气相色谱法测定麝香祛风湿油中桉油精、薄荷脑、水杨酸甲酯、桂皮醛及丁香酚的含量

Determination of eucalyptol,menthol,methyl salicylate,cinnamylaldehyde and eugenol in Shexiang Qufengshi oil by GC

目的:建立气相色谱法同时测定麝香祛风湿油中桉油精、薄荷脑、水杨酸甲酯、桂皮醛以及丁香酚5个成分的含量,从而全面地控制其质量。方法:采用TM^-1301毛细管柱(30 m×0.25 mm,0.25μm)色谱柱,氮气为载气,氢火焰离子检测器的温度为250℃,程序性升温(初始温度50℃,保持2 min;以60℃·min^-1上升到90℃,保持2 min;以8℃·min^-1上升到150℃;再以60℃·min^-1上升到235℃,保持3 min),进样口温度为230℃,进样量1μL,分流比为10∶1。结果:在该色谱条件下,样品中桉油精、薄荷脑、水杨酸甲酯、桂皮醛以及丁香酚分离度良好,经验证,它们均具有良好的线性关系。桉油精、薄荷脑、水杨酸甲酯、桂皮醛和丁香酚的检测下限分别为0.234 7、0.195 6、0.332 1、0.195 6和0.198 6μg·mL^-1,定量下限分别为0.704 6、0.625 0、0.997 3、0.631 7和0.635 2μg·mL^-1。3批样品中上述5个成分的含量范围分别为250.97~254.23、35.13~33.03、477.08~500.06、18.94~20.18、12.60~18.99 g·L^-1。结论:该方法能够通过多成分含量测定全面控制麝香祛风湿油的质量,从而提高该品种的质量标准。

establish a GC method for the determination of eucalyptol,menthol,methyl salicylate,cinnamylaldehyde and eugenol in Shexiang Qufengshi oil to control its quality comprehensively.capillary column(30 m×0.25 mm,0.25μm)was adopted,the carrier gas was nitrogen and the temperature of the flame ionization detector was 250℃.The column temperature was kept at 50℃for 2 min,then raised at 60℃·min^-1 to 90℃,held for 2 min,then raised at 8℃·min^-1 to 150℃,raised at 60℃·min^-1 to 235℃,and held for 3 min.The inlet temperature was 230℃,the injection volume was 1μL,and the split ratio was 10∶1.the optimal conditions,oeucalyptol,menthol methyl salicylate,cinnamylaldehyde and eugenol were well separated,and the results showed that they had good linearity.The LODs of oeucalyptol,menthol,methyl salicylate,cinnamylaldehyde and eugenol were 0.234 7μg·m L^-1,0.195 6μg·m L^-1,0.332 1μg·m L^-1,0.195 6μg·m L^-1 and 0.198 6μg·m L^-1,respectively.LOQs were 0.704 6μg·m L^-1,0.625 0μg·m L^-1,0.997 3μg·m L^-1,0.631 7μg·m L^-1,and 0.635 2μg·m L^-1,respectively.The contents of the above-mentioned 5 compounds in 3batches of samples were 250.97-254.23,35.13-33.03,477.08-500.06,18.94-20.18 and 12.60^-18.99 g·L^-1,respectively.proposed method can control the quality of Shexiang Qufengshi oil comprehensively by multiple-component assay,which improve the standard of the drug.