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环境化学  2015 

高效液相色谱串联大气压化学电离源质谱(HPLC-APCI-MS)法测定水中三氯生

Keywords: 三氯生,液液萃取,HPLC-APCI-MS,QA/QC

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Abstract:

建立了高效液相色谱串联大气压化学电离源质谱(HPLC-APCI-MS)测定水中三氯生的方法,预处理采用正己烷液液萃取法萃取三氯生,回收率达99.6%;优化的色谱质谱联机分析条件为检测波长230nm,流动相乙腈/水(75∶25),离子源APCI源,负离子模式;该分析方法能在5min内实现对水中三氯生的定性与定量分析.质量保证(QualityAssurance,QA)与质量控制(QualityControl,QC)研究得出,仪器检测限为0.18μg·L-1,相对标准偏差(relativestandarddeviations,RSD)为0.59%;空白加标实验回收率为103%,RSD为1.2%;以城市生活污水、河水和自来水为加标基质实验回收率为96.6%—108%,方法检测限为0.26—0.61μg·L-1,RSD为0.28%—0.81%.该方法操作简便,分析方法准确性、精密性与可靠性均较高.

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