目的 建立3個內(nèi)標(biāo)、3個波長法測定大川芎方不同制劑的天麻素類、苯酞類以及酚酸類3類成分的含量。方法 采用Agilent ZORBAX Eclipse XDB-C₁₈色譜柱，流動相為乙腈-0.05%磷酸水溶液，梯度洗脫，檢測波長為220、278、322 nm，柱溫為35℃，體積流量為1 mL/min。以天麻素、藁本內(nèi)酯、阿魏酸為內(nèi)標(biāo)，建立天麻素類（巴利森苷、巴利森苷B）、苯酞類（洋川芎內(nèi)酯I、H、A和歐當(dāng)歸內(nèi)酯A）以及酚酸類（綠原酸）成分的相對校正因子（RCF），在不同進(jìn)樣體積、不同色譜柱、不同添加劑條件下驗證其耐用性，利用RCF值計算2種大川芎方制劑中10個成分的含量，并與外標(biāo)法測定結(jié)果進(jìn)行比較，驗證方法的可行性。結(jié)果 所建立的方法相對校正因子耐用性良好（RSD≤3.5%），與外標(biāo)法的含量測定結(jié)果基本一致。結(jié)論 該3內(nèi)標(biāo)、3波長法可用于大川芎方制劑的藥效成分測定。

Objective Three internal standards and three wavelength methods were established to determine the content of gastrodin, phenolics and phenolic acids in different preparations of Dachuanxiong prescription. Methods The separation was carried out on Agilent ZORBAX Eclipse XDB-C18 column. The mobile phase consisted of acetonitrile-0.05% phosphoric acids aqueous solution with gradient elution. The detection wavelength was at 220, 278, 322 nm with flow velocity at 1.0 mL/min and column temperature at 35℃. Firstly, gastrodin, Z-ligustilide, ferulic acid were used as references to get the average relative correction factors (RCF value) of gastrodin analogues (parishin B, parishin), phthalides (senkyunolide I, senkyunolide H, senkyunolide A and levistolide A) and phenolic acids (chlorogenic acid) respectively. Secondly, durability test of RCF was carried out in different factors including inject volume, columns, and additives. Finally, the contents of 10 compounds in two kinds of Dachuanxiong prescription preparations was calculated based on the RCF value, and compared with the determination results of external standard method to verify the feasibility of the method. Results The result showed that durability of established method was good (RSD ranging below 3.5%), which is basically consistent with the content determination results of external standard method. Conclusion The determination method of three internal standards and three wavelengths can be used to determine the pharmacodynamic composition of Dachuanxiong prescription.

國家自然科學(xué)基金資助項目（81774155，81803703）；中國博士后科學(xué)基金項目（2018M630119）.