阿维菌素残留溶剂气相色谱检测方法的建立

Establishment of the Method for Determination of the Residual Solvent of Avermectin by Gas Chromatography

关键词:  阿维菌素  甲醇  残留溶剂  气相色谱法

Key words:  Avermectin  Methanol  Residual solvent  Gas chromatography

摘要:

为了建立阿维菌素残留溶剂气相色谱检查方法，采用6%氰丙基苯基-94%二甲基聚硅氧烷为固定相的毛细管柱，进样口温度：220℃，检测器温度：250℃，载气：氮气，流速：5ml/min，进样量：0.2μl，分流比：10:1，程序升温：初始温度为50℃，保持5分钟，以每分钟15℃的速率升温至80℃，再以每分钟26.7℃的速率升温至240℃。在该色谱条件下，甲醇与内标异丙醇及溶剂间二甲苯分离度良好，检出限为6μg/ml，重复性RSD为3.0%，添加回收率为90.8%。不同色谱柱、柱温、流速、不同进样口温度、不同检测器温度耐用性良好。表明该方法可用于阿维菌素残留溶剂的定量检测。

Abstract:

In order to establish a gas chromatographic method for the determination of the residual solvent of avermectin, a capillary column with 6% cyano propyl phenyl -94% two methyl polysiloxane as a stationary phase was used. The inlet temperature was 220℃; the detector temperature was 250℃; the carrier gas was nitrogen; the flow rate was 5ml/min; the injection volume was 0.2μl; the shunt ratio was 10:1; the heating program was 50℃ as the initial temperature which was kept 5min, and up to 80℃ with the heating rate of 15℃/min，and then up to 240℃ with the heating rate of 26.7℃/min. In this chromatographic condition, the separation of methanol, isopropanol and m-xylene was good, and the detection limit was 6μg/ml, the RSD of repeatability was 3.0%, the rate of recovery of sample addition was 90.8%. The durability of different column, oven temprature, flow rate, inlet temprature and detector temprature was good. Therefore this method could be used to the quantitative detection of the residual solvent of avermectin.