建立在食品及环境样品中特丁硫磷残留量的气相色谱检测及气质联用确证法。样品采用乙酸乙酯提取、活性炭-酸性氧化铝复合小柱净化,丙酮-正己烷混合溶液(体积比为1∶9)洗脱,样液浓缩后经GC-FPD检测,外标法定量,GC-MS定性。GC-FPD法分析时,特丁硫磷在不同样品、不同水平的加标回收率为74.5%~103.3%,RSD为2.1%~11.7%(n=5),方法的检出限为0.001 mg/kg。气质联用法确证时,特丁硫磷的SIM离子为186、231(Q,100)、288。A method for the determination of terbufos residue in food and environment samples was developed.The GC-FPD was used as quantitative detection system,and positive sample was confirmed by GC-MS with SIM mode.Terbufos was extracted with ethyl acetate and eluted with acetone/n-hexane(volume ratio was 1∶9).A SPE column(ENVI-Carb 0.25 g,3 mL) with 0.5 g acid aluminum oxide on the top of the cartridge was used for purification.The recoveries of terbufos in different samples ranged from 74.5% to 103.3% with relative standard deviations ranging from 2.1% to 11.7%(n=5).Under the proposed conditions,the detection limit was 0.001 mg/kg for FPD.When terbufos was confirmed by GC-MS,186,231(Q) and 288 were selected as the SIM ions.厦门市科技计划项目(3502Z20072003);; 厦门出入境检验检疫局科技计划项目(2006XK03
