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目的建立测定饮用水中双酚A(BPA)和壬基酚(NP)的在线固相萃取-液质联用法(On-line SPE LC-MS/MS)。方法水样经On-line SPE在线富集和净化,以甲醇-水为在线固相萃取流动相,流速2.0ml/min,采用沃特世Direct Connect HP XBridgeTMC18在线固相萃取柱(填料粒径10μm)进行在线固相萃取。以甲醇-0.1%氨水为分析流动相,流速0.4ml/min,采用沃特世UPLC BEH C18色谱柱进行分析。质谱检测器采用电喷雾电离源,以多反应监测(MRM)方式进行负离子监测,采用内标法对饮用水中的BPA和NP进行定量分析。结果该方法每个样品总耗时10min。BPA线性范围为5～1000ng/L,NP为10～5000ng/L,相关系数(r2>0.999)。BPA、NP的定量限(LOQ)分别为5和10ng/L,两种内分泌干扰物在3个加标水平下平均回收率为86.6%～105%,相对标准偏差3.11%～18.2%,日间精密度11.3%～13.2%。结论该方法实现了样品的自动化前处理,提高了分析效率,操作简单,灵敏度高,可用于饮用水中两种环境内分泌干扰物的痕量检测。
Abstract：Objective To develop a method for bisphenol A(BPA) and nonylphenol(NP) analysis in drinking water by on-line solid phase extraction(SPE) column switching liquid chromatography tandem mass spectrometry.Method Target compounds were concentrated and purified by a Waters Direct Connect HP XBridgeTM C18 column,with average particle size 10μm.The mobile phase of SPE extraction column was methanol/water at a flow-rate of 2.0ml/min.The analytical column was Waters BEH C18 column(2.1mm×50mm,1.7μm) and the mobile phase was methanol/0.1% ammonia water at a flow-rate of 0.4ml/min.BPA and NP were analyzed by liquid chromatography-electrospray ionization tandem mass spectrometry(LC-ESI-MS/MS) in the negative ion mode with multiple reactions monitoring(MRM).Results The whole run time of an individual sample was about 10 min.The linear calibration curves covered the range of 5-1000ng/L and 10-5000ng/L for BPA and NP,respectively,while the correlation coefficients(r2) were above 0.999.The quantification limits of the method were 5 and 10ng/L for BPA and NP,respectively.Recovery test was performed at three fortification levels,mean recoveries ranged from 86.6% to 105% with acceptable coefficients of variation(3.11%-18.2%,n=6).The inter-day precisions were less than 13.2%.Conclusion The established On-line SPE LC-MS/MS method needs no complicated sample pretreatment step,which is significantly time-saving.The analytical procedure is rapid,simple,and high-sensitive.It can be applied to analysis BPA and NP in drinking water.
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基本信息:
DOI：10.19813/j.cnki.weishengyanjiu.2013.01.030
中图分类号:R123.1;O657.72
引用信息:
[1]杨蕴嘉,牛宇敏,杨奕,等.在线固相萃取-液相色谱串联质谱法测定饮用水中的双酚A和壬基酚[J].卫生研究,2013,42(01):127-132.DOI:10.19813/j.cnki.weishengyanjiu.2013.01.030.
基金信息:
十二五国家科技支撑计划课题(No.2011BAK11B06); 北京市卫生系统高层次卫生技术人才培养计划项目
2013-01-30
2013-01-30