/L范围,最低定量限在0.20μg/L～0.46μg/L范围,RSDs在3.9%～8.2%范围;在加标水平为1.0μg/L、10.0μg/L和50.0μg/L时,3种酚类环境雌激素在牛蛙全血中的回收率分别在97%～106%、93%～109%、94%～96%范围。结论:本方法可用于牛蛙全血样品中酚类环境雌激素的测定。
Objective：To develop a rapid,sensitive and accurate method for the simultaneous determination of 3 trace phenolic environmental estrogens： BPA,4-tOP,4-NP,in bullfrog blood by ultrafast liquid chromatography-tandem mass spectrometry（UFLC-MS/MS）.Methods： Bullfrog blood samples were extracted by protein precipitation method.Chromatographic separation was performed on a Shim-pack XR-ODSⅡanalytical column（100 mm×2.0 mm i.d.,2.2 μm）.The QqQ mass spectrometer was operated by using electrospray ion source（ESI） in the multiple reaction monitoring（MRM） mode.Results： Linearities were in the range of 0.5 μg/L^100.0 μg/L with determination coefficients（R2） higher than 0.999 for all 3 phenolic environmental estrogens.The limits of detection（LODs） for phenolic environmental estrogens were in the range of 0.07 μg/L^0.15 μg/L and the limit of quantification（LOQs） in bullfrog blood samples were between 0.20 μg/L^0.46 μg/L.The relative standard deviations（RSDs） were in the range of 3.9%~8.2%.Recoveries were between 97%~106% at 1.0 μg/L,93%~109% at 10.0 μg/L and 94%~96% at 50.0 μg/L,respectively.Conclusion： The method can be applied to the routine analyses for the determination of the 3 phenolic environmental estrogens in bullfrog blood samples.
出处
《中国卫生检验杂志》
北大核心
2012年第9期2007-2010,共4页
Chinese Journal of Health Laboratory Technology
基金
宁波市农业与社会发展项目(2011C50058)
宁波市自然科学基金(2010A610010)
浙江省医药卫生平台研究计划骨干人才项目(2011RCB033)
宁波市农业与社会发展重点择优委托项目(2011C11021)
