GC法测定复方盐酸阿扑吗啡鼻喷剂中薄荷脑的含量

Determination of Menthol in Compound Apomorphine Nasal Spray by GC

目的:建立新药复方盐酸阿扑吗啡鼻喷剂中薄荷脑(C10H20O)的含量测定方法。方法:采用PEG-20M石英毛细管色谱柱(CBP125M×0.25μm,日本岛津)气相色谱法。检测器:氢火焰离子化检测器(FID);柱温:程序升温,初始温度80℃,保持2分钟,以每分种10℃的速率升温至180℃;进样口温度:180℃;检测器温度:200℃:载气:氮气;流速:40ml/分钟;分流比:1∶50。以正十四烷为内标物,内标法定量。结果:薄荷脑在0.188～2.25mg.ml-1范围内与峰面积呈良好的线性关系,r=0.99998(n=7);回收率为98.2%。分析了3批样品,薄荷脑的含量为标示量的99.4%～100.0%。结论:本法专属性强、简便、准确。为该复方制剂中薄荷脑成分提供了切实可行的质控方法。

Objective ：To establish a GC method for the quantitative determination of menthol （C10H20O）in Compound Apomorphine Hydrochloride Nasal Spray, Metbods：PEG-20M quartz capillary column （CBP1 25M × 0.25μm, Shimadzu） was used. Detector ：FID; Column temperature： temperature programmed,initial temperature was kept at 80℃ for 2 rain,then raised to 180℃ at the rate of 10℃·min^-1;Injector temperature：180℃;Detector temperature ： 200℃;Carrier gas：nitrogen;Flow rate： 40ml · min^-1;Split ratio：1： 50. The internal standard was tetradecane. The paper adopted internal calibration to quantify. Results：The standard curve of menthol was agood linear relationship in the range of 0.188-2.25 mg· ml^- 1, r=0.99998（n= 7）;The average recovery was 98.2%. Three batches of samples were abalyzed,the contents of menthol were 99.4% to 100.0 % of the labelled amount. Conclusion：The method is selective ,simple ,accurate and can be used for the quality control of this preparation.