摘要
目的建立HPLC法用于青紫颗粒制备工艺过程的质量控制,并对中试样品中丹酚酸B和绿原酸含量进行测定。方法丹酚酸B和绿原酸测定条件:色谱柱为Agilent Zorbax SB-C18柱(4.6 mm×250 mm,5μm),乙腈-0.1%磷酸为流动相梯度洗脱,流速为1 mL/min,柱温为30℃,检测波长为286 nm(丹酚酸B)和327 nm(绿原酸);以绿原酸及丹酚酸B转移率为指标,选取提取次数、提取时间、加水倍量为影响因素,采用正交设计优选最佳提取工艺,并优选浓缩温度和干燥温度。结果丹酚酸B和绿原酸分别在0.16~0.63μg(r=1.000 0)、0.03~0.14μg(r=1.000 0)范围内线性关系良好,平均加样回收率分别为99.05%、103.72%;最优提取工艺为:加12倍水,提取2次,每次1 h,浓缩温度控制在80℃以下,干燥温度控制在70℃以下。所测中试样品中丹酚酸B和绿原酸质量分数分别为(3.04±0.046)mg/g和(0.74±0.006)mg/g。结论建立的液相方法准确稳定,可用于青紫颗粒制备过程的质量控制,优选的提取工艺稳定可行,适合批量生产。
Objective A method of high-performance liquid chromatography was performed to control the quality of preparation process of Qingzi granules and determine salvianolic acid B and chlorogenic acid of pilot products.Methods An Agilent Zorbax SB-C18 column(4.6 mm×250 mm,5 μm) was used with a mobile phase of acetonitrile-0.1% phosphoric acid solution in gradient elution,at the detection wavelength of 286 nm(salvianolic acid B) and327 nm(chlorogenic acid),a column temperature of 30℃ and a flow rate of 1.0 mL/min.Taking the transfer rate of chlorogenic acid and salvianolic acid B as the index,the extraction times,extraction time and the amount of water as the influencing factors,the orthogonal design was used to optimize the extraction process,concentration and drying temperature.Results Salvianolic acid B and chlorogenic acid showed good linear relationship within the range of0.16-0.63 μg(r=1.000 0) and 0.03-0.14 μg(r=1.000 0),respectively.The average recovery rate of salvianolic acid B and chlorogenic acid was 99.05% and 103.72%,respectively.The best preparation process for Qingzi granules was as follows:adding 12 times the amount of water,extracting 2 times and each time for 1 h.The condensing and drying temperature should be controlled below 80℃ and 70℃,respectively.The content of salvianolic acid B and chlorogenic acid in pilot products was(3.04±0.046) mg/g and(0.74±0.006) mg/g,respectively.Conclusion The established method was accurate and sensitive,which could be used for the quality control of Qingzi granules.The optimized preparation method was suitable for mass-produced.
作者
马葆睿
倪健
庞琳诺
蔡梦如
覃柳莹
白杰
张志勤
张萌
王晓玲
曲昌海
MA Baorui;NI Jian;PANG Linnuo;CAI Mengru;QIN Liuying;BAI Jie;ZHANG Zhiqin;ZHANG Meng;WANG Xiaoling;QU Changhai(School of Chinese Materia Medica,Beijing University of Chinese Medicine,Beijing 102488,China;Beijing Children's Hospital affiliated to Capital Medical University,Beijing 102488,China)
出处
《广东药科大学学报》
CAS
2021年第2期18-23,共6页
Journal of Guangdong Pharmaceutical University
基金
重大新药创制科技重大专项项目(2018ZX09721003-002)。
