一体化固相萃取—GC/ECD测定水中有机氯农药  

Determination of Organochlorine Pesticides in Water Using Integrated Solid Phase Extraction Coupled with GC-ECD

作　　者：吴海兵[1] 曾鸿鹄[1,2] 梁延鹏[1,2] 莫凌云[1] 

机构地区：[1]桂林理工大学广西矿冶与环境科学实验中心,广西桂林541004 [2]广西危险废物处置产业化人才小高地,广西桂林541004

出　　处：《工业安全与环保》2014年第12期4-7,共4页Industrial Safety and Environmental Protection

基　　金：国家自然科学基金(51268008;21207024);教育部科学技术研究重点项目(教技司[2010]114号;编号210170);广西高校优秀人才资助计划项目(桂教人[2010]65号)

摘　　要：建立了采用一体化固相萃取提取和净化、GC－MS／GC－ECD联合定性定量同时检测水中14种有机氯农药的方法，优化了固相萃取和色谱条件。样品于一体化固相萃取仪上以10 mL／min流速经C18柱富集、6 mL体积比为1∶1的二氯甲烷／乙酸乙酯混合溶剂洗脱、氮吹浓缩后，GC－MS／GC－ECD分离检测。结果表明，14种OCPs在1．00～500μg／L范围内线性良好，方法检出限为1．76～15．10ng／L，平均加标回收率为69．6％～102．8％，RSD为1．62％～18．9％。实际样品分析表明该方法灵敏度和精密度高、准确性好、操作简便，适用于大批量水样中微量和痕量OCPs的测定。We developed an integrated method that combined solid -phase extraction and purification, GC -MS/GC -ECD for qualitative and quantitative determining 14 organochlorine pesticides in water. The solid -phase extraction and chromatography condition were optimized. The sample was extracted on the integrated method with 10 mL/min velocity by C18 column enrichment, eluted by 6 mL mixed solution of dichloromethane/ethyl acetate with the volume ratit of 1∶1 and concentrated by nitrogen, and was separated and detected by GC-MS/GC-ECD. The results indicate that 14 OCPs show a good linearity in the range of 1. 00-500μg/L. The detection limit was 1. 76-15. 10 ng/L, the average recovery was 69. 6%-102. 8%, RSD was 1. 62% -18. 9%. The analysis of actual samples demonstrate that this method shows high sensitivity and precision, good accuracy, simple operation, and suitable for determination of trace and ultra-trace OCPs in water samples.

关 键 词：一体化固相萃取 有机氯农药 

分 类 号：X832[环境科学与工程—环境工程]