高效液相色谱法同时测定藏药六味丁香散中4种成分的含量

Simultaneous determination of the content of 4 effective components in Liuwei Dingxiang pulvis

目的建立高效液相色谱法同时测定藏药六味丁香散中4种成分的含量。方法采用高效液相色谱法,以十八烷基硅烷键合硅胶为填充剂(250 mm×4.6 mm,5μm),以乙腈为流动相A,以0.05%磷酸溶液为流动相B,梯度洗脱,流速1 mL·min^(-1),检测波长268 nm,柱温30℃,进样量为10μL。结果没食子酸、土木香内酯、异土木香内酯、丁香酚线性范围分别为0.415～2.490μg·mL^(-1)(r=0.9999)、0.026～0.255μg·mL^(-1)(r=0.9999)、0.028～0.275μg·mL^(-1)(r=0.9999)、0.560～3.360μg·mL^(-1)(r=0.9999);精密度、稳定性、重复性试验均符合方法学测定要求;平均回收率分别在99.2%～101.1%、98.4%～100.0%、98.6%～101.0%、101.2%～101.6%,RSD值均<2.0%(n=3)。结论本方法准确、简便,可用于藏药六味丁香散中4种成分含量的同时测定。

Objective To establish an HPLC method to simultaneously determine 4 effective components in Tibetan medicine Liuwei Dingxiang pulvis. Methods C18 column(250 mm×4.6 mm, 5 μm) was used. The mobile phase consisted of acetonitrile(A) and 0.05% phosphori cacid aqueous solution(B) with gradient elution at the flow rate of 1.0 mL·min-1. The column temperature was 30 ℃, the detection wavelength was 268 nm, and the injection volume was 10 μL. Results The linear ranges of gallic acid, alantolactone, isoalantolactone, and eugenol were 0.415-2.490 μg·mL^-1(r = 0.9999), 0.026-0.255 μg·m L^-1(r = 0.9999), 0.028-0.275 μg·mL^-1(r = 0.9999), and 0.560-3.360 μg·mL^-1(r = 0.9999). The method was precise, stable and repeatable, meeting the requirements of methodology. The average recovery was 99.2%-101.1%, 98.4%-100.0%, 98.6%-101.0%, and 101.2%-101.6%, and the RSD value were less than 2.0%. Conclusion This method is accurate and simple. It can be used to control the quality of Liuwei Dingxiang pulvis.