摘要
目的:建立糖肾地黄汤的HPLC指纹图谱及多指标成分含量测定方法,为糖肾地黄汤的质量控制及评价提供参考。方法:采用Symmetry?C18柱(250 mm×4.6 mm,5μm);流动相为乙腈-0.1%磷酸水溶液,梯度洗脱;流速1.0 mL·min^(–1);柱温30℃;检测波长240 nm。采用《中药色谱指纹图谱相似度评价系统》(2012版)对10批样品的HPLC指纹图谱进行相似度评价,同时对其进行含量测定。结果:建立10批糖肾地黄汤的指纹图谱相似度均大于0.99,确认了20个共有峰,其中1、6、7、10、14、17、18、19(丹皮酚)号峰归属于牡丹皮,2、3、4、5(莫诺苷)、8(马钱子苷)、9、13号峰归属于山茱萸,11号峰(毛蕊异黄酮苷)归属于黄芪,15、16(丹酚酸B)、20(丹参酮ⅡA)归属于丹参,12号峰为山茱萸与牡丹皮;以莫诺苷、马钱子苷、毛蕊异黄酮苷、丹皮酚、丹参酮ⅡA和丹酚酸B 6项指标建立其质量控制标准,各批次样品中莫诺苷、马钱子苷、毛蕊异黄酮苷、丹皮酚、丹参酮ⅡA和丹酚酸B质量密度分别为69.18~70.21、81.82~82.84、4.31~4.32、346.33~347.26、189.37~190.58、8.39~8.47μg·mL^(–1)。结论:所建立的糖肾地黄汤指纹图谱和含量测定方法技术简单、灵敏度高、重复性好,可用于糖肾地黄汤的质量评价。
OBJECTIVE To establish the high performance liquid chromatography(HPLC)fingerprint and formulate a multi-indicator protocol for measuring the contents of Tangshen Dihuang Decoction(TDD)to provide references for its quality control(QC)and evaluations.METHODS Separation was performed on Symmetry®C18(250 mm×4.6 mm,5μm)at 30℃and eluted with acetonitrile-0.1%phosphoric acid at a flow rate of 1.0 mL·min^(–1),and a detection wavelength of 240 nm.Simi⁃larity Evaluation System of Chromatographic Fingerprints of Traditional Chinese Medicine(Edition 2012)was utilized for evalu⁃ating the similarity of HPLC fingerprints of 10 batches of samples and determining their specific contents.RESULTS HPLC fin⁃gerprint of 10 batches of TDD was performed.All similarities were greater than 0.99.A total of 20 common peaks were identi⁃fied.Peaks 1/6/7/10/14/17/18/19(paeonol)were attributed to peony bark,peaks 2/3/4/5(morroniside),peak 8(loganin),peaks 9/13 Corni Fructus,peak 11(calycosin-7-glucoside)Astragalus membranaceus,peaks 15/16(salvianolic acid B)and peak 20(tanshinoneⅡA)Salvia miltiorrhiza.Peak 12 was composed of Cornus officinalis and peony bark.QC standards were estab⁃lished by morroniside,loganin,calycosin-7-glucoside,paeonol,salvianolic acidⅡA and salvianolic acid B.Mass fractions of morroniside,loganin,calycosin-7-glucoside,paeonol,salvianolic acidⅡA and salvianolic acid B in each batch were(69.18−70.21),(81.82−82.84),(4.31−4.32),(346.33−347.26),(189.37−190.58)and(8.39−8.47)μg·mL^(–1)respectively.CONCLUSION Fingerprinting and content determination of TDD are simple,sensitive and reproducible.It may be employed as rationales for follow-up QC of TDD.
作者
刘诗琪
杨超茅
苟小军
LIU Shiqi;YANG Chaomao;GOU Xiaojun(Department of Geriatrics,Affiliated Baoshan Hospital,Shang-hai University of Traditional Chinese Medicine,Shanghai 201999,China;Central Laboratory,Baoshan District Hospital of Integrated Traditional Chinese&Western Medicine,Shanghai 201999,China)
出处
《中国医院药学杂志》
CAS
北大核心
2024年第16期1890-1896,共7页
Chinese Journal of Hospital Pharmacy
基金
上海市卫生健康委员会科研课题(编号:20214Y0195)
宝山区科学技术委员会科技创新专项资金医学卫生项目(编号:20-E-14)
宝山区卫生健康委优青(育才)计划项目(编号:BSWSYC-2023-05)。
关键词
糖肾地黄汤
高效液相色谱
指纹图谱
含量测定
Tangshen Dihuang Decoction
high performance liquid chromatography
fingerprint
content determination
