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

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，0.25 μm）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1 μL，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 6 μg·mL^-1，定量下限分别为0.704 6、0.625 0、0.997 3、0.631 7和0.635 2 μg·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。

Objective: To establish a GC method for the determination of eucalyptol,menthol,methyl salicylate,cinnamylaldehyde and eugenol in Shexiang Qufengshi oil to control its quality comprehensively. Methods: TM-1301 capillary column (30 m×0.25 mm,0.25 μm)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 1 μL,and the split ratio was 10:1. Results: Under 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 7 μg·mL^-1,0.195 6 μg·mL^-1,0.332 1 μg·mL^-1,0.195 6 μg·mL^-1 and 0.198 6 μg·mL^-1,respectively. LOQs were 0.704 6 μg·mL^-1,0.625 0 μg·mL^-1,0.997 3 μg·mL^-1,0.631 7 μg·mL^-1,and 0.635 2 μg·mL^-1,respectively. The contents of the above-mentioned 5 compounds in 3 batches 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. Conclusion: The proposed method can control the quality of Shexiang Qufengshi oil comprehensively by multiple-component assay,which improve the standard of the drug.

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