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目的:建立毛细管气相色谱法测定肤疾安药物中香兰素的含量。方法:采用气相色谱法,以DM-17毛细管色谱柱(30m×0.25mm×0.25μm)为分析柱进行分离测定。色谱柱:DM-17,30m×0.25mm×0.25μm;检测器:FID;进样口温度:230℃;检测器温度:300℃。用氮气作为载气,流速25mL.min-1;色谱柱采用梯度升温,开始温度50℃,然后以15℃.min-1的升温速率升至280℃,保持5min。分流比:20:1,进样量lμL,外标法定量。理论塔板数按香兰素峰计算应不低于40000。结果:香兰素的线性范围为0.060～0.60mg.mL-1(r=0.9997);方法重现性实验RSD为0.8%(n=5);平均回收率为99.1%,RSD为2.0%。结论:本方法简便、灵敏、重复性好,可用于肤疾安药物的质量控制。
Objective: To establish a capillary gas chromatographic method for the determination of vanillin in Gujiangan. Methods: The separation was determined by gas chromatography with DM-17 capillary column (30m × 0.25mm × 0.25μm) as the analytical column. Column: DM-17, 30 m × 0.25 mm × 0.25 μm; Detector: FID; Inlet temperature: 230 ° C .; Detector temperature: 300 ° C. Using nitrogen as a carrier gas, the flow rate of 25mL.min-1; column temperature gradient, the initial temperature of 50 ℃, and then at a temperature of 15 ℃ .min-1 raised to 280 ℃ for 5min. Split ratio: 20: 1, injection volume lμL, external standard method. Number of theoretical plates calculated by vanillin peak should not be less than 40,000. Results: The linear range of vanillin was 0.060-0.60 mg.mL-1 (r = 0.9997). The reproducibility of the method was 0.8% (n = 5). The average recovery was 99.1% and the RSD was 2.0%. Conclusion: The method is simple, sensitive and reproducible, and it can be used for the quality control of Gusan’an drugs.