经典名方当归四逆汤物质基准的关键质量属性研究

Research on Critical Quality Attributes of Substance Benchmarks for Classical Prescription Danggui Sini Decoction

该文建立了当归四逆汤物质基准的高效液相色谱(HPLC)特征图谱及多指标含量测定方法,阐明了当归四逆汤物质基准的关键质量属性,完善了其质量控制体系。使用的色谱柱为Pomenex Luna C 18(250 mm×4.6 mm,5μm),流动相为乙腈-0.05%磷酸水溶液,体积流量为1.0 mL·min-1,梯度洗脱,进样量为10μL,柱温30℃,检测波长为230 nm和290 nm。15批物质基准特征图谱的相似度均大于0.89;两个检测波长下共确定45个共有峰,并指认7个共有成分,分别为芍药苷、阿魏酸、甘草苷、甘草酸铵、细辛脂素、桂皮醛和藁本内酯;15批物质基准的平均出膏率为15.00%;芍药苷、甘草酸铵、细辛脂素、桂皮醛和藁本内酯的含量分别为8.226~13.46、1.929~6.535、0.02002~0.03430、0.07661~0.5433和0.07594~0.1406 mg·g^(-1)。该研究为经典名方当归四逆汤物质基准的质量控制和复方制剂的开发提供了科学依据。

A high performance liquid chromatography(HPLC)was established for determination of the characteristic spectra as well as the multi-index contents of substance benchmarks for classical prescription Danggui Sini decoction,which elucidated the critical quality attributes and improved the quality control system.The chromatographic analysis was performed on a Pomenex Luna C 18 column(250 mm×4.6 mm,5μm)at 30℃.The gradient elution was carried out with a linear gradient system consisted of acetonitrile-0.05%phosphoric acid water solution.The signal was monitored at 230 nm and 290 nm.The flow rate was maintained at 1.0 mL·min-1.The similarity of characteristic spectra for 15 batches of substance benchmarks was more than 0.89,while 45 common peaks were assessed,and 7 common components were identified as paeoniflorin,ferulic acid,liquiritin,ammonium glycyrrhizinate,asarinin,cinnamaldehyde and ligustilide.The average yield of dry extract for 15 batches of substance benchmarks was 15.00%.The contents of paeoniflorin,ammonium glycyrrhizinate,asarinin,cinnamaldehyde and ligustilide in the 15 batches of substance benchmarks were 8.226-13.46,1.929-6.535,0.02002-0.03430,0.07661-0.5433 and 0.07594-0.1406 mg·g^(-1),respectively.This study provides a scientific basis for the quality control of substance benchmarks as well as the development of compound preparation of Danggui Sini decoction.