作　　者： ; ; ;

机构地区： 华南理工大学环境科学与工程学院工业聚集区污染控制与生态修复教育部重点实验室

出　　处： 《环境化学》 2012年第6期909-914,共6页

摘　　要： 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230 nm,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5 min内实现对水中三氯生的定性与定量分析.质量保证(Quality Assurance,QA)与质量控制(Quality Control,QC)研究得出,仪器检测限为0.18μg·L-1,相对标准偏差(relative standard deviations,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. In this paper, the method ior triclosan determination in water by high periormance hquid chromatography and mass spectrometry with atmospheric pressure chemical ionization （HPLC-APCI-MS） was established. Triclosan was extracted from the sample by hexane, then the concentrated extract was determined by HPLCAPCI-MS, and the recovery rate was about 99.6%. The optimum conditions for triclosan determination were as follows. The detection wavelength was 230 nm, the mobile phase was 75/25 （V/V） MeCN,（H20 and the ion source was APCI （-）. Under such conditions, triclosan was separated and determined ：accurately in 5 minutes. The Quality Asaurance and Quality Control （QA/QC） studies were conducted and .the results showed that the instrument detection limits （IDL） of HPLC-MS for triclosan determination was 0.18 μg. L-1 , and the relative standard deviations （RSD） was 0.59%. In the spiked blank experiments, the recovery rate reached 103%, and RSD was 1.2%. Moreover, the sanitary sewage, river water and drinking water were used as spiking matrix, the recovery rate was 96.6%-108% the method detection limits （MDL） was 0. 26-0.61μg.L-1 and RSD was 0.28%-0.81%. The results showed this method had good accuracy, precision and reproducibility.

关 键 词： 三氯生 液液萃取

领　　域： [环境科学与工程]