水果中三唑酮残留量的气相色谱和气相色谱-质谱分析

Analysis of Residual Triadimefon in Fruit by Gas Chromatography and Gas Chromatography/Mass Spectrometry

水果中三唑酮残留用丙酮提取，经液－液分配净化，用气相色谱－电子捕获检测器测定，并用气相色谱－质谱（选择离子监测）进行确证。以ＨＰ－５大口径毛细管拄和ＨＰ－５ＭＳ毛细管柱为分离柱，选择出合适的色谱条件，三唑酮的分离效果良好。本方法对苹果样品的测定下限为５×１０－５ｇ／ｋｇ；添加浓度为５×１０－５～１，０×１０－３ｇ／ｋｇ的三唑酮；回收率为９６％以上；相对标准偏差小于４．０％。样品前处理采用了微量化学法（ＭｉｃｃＭ）技术，质谱（选择离子监测）确证的监测离子选Ｍ／Ｚ２９３、２０８、１８１。

The residual triadimefon in fruit was extracted by acetone. After clean-up by liquid-liquid partition, the triadimefon was determined by GC-ECD and identified by GC/MS (SIM). HP-5 and HP-5MS capillary columns were used. Under optimized GC conditions, a good separation was obtained with a detection limit 5 x 10-5 g/kg for an apple sample. When the fortifying concentration of triadimefon was in the range of 5 x 10-5-1. 0 x 10-3 g/kg, the recovery was >96% and .the RSD was <4%. The sample extraction and clean-up were per- formed according to the mcrochemical mehtod (MiccM). The m/z 293, 208, 181 were chosen as MS(SIM) monitoring ions.