气相色谱法同时测定无极膏中5个挥发性有效成分的含量

目的: 建立同时测定无极膏中合成樟脑、薄荷脑、水杨酸甲酯、冰片和麝香草酚5种主要成分含量的分析方法。 方法: 采用气相色谱法,色谱柱为聚乙二醇(PEG)-20M毛细管色谱柱(30 m×0.32 mm×0.25 μm),检测器为FID检测器,进样口温度为250 ℃,检测器温度为250 ℃。升温程序为初始温度150 ℃,保持5 min;10 ℃·min^-1升温至200 ℃,保持8 min;再以20 ℃·min^-1升温至240 ℃,保持25 min,分流比为10:1。 结果: 合成樟脑、薄荷脑、水杨酸甲酯、冰片和麝香草酚浓度分别在1.4934~7.4672 mg·mL^-1(r=0.9999),0.9304~4.6520 mg·mL^-1(r=0.9999),0.9075~4.5376 mg·mL^-1(r=0.9999), 0.1387~0.6936 mg·mL^-1(r=0.9999),0.0716~0.3580 mg·mL^-1(r=0.9999)质量浓度范围内线性关系良好。平均回收率(n=9)分别为98.8%,99.4%,98.6%,99.6%,99.7%。 结论: 该方法灵敏、快速简便、准确,可有效地控制无极膏的质量。

Objective: To develop a GC method for the determination of the five effective components in Compositus Mentholi cream. Methods: The GC was performed on a PEG-20M capillary column (30 m×0.32 mm×0.25 μm)with an FID detector.The injector temperature was 250 ℃ and detector temperature was set at 250 ℃.The temperature program of column oven was set as follows:150 ℃ for 5 min,increased to 200 ℃ at a rate of 10 ℃·min^{- 1} and kept for 8 min,then at 20 ℃·min^{- 1} to 240 ℃,held for 25 min.The injection split ratio was 10:1. Results: The calibration curves of synthetic camphor,menthol,methyl salicylate,synthetic borneol and thymol were linear in the concentration range of 1.4934-7.4672 mg·mL^-1 (r=0.9999),0.9304-4.6520 mg·mL^-1(r=0.9999),0.9075-4.5376 mg·mL^-1(r=0.9999),0.1387-0.6936 mg·mL^-1 (r=0.9999),0.0716-0.3580 mg·mL^-1 (r=0.9999),respectively.The mean recoveries (n=9)were 98.8%,99.4%,98.6%,99.6%,99.7%,respectively. Conclusion: The method is simple,rapid,accurate and reproducible.It can be used as the determination control method for Compositus Mentholi cream.

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