顶空固相微萃取-气相色谱法测定水中5种农药残留量  

GC Determination of Residual Amounts of 5 Pesticides in Water with Headspace Solid-Phase Microextraction

作　　者：陈烨[1] 刀谞[1] 谭丽[1] 许秀艳[1] 吕怡兵[1] 

机构地区：[1]中国环境监测总站,北京100012

出　　处：《理化检验（化学分册）》2015年第8期1174-1177,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家高技术研究发展计划(863计划)(2013AA06A308)

摘　　要：采用顶空固相微萃取-气相色谱法测定水中三乙基硫代磷酸酯、阿特拉津、甲基对硫磷、对硫磷和脱叶磷等5种农药残留量。优化的试验条件如下：①聚丙烯酸酯萃取纤维头；②萃取温度为80℃；③萃取时间为40min；④解吸时间为5min。用DB-35MS色谱柱（30m×0．32mm，0．25μm）分离，氮磷检测器检测。5种农药在一定的质量浓度范围内与其峰面积呈线性关系，方法的检出限（3S／N）在0．05～1．0μg·L-1之间。方法用于水库水样分析，加标回收率在37．0％～107％之间，测定值的相对标准偏差（n=5）在1．6％～25．0％之间。GC was applied to the determination of residual amounts of 5 pesticides, i. e. triethyl thiophosphate, atrazine, methyl parathion, parathion and tribufos in water with headspace solid phase microextraction. The optimized conditions found were as follows： ①extraction fiber type： polyacrylate; ② extraction temperature： 80℃ ; ③ extraction time： 40 minl @ desorption time： 5 min. The analytes were separated on DB-35MS column （30 m× 0. 32 mm, 0. 25 μm） and detected by NPD. Linear relationships between values of peak area and mass concentration of the 5 pesticides were kept in definite ranges. Detection limits （3S/N） found were ranged from 0. 05 to 1.0μg · L 1. The proposed method was applied to the analysis of samples of reservoir water, giving values of recovery and RSD＇s （n = 5） in the ranges of 37. 0%- 107% and 1. 6%- 25. 0%respectively.

关 键 词：气相色谱法 顶空 固相微萃取 水 农药 

分 类 号：O657.7[理学—分析化学]