替代对照品法同时测定川芎中丁苯酞和藁本内酯的含量

目的: 建立HPLC替代对照品法同时测定川芎中丁苯酞和藳本内酯。 方法: 采用Agilent Eclipse XDB-C₁₈(4.6 mm×150 mm,5 μm)色谱柱,以甲醇-水(52: 48)为流动相,流速1.0 mL·min^-1,丁苯酞检测波长228 nm,藁本内酯检测波长330 nm,柱温35 ℃。以丁苯酞作为藁本内酯的替代对照品,在不同条件下测定相对校正因子,利用相对校正因子和替代对照品同时测定川芎中丁苯酞和藁本内酯的含量。 结果: 丁苯酞和藁本内酯进样量分别在0.01~0.2 μg(r=0.9999)和0.1~2.0 μg(r=0.9999)范围内与峰面积呈良好的线性关系,测得相对校正因子f’为1.0806,不同条件下相对校正因子的重现性良好,利用相对校正因子计算川芎中待测成分含量与外标法实测值之间没有明显差异。 结论: 用丁苯酞替代藁本内酯作为对照品,同时测定川芎中丁苯酞及藁本内酯的含量,解决了藳本内酯对照品不稳定的难题,该方法可用于川芎的质量控制。

Objective: To establish an HPLC method for determination of butylphalide and ligustilide in Chuanxiong Rhizoma by substitution method of reference substance. Methods: Agilent Eclipse XDB-C₁₈(4.6 mm×150 mm,5 μm) was adopted,the mobile phase consisted of methanol-water(52: 48) at a flow rate of 1.0 mL·min^-1,the detection wavelength was 228 nm for butylphalide and 330 nm for ligustilide.To measure the relative correction factor of ligustilide under different condition using the butylphalide as substitute reference substance,and ligustilide in Chuanxiong Rhizoma was determined by substitute reference substance and the relative correction factor,the butylphalide was determined with the external standard method. Results: The linear response ranges(n=6) of butylphalide and ligustilide were 0.01-0.2 μg(r=0.9999) and 0.1-2.0 μg(r=0.9999),respectively.The relative correction factor(f’) was 1.0806. Conclusion: The substitute reference substance is adopted to determine butylphalide and ligustilide in Chuanxiong Rhizoma.This accurate method is available and applied for quality control of Chuanxiong Rhizoma.