肝肾颗粒的制备、质量标准及指纹图谱研究
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篇名: 肝肾颗粒的制备、质量标准及指纹图谱研究
TITLE:
摘要: 目的:制备肝肾颗粒,并初步拟定其质量标准,建立其高效液相色谱(HPLC)指纹图谱。方法:以送料速度、压辊速度、压辊压力、压辊间隙为考察因素,颗粒成型率为评价指标,采用单因素试验及正交试验优化肝肾颗粒干法制粒工艺。根据2015年版《中国药典》(四部)(以下简称“药典”)对其水分、粒度、溶化性进行测定;采用薄层色谱定性鉴别肝肾颗粒中的枸杞子、黄芪、党参;采用HPLC法定量测定肝肾颗粒中甜菜碱、毛蕊异黄酮葡萄糖苷、党参炔苷的含量,并绘制10批肝肾颗粒的指纹图谱。结果:肝肾颗粒干法制粒的最优工艺为送料速度25 r/min、压辊转速8 r/min、压辊压力7 MPa、压辊间隙1.1 mm,所制颗粒成型率为85.53%。肝肾颗粒的水分、粒度、溶化性均符合药典标准;枸杞子、黄芪、党参供试品薄层色谱在对照品色谱相应的位置上显相同颜色的斑点;甜菜碱的进样量线性范围为4.32~8.64 μg,毛蕊异黄酮葡萄糖苷、党参炔苷的检测质量浓度线性范围分别为5~30、10~60    μg/mL,精密度、重复性、稳定性(24 h)试验的RSD均<2.0%(n=5),平均回收率分别为97.02%、99.25%、101.04%(RSD均<1.7%,n=6或9),含量分别为4.298、0.054、0.025 mg/g;10批肝肾颗粒样品HPLC指纹图谱与对照指纹图谱相似度均>0.95。结论:优化后的肝肾颗粒制粒工艺稳定、可行,所建立的质量标准及HPLC指纹图谱可为肝肾颗粒的质量控制提供依据。
ABSTRACT: OBJECTIVE: To prepare Ganshen granules, formulate its quality standards primarily and establish its HPLC fingerprint. METHODS: Using feeding speed, roller speed, roller pressure and roller clearance as factor, grain forming rate as index, single factor test and orthogonal test were used to optimize the granulation technology of Ganshen granules. According to 2015 edition of Chinese Pharmacopeia (part Ⅳ) (shorted for pharmacopeia), moisture, granulation and dissolution were determined. TLC was used for the qualitative identification of Lycium barbarum, Astragalus membranaceus, Codonopsis pilosula in the Ganshen granules. HPLC method was used to determine the contents of betaine, calycosin-7-glucoside and lobetyolin in Ganshen granules. Fingerprints of 10 batches of Ganshen granules were drawn. RESULTS: The optimal dry granulation technology of Ganshen granules included that 25 r/min feeding speed, 8 r/min roller speed, 7 MPa roller pressure and 1.1 mm roller clearance, The grain forming rate is 85.83%. The moisture, granulation and solubility of Ganshen granule were all in line with pharmacopeia standard. TLC of L. barbarum, A. membranaceus and C. pilosula showed the same color spots on the corresponding positions of the reference chromatogram. The linear range of sample mass of betaine is 4.32-8.64 μg, and the linear range of mass concentration of calycosin-7-glucoside and lobetyolin were 5-30 and 10-60 μg/mL, respectively. RSDs of precision, reproducibility and stability tests (24 h) were all lower than 2.0% (n=5). Average recoveries were 97.02%, 99.25% and 101.04% (all RSD<1.7%, n=6 or n=9). The contents of them were 4.298、0.054、0.025 mg/g, respectively. The similarity of HPLC fingerprints of 10 batches of Ganshen granules to control fingerprint was higher than 0.95. CONCLUSIONS: The optimal granulation technology of Ganshen granule is stable and feasible, and established quality standard and HPLC fingerprint can provide reference for quality control of Ganshen granule.
期刊: 2019年第30卷第21期
作者: 程杰,张屏,包保全,梁雨娜,唐雨晨,刘德旺
AUTHORS: CHENG Jie,ZHANG Ping,BAO Baoquan,LIANG Yuna,TANG Yuchen,LIU Dewang
关键字: 肝肾颗粒;干法制粒;制备;正交试验;含量测定;质量标准;指纹图谱
KEYWORDS: Ganshen granules; Dry granulation; Preparation; Orthogonal test; Content determination; Quality standard; Fingerprint
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