固相微萃取-气相色谱法测定水中有机磷农药  

GC Determination of Organophosphorus Pesticides in Water with Solid Phase Micro-extraction

作　　者：刘静[1] 曾兴宇[1] 烟卫[1] 张艳萍[1] 王意[1] 刘小骐[1] 

机构地区：[1]国家海洋局天津海水淡化与综合利用研究所,天津300192

出　　处：《理化检验（化学分册）》2012年第8期950-952,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家海洋局业务化项目(1511112000005);中央级公益性科研院所基本科研业务费专项资金项目(K-JBYWF-2009-T203;K-JBYWF-2010-G16)

摘　　要：提出了固相微萃取样品-气相色谱法测定水中6种有机磷农药残留量的方法。为使固相微萃取达到更高的效率,选择65μm的聚二甲基硅氧烷/二乙烯苯(PDMS/DVB)萃取头,萃取温度及时间为80℃和20 min,在10 mL试样中加入氯化钠1.5 g作为盐析剂。用HP-5毛细管色谱柱分离,电子捕获检测器检测。6种有机磷农药的质量浓度均在1.0～50.0μg·L^(-1)范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.026～0.064μg·L^(-1)之间。方法用于水样分析,测定值的相对标准偏差(n=6)在3.0～5.6%之间,加标回收率在86.2%～115.7%之间。GC with sample pretreatment by solid phase micro-extraction （SPME） was applied to the determination of residual amounts of 6 organphosphorus pesticides in water. To attain a higher efficiency for SPME, the 65μm PDMS/DVB micro-extractor was selected, and the extraction was carried out at 80 ℃ for 20 min, with addition of 1. 5 g NaCl to 10 mL of sample solution as salting out agent. The analyte were separated on HP-5 capillary column and detected by ECD. Linear relationships between Values of peak area and mass concentration of the 6 organphosphorus pesticides were kept in the same range of 1.0--50. 0 μg · L-1 , with detection limit （3S/N） in the range of 0. 026--0. 064 μg ·L-1. The proposed method was applied to the analysis of water samples, giving values of recovery found by standard addition method in the range of 86.2 %-115.7% with RSD＇s （n： 6） in the range of 3. 0 %- 5.6 %.

关 键 词：固相微萃取 气相色谱法 电子捕获检测器 水 有机磷农药 

分 类 号：O652.63[理学—分析化学]