复方薄荷脑软膏中挥发性成分的定性与定量分析

Qualitative and quantitative analysis of volatile components in compound menthol ointment

目的:建立毛细管气相色谱内标法对复方薄荷脑软膏的5种挥发性成分进行定性和定量分析。方法:采用HP-INNOWAX(30 m×0.32 mm,0.5μm)石英毛细管柱。程序升温:起始温度为60℃,保持8 min,以10℃·min^(-1)的速率升至200℃,保持3 min。进样口温度:200℃,进样量:1μL,分流比:10∶1。检测器为氢火焰离子化检测器(FID),温度:250℃。载气为高纯氦,流速:2.0 mL·min^(-1)。结果:样品在薄荷脑、樟脑、水杨酸甲酯、桉油精和α-蒎烯对照品相同保留时间处出现色谱峰。薄荷脑、樟脑和水杨酸甲酯的标准曲线呈良好的线性关系(r≥0.9990);平均回收率分别为98.21%、98.86%、97.88%,RSD为1.58%、1.69%、2.27%(n=9);校正因子RSD均小于0.2%。测得3批样品中,薄荷脑含量在13.09~13.47 mg·g^(-1),樟脑含量在82.03~89.21 mg·g^(-1),水杨酸甲酯含量在3.30~3.65 mg·g^(-1)范围内。结论:本法专属性强,操作简单,有利于复方薄荷脑软膏的质量控制。

Objective:To establish capillary gas chromatography internal standard method for qualitative and quantitative analysis of five volatile components in compound menthol ointment.Methods:A HP-INNOWAX(30 m×0.32 mm,0.5μm)quartz capillary column was used.Temperature program:the initial temperature was 60℃,held for 8 min,then increased to 200℃at a rate of 10℃·min^(-1),and held for 3 min.Injection port temperature:200℃,injection volume:1μL,split ratio:10∶1.The detector was a flame ionization detector(FID),and the temperature was 250℃.Carrier gas was high-purity helium,flow rate:2.0 mL·min^(-1).Results:The samples showed chromatographic peaks at the same retention time of menthol,camphor,methyl salicylate,eucalyptol andα-pinene reference substance.The standard curves of menthol,camphor and methyl salicylate showed a good linear relationship(r≥0.9990);the average recoveries were 98.21%,98.86%,97.88%,and the RSDs were 1.58%,1.69%,2.27%(n=9);the correction factor RSDs were all less than 0.2%.In the three batches of samples,the content of menthol was in the range of 13.09-13.47 mg·g^(-1),the content of camphor was in the range of 82.03-89.21 mg·g^(-1),and the content of methyl salicylate was in the range of 3.30-3.65 mg·g^(-1).Conclusion:This method has strong specificity and simple operation,which is beneficial to the quality control of compound menthol ointment.