世界中医药

作者	单位
万佳丽1，明凯利2，向阳2，林凤杰1，王丫头2，熊莉2，周翔2，余敏2，黄志军1，2	1 武汉理工大学，武汉，430070； 2 健民药业集团股份有限公司，武汉，430052

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中文摘要:

目的：建立准确可靠的小金胶囊中麝香酮含量测定方法。方法：采用（5%-苯基）-甲基聚硅氧烷为固定相的色谱柱（30 m×0.32 mm×1.8 μm），FID检测器温度为300 ℃，载气为氮气，流速为1.5 mL/min，未分流，柱温为程序升温，进样量为1 μL。以正十八烷为内标物，采用内标法以峰面积比进行检验计算。结果：阴性对照品溶液在与内标溶液、对照品溶液和供试品溶液色谱图相同时间处未见相同色谱峰，麝香酮在进样量为0.120 1~1.200 6 ng的范围内线性关系良好（R2=0.999 7），精密度、稳定性、重复性试验的RSD均<3%，平均回收率为99.93%，RSD为1.30%（n=6）。结论：该方法操作简便，与本品现行药典方法相比，检测结果更准确重复性更好，检测时间大大缩短，可用于小金胶囊中麝香酮的含量测定。

English Summary:

To establish an accurate and reliable method for determination of musk ketone in Xiaojin Capsules.Methods:(5%-phenyl)-methylpolysilicone was used as the stationary phase column(30 m × 0.32 mm × 1.8 μm).FID detector temperature was 300 ℃.Carrier gas was nitrogen.The flow rate was 1.5 mL/min,with no shunt.Column temperature was programmed temperature.And injection volume was 1 μL.N-octadecane was used as internal standard,and internal standard method was used to perform test and calculation according to the peak area ratio.Results:The same chromatographic peak was not seen at the same time in chromatograms of negative reference solution,internal standard solution,reference solution and test solution.Musk ketone had a good linear relationship in the range of 0.1201~1.2006 ng injection volume(R2 = 0.999 7).RSD for precision,stability,and repeatability tests was < 3%.The average recovery was 99.93% and the RSD was 1.30%(n = 6).Conclusion:The method is simple and convenient to operate.Compared with the current pharmacopoeia method for the product,its detection result is more accurate and repeatable,with detection time greatly shortened,and it can be used for determining the content of musk ketone in Xiaojin Capsules.

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