毛细管气相色谱法测定依诺昔酮原料药中6种有机溶剂残留量

目的:建立测定依诺昔酮原料药中6种有机溶剂(乙醇、丙酮、乙醚、二氯甲烷、乙酸乙酯与甲苯)残留量的方法。方法:采用毛细管气相色谱法。色谱柱为DB-1301毛细管柱;柱温采用程序升温;氢火焰离子化检测器,检测器温度为250℃;载气为高纯氮气;进样口温度为200℃;分流比为10∶1;顶空进样,加热温度为100℃,加热时间为40 min;进样瓶装量为2 ml。结果:乙醇、丙酮、乙醚、二氯甲烷、乙酸乙酯与甲苯在各自检测质量浓度范围内线性关系良好(r=0.999 6⁰.999 9);平均回收率为99.9%0.999 9);平均回收率为99.9%¹01.3%(RSD=0.76%101.3%(RSD=0.76%¹.89%,n=3);检测限分别为0.04、0.11、0.21、0.07、0.16、0.08 ng;3批样品中只检出乙醇。结论:建立的方法快速、灵敏、准确,可用于依诺昔酮原料药中有机溶剂残留量测定。

Determination of 6 Residual Organic Solvents in Enoximone Raw Material by Capillary Gas Chromatography

OBJECTIVE： To establish the method for the determination of 6 residual organic solvents as alcohol, acetone, di- ethyl ether, dichloromethane, ethyl acetate and methylbenzene in enoximone. METHODS： Capillary gas chromatography was used. The determination was performed on DB-1301 capillary column by temperature progralnming; flame ionization detector was used with temperature of 250 %. High-purity N2 was used as carrier gas; the temperature of injector was 200 ℃ ; split ratio was 10 ： 1. The heating temperature of headspace sampling was set at 100 ℃, heating time was 40 rain; the volume of sampling was 2 ml. RE- SULTS： There was good linear relationship of alcohol, acetone, diethyl ether, dichloromethane, ethyl acetate and methylbenzene （r=0.999 6-0.999 9） with average recoveries of 99.9%-101.3% （RSD=0.76%-l.89%, n=3）. The detection limits were 0.04, 0.11, 0.21, 0.07, 0.16 and 0.08 ng, respectively. Only the alcohol was detected in 3 batches of sample. CONCLUSIONS： The method is rapid, simple and accurate, It can be used for the determination of residual organic solvents in enoximone raw material. KEYWORDS Enoximone; Raw material; Organic solvents; Residual; Capillary gas chromatography