分散液相微萃取技术与GC/MS联用检测生物样品中拟除虫菊酯类杀虫剂

Determination of pyrethroid pesticides in urine by dispersive liquid- liquid microextraction coupled with GC- MS

建立了分散液相微萃取与GC/MS联用分析人体尿液中拟除虫菊酯类杀虫剂的方法。确定了分散液相微萃取最优萃取条件：30 mg薄荷醇作为萃取剂,0.5 m L甲醇作为分散剂,萃取时间为2 min,离心时间为5 min,在此条件下进行分析,三氟氯氰菊酯、氯菊酯、氰戊菊酯的检出限分别为3.3,3.3和10 ng/m L,相对标准偏差分别为1.8%～12%,3.3%～5.7%,3.8%～13%,富集倍数分别为460,512,1302。

A method was developed for determination of the pyrethroid pesticides in urine by dispersive liquidliquid microextraction（ DLLME） coupled with GC-MS. The optimal extraction for DLLME was carried out by using 30 mg of menthol as an extraction solvent and 0. 5 m Lof alcohol as a disperser for 2 minute extraction and5 minute centrifugation. Under the optimized conditions,the LODs of cyhalothrin,pemethrin,fenvalerate were3. 3,3. 3 and 10 ng / m L; the RSDs were 1. 8% ～ 12%,3. 3% ～ 5. 7%,3. 8% ～ 13%; and the enrichment factors were 460,512,1302,respectively. The method using menthol as an extraction solvent demonstrated some advantages such as high enrichment efficiency,less interference of biological impurities,benign to environment,etc. The method can be used to analyze trace amounts of pyrethroids in biological samples.