养血安神片质量评价方法研究  

Quality Evaluation Methods of Yangxue Anshen Tablets

作　　者：杨美丽[1] 张少杰[1] 杨金蕊[1] 王楠 潘炫屹 付萍萍[1] 徐彬 YANG Meili;ZHANG Shaojie;YANG Jinrui;WANG Nan;PAN Xuanyi;FU Pingping;XU Bin(Baoding Institute for Food and Drug Control,Baoding,Hebei,China 071000;Affiliated Hospital of Hebei University,Baoding,Hebei,China 071000)

机构地区：[1]河北省保定市食品药品检验所,河北保定071000 [2]河北大学附属医院,河北保定071000

出　　处：《中国药业》2023年第13期77-82,共6页China Pharmaceuticals

基　　金：河北省保定市科技计划项目[2241ZF096]。

摘　　要：目的建立养血安神片的质量控制方法。方法采用薄层色谱法对制剂中熟地黄、墨旱莲、首乌藤进行定性鉴别,采用高效液相色谱法测定2,3,5,4'-四羟基二苯乙烯-2-O-β-D-葡萄糖苷(简称二苯乙烯苷)的含量,基于整体控制思路建立波长切换法指纹图谱,采用显微检查法筛查异性有机物,采用原国家食品药品监督管理局批准的补充检验方法筛查非法添加化学成分。结果薄层色谱图中,熟地黄、墨旱莲、首乌藤的特征斑点均显色清晰,且阴性对照无干扰。二苯乙烯苷的质量浓度在0.0393~0.9828μg范围内与峰面积线性关系良好(r=0.9990,n=6);检测限为0.0004μg,定量限为0.0013μg;精密度、稳定性、重复性试验结果的RSD均小于2.0%;平均加样回收率为99.15%,RSD为0.99%(n=6);16批样品每片含二苯乙烯苷0.06~0.57 mg。指纹图谱标定了13个共有峰,相似度为0.771~0.985,指认2号峰为没食子酸、4号峰为原儿茶酸、5号峰为绿原酸、9号峰为二苯乙烯苷。聚类分析结果显示,相似度低于0.80的样品质量存疑。显微检查结果显示,4批样品检查结果异常,提示生产工艺存在问题。安全性考察结果显示,均未检出非法添加化学成分。结论所建立的方法准确、可靠,可用于养血安神片的质量控制及评价。Objective To establish a quality control method for Yangxue Anshen Tablets.Methods Thin-layer chromatography(TLC)was used for the qualitative identification of Rehmanniae Radix Praeparata,Ecliptae Herbs,and Polygoni Multiflori Caulis in the preparation.High-performance liquid chromatography(HPLC)was used for the content determination of 2,3,5,4'-tetrahydroxy stilbene-2-O-β-D-glucoside.Based on the overall control concept,the wavelength-switching method fingerprint was established.Microscopic examination was used to screen for heterologous organic compounds,and the supplementary inspection method approved by the former National Food and Drug Administration was used to screen for illegally added chemical components.Results In the TLC chromatograms,the characteristic spots of Rehmanniae Radix Praeparata,Ecliptae Herbs,and Polygoni Multiflori Caulis were all clear,and the negative control has no interference.The linear range of 2,3,5,4'-tetrahydroxy stilbene-2-O-β-D-glucoside was 0.0393-0.9828μg(r=0.9990,n=6).The limit of detection was 0.0004μg and the limit of quantification was 0.0013μg.The RSDs of precision,stability,and repeatability test results were all lower than 2.0%.The average recovery rate of 2,3,5,4'-tetrahydroxy stilbene-2-O-β-D-glucoside was 99.15%with an RSD of 0.99%(n=6).The content of 2,3,5,4'-tetrahydroxy stilbene-2-O-β-D-glucoside in 16 batches of samples was in the range of 0.06-0.57 mg.A total of 13 common peaks were identified by fingerprints,with a similarity of 0.771-0.985.Peak 2 was identified as gallic acid,peak 4 was identified as protocatechuic acid,peak 5 was identified as chlorogenic acid,and peak 9 was identified as 2,3,5,4'-tetrahydroxy stilbene-2-O-β-D-glucoside.The clustering analysis results showed that the quality of samples with a similarity of less than 0.80 was questionable.The microscopic examination results showed that the results of the four batches of samples were abnormal,indicating that there were problems in the production process.The safety inspection results sho

关 键 词：养血安神片 薄层色谱法 含量测定 指纹图谱 显微检查 质量评价 

分 类 号：R932[医药卫生—生药学] R284.1[医药卫生—药学] R286.0