槐角炭质量标准提升研究_牛艳.pdf

29 Okamoto W,Okamoto I,Yoshida T,et al.Identification of c-Src as a potential therapeutic target for gastric cancer and of MET activation as a cause of resistance to c-Src inhibitionJ.Mol Cancer Ther,2010,9(5):1188-1197.30 Lin P,Cheng T,Ma S,et al.Bacillus bombysepticus alpha-toxin binding to G protein-coupled receptor kinase 2 regulates cAMP/PKA signaling pathway to induce host deathJ.PLoS Pathog,2016,12(3):e1005527.31 Peng R,Zhao G X,Li J,et al.Auphen and dibutyryl cAMP suppress growth of hepatocellular carcinoma by regulating expression of aquaporins 3 and 9 in vivoJ.World J Gastroenterol,2016,22(12):3341-3354.32 Abudoureyimu A,Muhemaitibake A.Arsenic trioxide regulates gastric cancer cell apoptosis by mediating cAMPJ.Eur Rev Med Pharmacol Sci,2017,21(3):612-617.33 王恩宇,王景辉,丁芮,等.“黄连-半夏”药对治疗胃癌的网络药理学研究和实验验证J.中国中药杂志,2020,45(8):1779-1788.34 Pearce L R,Komander D,Alessi D R.The nuts and bolts of AGC protein kinasesJ.Nat Rev Mol Cell Biol,2010,11(1):9-22.35 Wu Y,Yuan M,Su W,et al.The constitutively active PKG II mutant effectively inhibits gastric cancer development via a blockade of EGF/EGFR-associated signalling cascadesJ.Ther Adv Med Oncol,2018,10:1758834017751635.36 Wu Y,Yao X,Zhu M,et al.PKG II reverses HGF-triggered cellular activities by phosphorylating serine 985 of c-Met in gastric cancer cellsJ.Oncotarget,2016,7(23):34190-34200.37 Wu Y,Chen Y,Qu R,et al.Type II cGMP-dependent protein kinase inhibits EGF-triggered signal transduction of the MAPK/ERK-mediated pathway in gastric cancer cellsJ.Oncol Rep,2012,27(2):553-558.收稿日期：2022-03-04基金项目：中药配方颗粒质量识别与控制关键技术研究及产业化应用（编号：2021CXGC010511）；泉城产业领军人才支 持计划创新团队项目（编号：MRJT2105）作者简介：牛艳，主管中药师，主要从事中药质量评价及标准制修订，E-mail:*通讯作者：林永强，主任药师，主要从事中药质量控制及标准制修订，E-mail: 槐角炭质量标准提升研究牛 艳，许丽丽，穆向荣，林永强*（山东省食品药品检验研究院，国家药品监督管理局胶类产品质量评价重点实验室，中药标准创新与质量评价工程实验室，中药配方颗粒共性技术山东省工程研究中心，山东 济南 250101）摘 要:目的 提升槐角炭饮片的地方标准。方法 收集槐角炭饮片18批。采用显微镜对样品粉末显微特征进行观察；采用高效液相色谱法（HPLC）对样品进行定性鉴别；建立槐角炭的特征图谱；参照中国药典2020年版测定样品的水分、总灰分、酸不溶性灰分、重金属及有害元素、浸出物；采用HPLC测定槐角苷的含量。结果 18批样品的显微特征基本相同，重复性较好；HPLC色谱图中均呈现与槐角苷对照品相应的色谱峰；确定了10个共有峰作为指纹图谱的特征峰；水分的平均值为5.5%，灰分的平均值为4.7%，醇溶性浸出物的平均值为58.0%，酸不溶性灰分及重金属测定结果较低；槐角苷进样量在0.10161.016 g范围内与峰面积线性关系良好，精密度、重复性试验的RSD均小于2%，平均回收率为103.3%，RSD为1.02%（n=6）。结论 建议在槐角炭饮片的地方质量标准中增加显微鉴别、液相色谱鉴别、特征图谱、水分（不得过10.0%）、灰分（不得过6.0%）、浸出物（不得低于40.0%）及含量测定（槐角苷不得少于2.0%）项，暂不列入“酸不溶性灰分、重金属及有害元素”项。该研究结果可为槐角炭饮片地方质量标准的修订提供参考。关键词：槐角炭；地方质量标准；显微鉴别；特征图谱；高效液相色谱法中图分类号：R284 文献标识码：A 文章编号：1672-979X（2023）01-0025-06DOI：10.3969/j.issn.1672-979X.2023.01.005Improvement of Quality Standard of Sophorae Fructus CarbonisataNIU Yan,XU Li-li,MU Xiang-rong,LIN Yong-qiang（Key Laboratory for Quality Evaluation of Gel Products of National Medical Products Administration,Shandong 食品与药品 Food and Drug 2023年第25卷第1期 25Engineering Laboratory for Standard Innovation and Quality Evaluation of TCM,Shandong Engineering Research Center for Generic Technology of Traditional Chinese Medicine Formula Granules,Shandong Institute for Food and Drug Control,Jinan 250101,China）Abstract:Objective To improve the local standard of of Sophorae Fructus Carbonisata decoctionpieces.Methods A total of 18 batches of Sophorae Fructus Carbonisata were collected.The microscopic characteristics of the samples were identified by microscope.The samples were qualitatively identified by high performance liquid chromatography(HPLC).The HPLC characteristic spectrum of Sophorae Fructus Carbonisata was established.The moisture,total ash,acid insoluble ash,heavy metals and harmful elements,and the leachable chemicles of the samples were determined according to the Chinese Pharmacopoeia(2020 Edition)The content of sophoricoside was determined by HPLC.Results The microscopic characteristics of 18 batches of Sophorae Fructus Carbonisata were essentially the same,and the repeatability was good.The chromatographic peak of sophoricoside was found in the liquid chromatogram of all the samples.Ten chromatographic peaks were selected as common peaks in the fingerprint.The average contents of moisture,total ash and alcohol soluble extract were 5.5%,4.7%,58.0%,respectively.The contents of acid insoluble ash,heavy metals and harmful elements were very low.The linear range of sophoricoside was 0.1016-1.106 g.The RSDs of precision and repeatability tests were less than 2%,and the average recovery of sophoricoside was 103.3%with RSD of 1.02%(n=6).Conclusion It is suggested that the items of microscopic identification,HPLC identification,moisture limit(not more than 10.0%),ash limit(not more than 6.0%),alcohol soluble extract limit(not less than 40.0%)and content determination(the content of sophoricoside not less than 2.0%)should be added to the local quality standard of Sophorae Fructus Carbonisata,but the items of“acid insoluble ash,heavy metals and harmful elements”should not be included temporarily.This study provides reference for the revision of the local quality standard of Sophorae Fructus Carbonisata.Key Words:Sophorae Fructus Carbonisata;local quality standard;microscopic identification;characteristic