远志中远志酮Ⅲ和3,6′-二芥子酰基蔗糖含量测定方法的改进  

Improvement on the determination method of polygalaxanthoneⅢand 3,6′-disinapoyl sucrose in Polygala tenuifolia

作　　者：谢元彪 李淞明 詹常森 XIE Yuanbiao;LI Songming;ZHAN Changsen(Shanghai Hutchison Pharmaceutical Co.,Ltd.,Shanghai Innovation Engineering and Technology Research Center of Solid Preparations of Traditional Chinese Medicine,Shanghai 201401,China)

机构地区：[1]上海和黄药业有限公司,上海中药固体制剂创新工程技术研究中心,上海201401

出　　处：《中国药品标准》2023年第5期488-497,共10页Drug Standards of China

基　　金：上海市科学技术委员会科研计划项目(19401902000)。

摘　　要：目的:改进《中国药典》2020年版所载远志中远志(口山)酮Ⅲ和3,6′-二芥子酰基蔗糖的含量测定方法,解决远志(口山)酮Ⅲ中包含杂质成分且无法完全分离及甲醇和70%甲醇对远志(口山)酮Ⅲ和3,6′-二芥子酰基蔗糖响应值差异大的问题。方法:对照品溶液和供试品溶液的制备均以甲醇作为溶剂,供试品溶液采用超声提取,采用UHPLC方法,以乙腈(A)-0.1%磷酸溶液(B)为流动相,梯度洗脱(0~5 min,10%A→14%A;5~12 min,14%A→17%A;12~17 min,17%A→19%A;17~22 min,19%A→21%A;22~30 min,100%A);柱温30℃,体积流量0.3 mL·min^(-1),检测波长320 nm,进样量3μL。结果:采用70%甲醇制备的远志(口山)酮Ⅲ和3,6′-二芥子酰基蔗糖对照品溶液的峰面积分别比采用甲醇制备的相同浓度对照品溶液的峰面积高38.9%和34.5%;采用药典方法测得的远志(口山)酮Ⅲ中实际包含了杂质成分远志(口山)酮Ⅺ,而采用UHPLC梯度洗脱方法可以将远志(口山)酮Ⅲ中包含的杂质成分远志(口山)酮Ⅺ完全分开。结论:改进方法解决了远志(口山)酮Ⅲ中包含杂质成分远志(口山)酮XI且无法完全分离及甲醇和70%甲醇对远志(口山)酮Ⅲ和3,6′-二芥子酰基蔗糖响应值差异大的问题,可以更准确地反映远志中这2个指标成分的真实含量。Objective:To improve the determination method of polygalaxanthoneⅢand 3,6′-disinapoyl sucrose in Polygala tenuifolia in the Chinese Pharmacopoeia 2020 in order solve the problem of impurities in polygalaxanthoneⅢthat cannot be completely separated,as well as the significant difference in response values between methanol and 70%methanol to polygalaxanthoneⅢand 3,6′-disinapoyl sucrose.Methods:Using methanol as the solvent for the preparation of the reference solution and the test solution,and the test solution was extracted by ultrasoinic extraction method.UHPLC method was adopted with acetonitrile(A)-0.1%phosphoric acid solution(B)as the mobile phase using gradient elution(0-5 min,10%A→14%A;5-12 min,14%A→17%A;12-17 min,17%A→19%A;17-22 min,19%A→21%A;22-30 min,100%A)at the flow rate of 0.3 mL·min^(-1).The detection wavelength was at 320 nm.The sample injection volume was 3μL.Results:The peak areas of the reference solution of polygalaxanthoneⅢand 3,6′-disinapoyl sucrose prepared with 70%methanol were 38.9%and 34.5%higher than those of the same concentration reference solution prepared with methanol,respectively.The impurity component polygalaxanthoneⅪwas actually contained in polygalaxanthoneⅢmeasured by pharmacopoeia methods,and the impurity component polygalaxanthoneⅪcontained in polygalaxanthoneⅢcould be completely separated by UHPLC gradient elution method.Conclusion:The improved method can solve the problem of impurity component polygalaxanthone XI contained in polygalaxanthoneⅢand could not be completely separated,as well as the significant difference in response values between methanol and 70%methanol to polygalaxanthoneⅢand 3,6′-bissinoyl sucrose,which can more accurately reflect the true content of these two indicator components in Polygala tenuifolia.

关 键 词：远志 远志(口山)酮Ⅲ 3 6′-二芥子酰基蔗糖 含量测定 UHPLC 

分 类 号：R921.2[医药卫生—药学]