顶空气相色谱法测定乙酰氨基阿维菌素对照品中的残留溶剂

Determination of Residual Solvents in Eprinomectin by Headspace Gas Chromatography

关键词:  乙酰氨基阿维菌素  顶空气相色谱法  残留溶剂

Key words:  eprinovermectin  headspace gas chromatography  residual solvents

摘要:

建立了乙酰氨基阿维菌素对照品中的残留溶剂乙醇、甲醇和丙酮的顶空气相色谱测定法。采用Agilent-HP-5毛细管色谱柱，以氮气为载气，氢火焰离子化检测器为检测器，进样口温度200℃，检测器温度为250℃，以起始温度50℃，保持10min，再以每分钟10℃的速率升温至180℃，顶空瓶平衡温度为80℃，平衡时间为30min。结果表明，在该色谱条件下乙醇、甲醇和丙酮与空白溶剂N，N-二甲基甲酰胺分离良好。乙醇在11～974μg/mL的范围内线性关系良好，检测限为5μg/mL，定量限为11μg/mL，回收率为92.1%～109.9%；甲醇在8～606μg/mL的范围内线性关系良好，检测限为4μg/mL，定量限为15μg/mL，回收率为94.4%～109.5%；丙酮在12～972μg/mL的范围内线性关系良好，检测限为2μg/mL，定量限为6μg/mL，回收率为92.5%～102.4%。该方法分离度好，回收率高，适用于乙酰氨基阿维菌素对照品中残留溶剂的检测。

Abstract:

A headspace gas chromatography method for the determination of residual solvents ethanol, methanol and acetone in eprinomectin was established. Agilent-HP-5 capillary chromatographic column was used to detect the three solvents with nitrogen as carrier gas, the hydrogen flame ionization detector was used, the inlet temperature was 200℃ and the detector temperature was 250℃, the heating program started at 50℃ which hold for 10 min and the temperature was increased to 180°C at a rate of 10℃/min, the equilibrium temperature of the headspace bottle was 80°C and the equilibrium time was 30 minutes. The results showed that ethanol, methanol and acetone were well separated from N,N-Dimethylformamide under this chromatographic condition. Ethanol had a good linear relationship in the range of 11~974μg/mL, the limit of detection and limit of quantification were 5μg/mL and 11μg/mL, respectively, and the recovery rate was 92.1%~109.9%; the methanol had a good linear relationship in the range of 8~606μg/mL, the limit of detection and limit of quantification were 4μg/mL and 15μg/mL, respectively, and the recovery rate was 94.4%~109.5%; acetone had a good linear relationship in the range of 12~972μg/mL, the limit of detection and limit of quantification were 2μg/mL and 6μg/mL, respectively, and the recovery rate was 92.5%~102.4%. The method has good resolution, high recovery rate and is suitable for the detection of residual solvents in eprinomectin.