经典名方芍药甘草汤物质基准质量标准研究
Quality Value Transfer for Substance Benchmark of Classical Famous Prescription Shaoyao Gancao Decoction
曲缘章 1李丹 2刘佳萌 1马生军 3孙博 1李宝国 4李刚 5杨林勇 5刘岩 6朱广伟7
作者信息
- 1. 中国中医科学院中药研究所,北京,100700
- 2. 神威药业集团有限公司,石家庄,051430
- 3. 新疆农业大学食品科学与药学学院,乌鲁木齐,830052
- 4. 山东中医药大学,济南,250355
- 5. 盛实百草药业有限公司,天津,300301
- 6. 河南中医药大学,郑州,450046
- 7. 中国中医科学院中药研究所,北京,100700;中国中医科学院博士后科研流动站,北京,100700
- 折叠
摘要
目的:建立芍药甘草汤(SGD)物质基准及对应实物薄层鉴别方法、超高效液相色谱(UHPLC)特征图谱,并对其进行多成分含量测定,研究量值传递规律,结合出膏率、水分等数据,探讨SGD质量标准.方法:制备18批SGD物质基准和对应实物.薄层鉴别使用1％NaOH制备的硅胶G薄层板,以乙酸乙酯∶甲酸∶冰醋酸∶水(15∶1∶1∶2)为展开剂,以10％的硫酸乙醇溶液为显色剂.使用超高效液相色谱-二极管阵列检测器(UHPLC-DAD)法建立SGD物质基准及对应实物特征图谱,指认特征峰;对饮片、物质基准、对应实物进行多成分含量测定,分析指标成分从饮片-物质基准-对应实物的传递规律.结果:薄层鉴别显示色谱斑点清晰,阴性无干扰.SGD物质基准和对应实物特征图谱相似度均大于0.9,共匹配14个特征峰,指认出6个.指标成分含测结果为:芍药苷、甘草苷、甘草酸在物质基准中分别为0.48～0.83 mg/mL、0.13～0.32 mg/mL、0.31～0.60 mg/mL,在对应实物中分别为 2.21％～3.40％、0.64％～1.59％、1.56％～3.00％.饮片-物质基准的平均转移率分别为芍药苷51.15％、甘草苷36.65％、甘草酸37.03％;物质基准-对应实物的平均转移率分别为芍药苷100.19％、甘草苷99.55％、甘草酸100.49％.结论:通过各项研究结果能够较为全面地对SGD物质基准和对应实物的质量进行把控,实现了对经典名方SGD开发研究的全过程质量控制.
Abstract
Objective:To establish thin-layer chromatography(TLC)identification method and ultra-high performance liquid chro-matography(UHPLC)characteristic chromatogram for the substance benchmark of Shaoyao Gancao Decoction(SGD),and to deter-mine its multi-component content and study the law of value transfer.Additionally,combined with the extraction yield and moisture,the quality standard of SGD was discussed.Methods:A total of 18 batches of SGD substance benchmarks and corresponding objects were prepared.TLC identification:1％sodium hydroxide(NaOH)for preparation of silica gel plate,ethyl acetate:formic acid:gla-cial acetic acid:water at the ratio of 15∶1∶1∶2 as the developing sol vent,and 10％sulfuric acid/ethanol solution as the visualiza-tion reagent.Ultra-high-performance liquid chromatography method with diode array detection(UHPLC-DAD)method was em-ployed to establish the characteristic chromatograms for SGD substance benchmarks and corresponding objects,and identify and the characteristic peaks.The multi-component contents of decoction pieces,substance benchmarks and corresponding objects were de-termined,and the transfer law of the index components from decoction pieces to substance reference to corresponding material was analyzed.Results:The spots in TLC were clear and easy to be identified,and the negative control showed no interference.Both the similarity of substance benchmarks and corresponding objects were greater than 0.9,and 14 characteristic peaks were matched,with 6 identified.The index component test indicated that paeoniflorin,liquiritin,and glycyrrhizic acid in the substance benchmarks were 0.48 to 0.83 mg/mL,0.13 to 0.32 mg/mL,and 0.31 to 0.60 mg/mL,respectively,and 2.21％to 3.40％,0.64％to 1.59％,and 1.56％to 3.00％,respectively in the corresponding objects.The average transfer rates from decoction pieces to substance benchmarks were paeoniflorin 51.15％,liquiritin 36.65％,and glycyrrhizic acid 37.03％,and those from substance benchmarks to corresponding objects were paeoniflorin 100.19％,liquiritin 99.55％,and glycyrrhizic acid 100.49％.Conclusion:Through vari-ous studies,it is possible to comprehensively control the quality of SGD substance benchmarks and corresponding objects and thus achieve the whole-process quality control in the development and research of SGD.
关键词
经典名方/芍药甘草汤/物质基准/对应实物/质量控制/超高效液相色谱-二极管阵列检测器/芍药苷/甘草苷/甘草酸Key words
Classical famous prescription/Shaoyao Gancao Decoction/Substance benchmark/Corresponding object/Quality con-trol/Ultra-high-performance liquid chromatography method with diode array detection(UHPLC-DAD)/Paeoniflorin/Liquiritin/Glycyrrhizic acid引用本文复制引用
基金项目
"重大新药创制"科技重大专项(2018ZX09721005)
中国中医科学院科技创新工程项目(CI2021A04506)
出版年
2023
国家科技期刊平台
NSTL
维普
万方数据