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

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

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℃；栽气为高纯氮气；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40rain；进样瓶装量为2ml。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=0．9996～0．9999）；平均回收率为99．9％～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、0．08ng；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。

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