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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,5μm),流动相为乙腈-0.2%磷酸水溶液(41∶59),流速1.0 m L·min-1,柱温30℃,检测波长270 nm。以丹参酮ⅡA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ⅡA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ⅡA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 establish a test for simultaneous determination of tanshinones in Zilongjin tablets. Methods: The column was Agilent ZORBAX Extend-C18 column (4.6 mm × 150 mm, 5 μm) with acetonitrile-0.2% phosphoric acid solution (41:59) at a flow rate of 1.0 mL · min-1 using high performance liquid chromatography -1, column temperature 30 ℃, detection wavelength 270 nm. Tanshinone Ⅱ A was used as internal standard to establish the relative correction factor between it and dihydrotanshinone Ⅰ, cryptotanshinone and tanshinone Ⅰ. Then the content of dihydrotanshinone Ⅰ, cryptotanshinone, tanshinone Ⅰ and tanshinone ⅡA in five batches of Zilongjin tablets were measured by a multi-assessment method and external standard method, and the relative average deviation (RAD) of the two methods was measured. Results: The injection rates of dihydrotanshinone Ⅰ, cryptotanshinone, tanshinone Ⅰ and tanshinone ⅡA were 6.16 ~ 61.6 ng (r = 0.999 9), 19.04-190.4 ng (r = 0.999 9) and 11.58-115.8 ng 9). The average recoveries were 99.4%, 98.7%, 98.0% and 98.5%, respectively. The RSDs were 0.5%, 0.4%, 0.9% and 0.8%, respectively. RAD: dihydrotanshinone Ⅰ of 5 batches of samples were 0.3%, 0.1%, 0.3%, 0.3%, 0.4% and cryptotanshinone were 0.08%, 0.04%, 0.3%, 0.04% 0.04% and tanshinone I respectively 0.1%, 0.2%, 0.2%, 0.07%, 0.2%, indicating that there is no significant difference between the two methods. Conclusion: The method is sensitive, simple and accurate. The method can simultaneously determine the content of four components in Radix Salviae Miltiorrhizae and can be used for the quality control of Radix Aconitum and further improve the quality standard.