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作 者:陈砚朦[1] 钟淑婷[1] 甘凤娟[1] 韩媛媛[1] 肖湖[1] 周明灿[1] 张少彬[1]
机构地区:[1]广东省东莞市疾病预防控制中心,广东东莞523000
出 处:《中国卫生检验杂志》2008年第12期2463-2466,共4页Chinese Journal of Health Laboratory Technology
摘 要:目的:建立检测生活饮用水中2,4-滴、2,4,6-三氯酚和五氯酚的超高效液相色谱/串联质谱法(UPLC-MS/MS)。方法:水样经高速离心,Waters ACQUITY UPLC BEHC181.0×50 mm柱分离,以纯水和乙腈为流动相,采用UPLC-ESI-MS/MS法,以负离子检测方式,多离子反应监测(MRM)定量法检测生活饮用水中2,4-滴、2,4,6-三氯酚和五氯酚。结果:经方法学验证,该方法对2,4-滴、2,4,6-三氯酚和五氯酚的最低检测限分别为0.5、3.0、1.0μg/L(进样量10μl)。在线性范围中,相关系数r均大于0.99,平均回收率分别在85%~115%之间。结论:方法快速、灵敏度高、操作简单、定量准确、测定浓度范围宽阔,是生活饮用水样品中2,4-滴、2,4,6-三氯酚和五氯酚含量快速检测的理想方法。对东莞市生活饮用水样品检测表明:此水体中2,4-滴、2,4,6-三氯酚和五氯酚的含量都低于检测限。Objective:A UPLC-MS/MS method was developed for the determination of 2,4-D,2,4,6-trichlorophenol and Pentachlorophenol in drinking water.Methods:After centrifugation,determined by UPLC-ESI(-)-MS/MS,quantified with multiple reaction monitoring(MRM) mode,performed on a Waters ACQUITY UPLC BEH C18 1.0×50 mm column,water and acetonitrile was used as mobile phase.Results:The detection limits(LOD) for2,4-D,2,4,6-trichlorophenol and pentachlorophenol were 0.5,3.0,1.0 μg/L.In the linear ranges,correlation coefficients was above 0.99.The mean recoveries were between 85% and 115%.Conclusion:By coupling the ACQUITY UPLC with Quattro PremierTMXE,a rapid and sensitive method has been developed for the trace level quantitation and confirmation of 2,4-D,2,4,6-trichlorophenol and PCP in drinking water for its excellent sensitivity and selectivity.
关 键 词:超高效液相色谱-电喷雾串联四极杆质谱 多离子反应监测(MRM) 2 4-滴 2 4 6-三氯酚 五氯酚
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