固相萃取-毛细管气相色谱法测定生活饮用水中16种硝基苯类化合物  

Simultaneous Determination of 16 Nitrobenzene Compounds in Drinking Water by Solid Phase Extraction-Gas Chromatography coupled with Electron Capture Detection

作　　者：邹海民[1] 周琛[2] 余辉菊[1] 张潜[1] 曾红燕[2] 李永新[2] 

机构地区：[1]成都市疾病预防控制中心,成都610047 [2]四川大学华西公共卫生学院,成都610041

出　　处：《分析化学》2016年第2期297-304,共8页Chinese Journal of Analytical Chemistry

基　　金：四川省科技支撑计划基金(No.2012SZ0196)资助项目~~

摘　　要：建立了生活饮用水中16种硝基苯类物质的固相萃取-毛细管气相色谱-电子捕获检测方法。实验优化了色谱柱、升温程序等色谱条件,并对影响固相萃取效果的主要因素（萃取小柱、洗脱剂和洗脱体积）进行了考察。水样中16种硝基苯类物质经Oasis HLB固相萃取柱吸附、正己烷-丙酮（3∶1,V/V）洗脱后,采用DB-1701毛细管气相色谱柱程序升温分离、ECD检测,在33 min内完成所有待测组分的测定。16种硝基苯类组分在各自的线性范围内相关系数r≥0.998,方法的检出限为0.01~0.77μg/L（S/N=3）,定量限为0.03~2.57μg/L（S/N=10）,日内精度和日间精度分别在1.0%~3.8%和2.3%~4.8%间,样品加标回收率为83.6%~111.8%,加标样品的RSD为1.2%~5.1%。应用本方法对50份水样进行了分析,结果表明,本方法准确、灵敏、快速,适用于水质的常规分析,可为水样中硝基苯类物质的污染评价提供技术支持。A solid phase extraction （SPE）-gas chromatography coupled with electron capture detection （GC- ECD） method was developed for the simultaneous determination of 16 nitrobenzene compounds in drinking water. The chromatographic conditions, i.e. the chromatographic column and the programmed temperature, were optimized, and the extraction conditions, i.e. the type of extraction column, elution solvent and volume of elution solvent, were also optimized. Water samples were extracted with Oasis HLB columns and eluted by the mixture of n-hexane and acetone （3： 1, V/V）. All the target compounds were chromatographically separated on a DB-1701 capillary column with programed temperature, and were detected by electron capture detector. The favorable resolutions of all target compounds were achieved within 33 min. Under the optimal analytical conditions, the peak area of each analyte and its concentration had a good correlation within the linear range （ r≥0. 998 ）. The limit of detection （LOD） and limit of quantification （LOQ） of the method were 0.01-0.77 μg/L （S/N=3） and 0.03-2.57 μg/L （S/N= 10）, respectively. The intra- and inter-day relative standard deviations （RSDs） of the sample were 1.0% -3.8% and 2.3% -4.8% , respectively. Spiked recoveries of the analytes were 83.6% -111.8% and the RSDs of the spiked samples were 1.2% - 5.1%. This proposed method has been applied in the detection of 50 water samples. The results indicated that the new solid phase extraction -gas chromatography coupled with electron capture detection method was specific, sensitive and reproducible, and could be used for the determination of 16 nitrobenzene compounds in drinking water

关 键 词：气相色谱法 固相萃取 硝基苯类 饮用水 

分 类 号：R123.1[医药卫生—环境卫生学] O657.71[医药卫生—公共卫生与预防医学]