GC同时测定红花逍遥片中6种挥发性成分含量

Simultaneous Determination of Six Volatile Components in Honghua Xiaoyao Tablets by GC

关键词:  红花逍遥片  气相色谱  薄荷酮  薄荷脑  2-甲氧基-4-乙烯基苯酚  正丁烯基苯肽  苍术酮  藁本内酯  含量测定

Key words:  Honghua Xiaoyao tablets  GC  menthone  menthol  2-methoxy-4-vinylphenol  3-butenyl phthalide  atractyline  ligustilide  content determination

摘要:

目的 建立同时测定红花逍遥片中薄荷酮、薄荷脑、2-甲氧基-4-乙烯基苯酚、正丁烯基苯肽、苍术酮、藁本内酯6种含量的测定方法。方法 采用HP-5(30 m×250 μm，0.25 μm)色谱柱，柱温箱程序升温；进样口温度250 ℃；检测器温度为280 ℃，分流进样，分流比10∶1。结果 6种成分完全分离，并与其他成分均能达到良好分离；薄荷酮、薄荷脑、2-甲氧基-4-乙烯基苯酚、正丁烯基苯肽、苍术酮、藁本内酯质量浓度分别在1.37~87.38，13.67~874.55，2.05~65.49，3.35~107.20，3.49~111.60，6.95~444.60 μg·mL^-1内与峰面积呈良好的线性关系(r≥0.999 0)；平均回收率(n=6)分别为97.63%，94.25%，97.54%，103.81%，94.30%，98.97%；RSD分别为3.27%，1.80%，2.39%，1.75%，2.32%，2.36%，并测定其在39批次红花逍遥片中的含量。结论 该方法操作简便，准确可靠，重复性好，可用于红花逍遥片质量控制。

Abstract:

OBJECTIVE To develop a method for simultaneous content determination of menthone, menthol, 2-methoxy-4-vinylphenol, 3-butenyl phthalide, atractyline, ligustilide in Honghua Xiaoyao tablets. METHODS The quantitative analysis was carried out on a capillary of HP-5(30 m×250 μm, 0.25 μm) column combined with an oven temperature program; inlet port temperature 250 ℃; detector temperature 280 ℃, split sampling at a split ratio 10∶1. RESULTS The 6 components were completely separated and could be well separated from other components; menthone, menthol, 2-methoxy-4-vinylphenol, 3-butenyl phthalide, atractyline, ligustilide showed a good linear relationship with the chromatographic peak area within the range of 1.37-87.38, 13.67-874.55, 2.05-65.49, 3.35-107.20, 3.49-111.60, 6.95-444.60 μg·mL^-1(r≥0.999 0). The average recovery was 97.63%(RSD=3.27%), 94.25%(RSD=1.80%), 97.54%(RSD=2.39%), 103.81%(RSD=1.75%), 94.30% (RSD=2.32%), 98.97%(RSD=2.36%)(n=6), respectively. And its content in 39 batches of Honghua Xiaoyao tablets were determined. CONCLUSION This method is easy to operate, accurate, reliable, and has good repeatability, can be used to supplement the insufficient quality control of Honghua Xiaoyao tablets.