王发++李继++刘芳

[摘要] 目的 建立复方枸橼酸喷托维林颗粒中薄荷脑和麝香草酚的定性鉴别和含量测定方法。方法 采用薄层色谱法对薄荷脑和麝香草酚进行定性鉴别，采用GC色谱法对薄荷脑和麝香草酚进行含量测定。色谱条件：使用DB-WAX（30 m×0.32 mm×0.25 μm）毛细柱，FID检测器，进样口温度230℃，检测器温度250℃。结果 薄层鉴别斑点清晰，阴性对照无干扰。在选定的色谱条件下，两种物质分离良好，薄荷脑的回归方程为y = 2681.10x-10.81（r = 1.00），平均回收率为98.0%（n=6，RSD=2.3%），线性范围为：0.016～1.55 g/L；麝香草酚的回归方程为y =2762.00x-6.64（r = 1.00），平均回收率为100.4%（n=6，RSD=1.5%），线性范围为：0.010～1.00 g/L。三批样品中两种组分的含量分别为0.13 mg/g和0.096 mg/g。结论 该方法简单准确，可用于该制剂中的薄荷脑和麝香草酚的定性鉴别和含量测定。

[关键词] 复方枸橼酸喷托维林颗粒；薄荷脑；麝香草酚；薄层色谱法；气相色谱法

[中图分类号] R92 [文献标识码] A [文章编号] 1673-7210（2017）04（c）-0134-04

[Abstract] Objective To establish a method of qualitative identification and content determination of menthol and thymol in Compound Pentoxyverine Citrate Granules. Methods TLC was applied for qualitative of menthol and thymol； GC was used for quantitative determination of menthol and thymol. A DB-WAX column （30 m×0.32 mm×0.25 μm） was used. The inlet temperature was 230℃ and the FID detector temperature was 250℃. Results TLC spots were clear and well separated， there was no interference for negative sample. A good resolution was obtained by this method between the peaks of menthol and thymol. The linearity equation of menthol was y =2681.10x -10.81 （r = 1.00）， the average recovery was 98.0% （n=6， RSD =2.3%）， and the linear range was 0.016-1.55 g/L. The linearity equation of thymol was y = 2762.00x-6.64 （r =1.00）， the average recovery was 100.4% （n=6， RSD =1.5%）， and the linear range was 0.010-1.00 g/L. The average contents of 3 batches of samples were 0.13 mg/g and 0.096 mg/g. Conclusion The method was simple and accurate， which can be used for qualitative identification and content determination of menthol and thymol in Compound Pentoxyverine Citrate Granules.

[Key words] Compound Pentoxyverine Citrate Granules； Menthol； Thymol； TLC； GC

复方枸橼酸喷托维林颗粒是由枸橼酸喷托维林、盐酸麻黄碱、枸橼酸、薄荷脑（0.15 mg/g）、麝香草酚（0.10 mg/g）和一些辅料组成的复方制剂。临床用于上呼吸道感染等引起的咳嗽、咯痰。方中薄荷脑为薄荷油中提取的一种饱和环状醇，具有芳香性，主要用于皮肤或黏膜产生清凉感，以减轻不适及疼痛。麝香草酚具有杀菌作用，能促进气管纤毛运动，有利于气管黏液的分泌，易起祛痰作用。现行国家标准[1]202-203采用容量法只对制剂中枸橼酸喷托维林的量进行了控制，并未对薄荷脑和麝香草酚进行控制。本文参考相关文献[2-20]，采用TLC法对制剂中薄荷脑和麝香草酚进行定性鉴别，采用GC法进行定量分析，实验结果表明，本方法简便、准确，可用于该品种的质量控制。……