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目的:测定CO2超临界萃取的当归油药效组分藁本内酯、正丁烯基苯酞、正丁基苯酞。方法:采用HPLC,ZORBAX-Eclipse XDB-C18色谱柱(4.6 mm×25 cm,5μm),流动相0.05 mol.L-1醋酸铵水溶液(pH 4.0±0.2)(A)-乙腈(B),梯度洗脱(0～10 min,30%B;10～60 min,30～60%B;60～65 min,60%B;65～70 min,60～30%B),检测波长274 nm,流速1.0 mL·min-1,柱温25℃。结果:超临界萃取的当归油药效组分藁本内酯、正丁烯基苯酞、正丁基苯酞分别在0.461 0～20.842 6μg,0.012 6～0.476 8μg,0.022 8～0.825 1μg呈良好的线性关系;平均加样回收率分别为101.27%,99.12%,97.14%。结论:HPLC可用于超临界萃取的当归油药效组分测定,为建立当归油及其制剂与临床疗效对应的质量标准提供了新的思路和方法。
Objective: To determine the effective components of ligustilide, n-butenylphthalide and n-butylphthalide in the supercritical CO2 extraction of Angelica sinensis. METHODS: The mobile phase consisted of 0.05 mol·L-1 ammonium acetate aqueous solution (pH 4.0 ± 0.2) (A) -acetonitrile (B), gradient on a ZORBAX-Eclipse XDB-C18 column (4.6 mm × 25 cm, (0-10 min, 30% B; 10-60 min, 30-60% B; 60-65 min, 60% B; 65-70 min, 60-30% B) at a detection wavelength of 274 nm. 1.0 mL · min-1, column temperature 25 ℃. Results: The effective fractions of ligustilide, n-butenylphthalide and n-butylphthalide in the supercritical fluid extraction were 0.461 0 ~ 20.842 6μg, 0.012 6 ~ 0.476 8μg and 0.022 8 ~ 0.825 1μg respectively The average recovery was 101.27%, 99.12% and 97.14%, respectively. Conclusion: HPLC can be used for the determination of the effective components of Angelica Sinensis oil by supercritical fluid extraction. It provides a new idea and method for establishing the quality standard of angelica oil and its preparation and clinical efficacy.