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建立了中华圆田螺中莠去津(ATZ)及其主要代谢物脱乙基莠去津(DE-ATZ)、脱异丙基莠去津(DI-ATZ)和脱乙基-脱异丙基莠去津(DEDI-ATZ)的GC-MS分析方法。样品经乙腈匀浆、超声提取后,经由中性氧化铝,ZnSO_4,Na_2SO_4组成的层析柱脱脂、脱蛋白和脱水净化处理,使用HP-5毛细管柱在TIC模式下定性,SIM模式下外标法定量检测。测定结果表明,4种物质质量浓度在0.01~2 mg/L范围内线性良好,相关系数(r2)均≥0.999,方法检出限均为3μg/kg。加标回收率70%~109%,相对标准偏差(RSD)均低于9.6%(n=5)。方法用于测定城市景观湖内中华圆田螺中的ATZ及代谢物,表明ATZ和DI-ATZ均有检出。
ATRA and its major metabolites, DE-ATZ, DI-ATZ and de-ethyl-de-isopropyl Atrazine (DEDI-ATZ) by GC-MS analysis method. The samples were homogenized with acetonitrile, extracted by ultrasonic, degreased, deproteinized and dehydrated by a chromatographic column composed of neutral alumina, ZnSO 4 and Na 2 SO 4, characterized by HP-5 capillary column in TIC mode, Law quantitative test. The results showed that the linearity of the four substances in the range of 0.01-2 mg / L was good, and the correlation coefficient (r2) was ≥0.999. The detection limits were 3 μg / kg. The spiked recoveries ranged from 70% to 109% with relative standard deviations (RSDs) below 9.6% (n = 5). The method was applied to the determination of ATZ and metabolites in the snakehead snail in the lake, indicating that both ATZ and DI-ATZ were detected.