一测多评法测定紫龙金片中丹参酮类成分的含量

目的: 建立一测多评法同时测定紫龙金片中丹参酮类成分. 方法: 采用高效液相色谱法测定,色谱柱为Agilent ZORBAX Extend-C₁₈柱(4.6 mm×150 mm,5 μm),流动相为乙腈-0.2%磷酸水溶液(41: 59),流速1.0 mL · min^-1,柱温30 ℃,检测波长270 nm.以丹参酮Ⅱ_A为内标,建立其与二氢丹参酮Ⅰ、隐丹参酮和丹参酮Ⅰ的相对校正因子,实现一测多评.再分别采用一测多评法和外标法测定5批紫龙金片中二氢丹参酮Ⅰ、隐丹参酮、丹参酮Ⅰ和丹参酮Ⅱ_A的含量,考察2种方法测定结果的相对平均偏差(RAD). 结果: 二氢丹参酮Ⅰ、隐丹参酮、丹参酮Ⅰ和丹参酮Ⅱ_A进样量分别在6.16~61.6 ng(r=0.999 9)、19.04~190.4 ng(r=0.999 9)、11.58~115.8 ng(r=0.999 9)、20.08~200.8 ng(r=0.999 9)范围线性良好;平均回收率分别为99.4%、98.7%、98.0%、98.5%,RSD分别为0.5%、0.4%、0.9%、0.8%.2种方法测得的5批样品含量的RAD:二氢丹参酮Ⅰ分别为0.3%、0.1%、0.3%、0.3%、0.4%、隐丹参酮分别为0.08%、0.04%、0.3%、0.04%、0.04%、丹参酮Ⅰ分别为0.1%、0.2%、0.2%、0.07%、0.2%,表明2种方法测得结果无显著性差异. 结论: 该方法灵敏、简便、准确,能同时测定丹参中4个成分的含量,可用于紫龙金片的质量控制,进一步提高质量标准.

Objective: To develop a new method for simultaneous determination of tanshinones in Zilongjin tablets. Methods: The HPLC system consisted of the Agilent ZORBAX Extend-C₁₈(4.6 mm×150 mm,5 μm)column and acetonitrile-0.2% phosphoric acid(4159)as the mobile phase at 30 ℃ as the column temperature,the flow rate was 1.0 mL · min^-1 and the detective wavelength was 270 nm.Dihydrotanshinone Ⅰ,cryptotanshinone,tanshinone Ⅰ and tanshinone Ⅱ_A were selected as analytes to evaluate the quality of Zilongjin tablets.The relative analysis correction factors(RCFs)of tanshinone Ⅱ_A as the internal standard to other three tanshinones were calculated in the quantitative analysis of multi-components by single marker(QAMS).QAMS and the external standard method(ESM)were used respectively to determine the content of dihydrotanshinone Ⅰ,cryptotanshinone,tanshinone Ⅰ and tanshinone Ⅱ_A in 5 batches of Zilongjin tablets.Relative average deviations(RADs)of external standard method and QAMS method were compared. Results: Dihydrotanshinone Ⅰ,cryptotanshinone,tanshinone Ⅰ and tanshinone Ⅱ_A showed a good linear relationship in the ranges of 6.16-61.6 ng(r=0.999 9), 19.04-190.4 ng(r=0.999 9),11.58-115.8 ng(r=0.999 9),20.08-200.8 ng(r=0.999 9),respectively. The average recoveries were 99.4%,98.7%,98.0%,98.5% and the RSDs were 0.5 %,0.4 %,0.9 %,0.8 %,respectively.By QAMS method and external standard method,the relative average deviation(RAD)of dihydrotanshinone Ⅰ was 0.3%,0.1%,0.3%,0.3%,0.4%,respectively;the RAD of cryptotanshinone was 0.08%,0.04%,0.3%,0.04%,0.04%,respectively;the RAD of tanshinone Ⅰ was 0.1%,0.2%,0.2%,0.07%,0.2%,respectively in the 5 samples.No significant differences were found in the quantitative analysis results of tanshinones by the two methods. Conclusion: QAMS method for simultaneous determination of tanshinones is sensitive,simple,accurate,and suitable for the quality control of Zilongjin tablets.The method can further improve the quality standards and ensure the curative effect of production.