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建立了一步提取三步净化法-气质联用技术检测饲料中四氟甲醚菊酯、胺菊酯、联苯菊酯、甲氰菊酯、三氟氯氰菊酯、氯菊酯、氯氰菊酯、氟氰戊菊酯、氰戊菊酯、氟胺氰菊酯、溴氰菊酯等11种拟除虫菊酯农药残留的方法。样品经乙腈-水(体积比2∶1)溶液提取,正己烷萃取,再经正己烷饱和的乙腈萃取,固相萃取三步净化过程,经DB-5MS色谱柱分离,以氦气为载气,以选择离子扫描方式(SIM)检测。结果表明,方法线性相关系数r≥0.9893,仪器定量限为0.10~5.00μg/kg。样品加标的平均回收率为82.82%~118.54%,相对标准偏差为3.11%~9.22%。
A three-step purification method of GC-MS was established for the determination of tetramethrin, tetramethrin, bifenthrin, fenpropathrin, cyhalothrin, permethrin, cypermethrin, Pyrethrins, fenvalerate, fluvalinate, deltamethrin and other 11 kinds of pyrethroid pesticide residues. The sample was extracted with acetonitrile-water (2: 1 by volume), extracted with n-hexane, extracted with n-hexane saturated acetonitrile and purified by solid-phase extraction. The sample was separated by DB-5MS column and helium , To select ion scan mode (SIM) test. The results showed that the linear correlation coefficient r ≥ 0.893, the limit of quantification was 0.10 ~ 5.00μg / kg. The average recoveries of spiked samples were 82.82% ~ 118.54% with relative standard deviations of 3.11% ~ 9.22%.