饮用水中多氯联苯的固相萃取-同位素内标法气相色谱/三重四级杆质谱测定法被引量：1

Determination of polychlorinated biphenyls in drinking water by gas chromatography coupled with triple quadrupole mass spectrometry using isotope internal standards after solid phase extration

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摘要目的建立一种同时测定饮用水中15种多氯联苯(PCBs)的固相萃取-同位素内标法气相色谱/三重四极杆质谱联用(GC-MS/MS)方法。方法采用盐酸调节水样pH值为3,以5 ml/min的流速经C_(18)固相萃取柱富集,7 ml丙酮和5 ml乙腈洗脱,氮吹蒸发浓缩后,正己烷定容至1.0 ml。采用EI源,在多反应监测(MRM)模式下测定,^(13)C同位素内标法定量。结果 15种PCBs 50~1 000 ng/L范围内具有良好的线性关(r>0.994),方法的检出限为0.004~0.010μg/L。在0.1和0.5μg/L2种水平下的加标回收率为75.3%~118.5%,相对标准偏差为1.8%~15.1%。结论该方法通过固相萃取富集,气相色谱三重四极杆质谱多反应监测法检测,水样处理简单,快速,可靠。通过每种氯代PCBs都采用一种^(13)C同位素内标,减少了基质干扰,使目标物得到较好的分离,提高了灵敏度,增强了定性、定量的准确度。可用于生活饮用水中15种PCBs的测定。 [Objective]To develop a method for simultaneous determination of 15 polychlorinated biphenyls（PCBs）in drinking water by gas chromatography-triple quadrupole mass spectrometry（GC-MS/MS）using isotope internal standards after solid phase extraction.[Methods]The water samples were extracted under p H =3 and flow rate of 5 ml/min by a C_（18）solid-phase extraction column,eluted by 7 ml acetone and 5 ml acetonitrile. The eluent was treated by nitrogen blowing until nearly dry and the solvent exchanged with hexane as 1.0 ml.The target compounds were determined in multiple monitoring（MRM）mode and quantified by the ^13C internal standards.[Results]The method showed good linearity in the range of 50.0-1 000.0 ng/L（r0.994）.The limits of detection were 0.004-0.010 μg/L. The average recoveries were 75.3%-118.5% at the addition mass concentration of 0.1 0.5μg/L and 0.5μg/L.The relative standard derivations were 1.8%-15.1%.[Conclusion]The method for determination of PCBs in drinking water by gas chromatography-triple quadrupole mass spectrometry after solid phase extraction is rapid,simple and reliable. The method uses^13C PCBs as internal standards to reduce the background interference,effectively separate the target compounds,and improve the sensitivity and accuracy. It is suitable for determination of 15 PCBs in drinking water.

作者代澎张晓妍 DAI Peng ZHANG Xiao-yan(Physicochemical Section, Shenyang Center for Disease Control and Prevention, Shenyang Liaoning, 110031, China Monitoring Department ,Liaoning Center far Nuclear and Radiation Monitoring,Shenyang Liaoning, 110161, China)

机构地区沈阳市疾病预防控制中心理化科辽宁省核与辐射监测中心监测科

出处《职业与健康》 CAS 2016年第21期2929-2932,共4页 Occupation and Health

关键词多氯联苯三重四极杆气相色谱质谱法固相萃取同位素内标生活饮用水 Polychlorinated biphenyls（PCBs） Gas chromatography triple quadrupole mass spectrometry Solid phase extraction ^13C internal standards Drinking water

分类号 R115 [医药卫生—公共卫生与预防医学]