伤科灵喷雾剂特征图谱及4个成分含量测定方法的建立  

Establishment of characteristic chromatogram and determination method of four components in Shangkeling spray

作　　者：支苑 肖婷 何旭洪 朱志军 曾丽 陶玲 沈祥春 茅向军 ZHI Yuan;XIAO Ting;HE Xuhong;ZHU Zhijun;ZENG Li;TAO Ling;SHEN Xiangchun;MAO Xiangjun(Guizhou Engineering Center of High Efficacy Application of Natural Medicinal Resources/High Educational Key Laboratory of Natural Medicinal Pharmacology and Drug Gability/Guizhou Medical University-Guiyang Joint Laboratory/Key Lab of Optimal Utilization of Natural Medicine Resources/School of Pharmacy,Guizhou Medical University,Guiyang 550025,China;Guizhou Hengba Pharmaceutical Co.,Ltd.,Guiyang 550008,China;Guizhou Drug Evaluation and Inspection Center,Guiyang 550081,China)

机构地区：[1]贵州医科大学贵州省天然药物资源高效利用工程中心/贵州省普通高等学校天然药物药理与成药性评价特色重点实验室/贵州医科大学-贵阳市联合重点实验室/天然药物资源优效利用重点实验室/贵州医科大学药学院,贵阳550025 [2]贵州恒霸药业有限责任公司,贵阳550008 [3]贵州省药品审评查验中心,贵阳550081

出　　处：《中国药房》2022年第19期2369-2372,2377,共5页China Pharmacy

基　　金：国家自然科学基金资助项目(No.82060729);贵州省科技计划项目(No.黔科合基础-ZK[2021]一般535,No.黔科合平台人才[2017]5802);贵州医科大学国家自然科学基金培育项目(No.19NSP074)。

摘　　要：目的建立伤科灵喷雾剂的定性、定量分析方法,为伤科灵喷雾剂的整体质量控制奠定基础。方法以11批伤科灵喷雾剂为样品,采用高效液相色谱(HPLC)法进行测定。色谱条件:采用Ultimate?XB-C18色谱柱,以乙腈-0.1%磷酸水溶液为流动相进行梯度洗脱;检测波长为210 nm;柱温为35℃;流速为1.0 mL/min。采用《中药色谱指纹图谱相似度评价软件(2012版)》建立11批样品的HPLC特征图谱并进行相似度分析,通过与对照品图谱比对进行色谱峰的指认。采用HPLC法测定样品中苦参碱、氧化苦参碱、东莨菪内酯、异嗪皮啶的含量。结果11批样品共标定了18个共有特征峰,指认了其中4个共有特征峰,分别为峰2(苦参碱)、峰3(氧化苦参碱)、峰6(东莨菪内酯)、峰7(异嗪皮啶)。11批样品的特征图谱与对照特征图谱R的相似度均≥0.990。含量测定方法学考察结果均符合相关要求,11批样品中苦参碱、氧化苦参碱、东莨菪内酯、异嗪皮啶的含量分别为14.48~44.86、32.53~69.76、11.28~20.96、10.36~22.49μg/mL。结论本研究成功建立了伤科灵喷雾剂HPLC特征图谱和4个指标成分的定量分析方法,可用于该制剂的质量控制。OBJECTIVE To establish a method for qualitative and quantitative analysis of Shangkeling spray,which can be a certain foundation for the overall quality evaluation of Shangkeling spray.METHODS Eleven batches of Shangkeling spray were determined by high performance liquid chromatography(HPLC).The separation was performed on Ultimate?XB-C18column with mobile phase consisted of acetonitrile-0.1% phosphoric acid(gradient elution) at the flow rate of 1.0 mL/min.The detection wavelength was set at 210 nm,and column temperature was 35 ℃.Similarity Evaluation Software of Chromatographic Fingerprint of Traditional Chinese Medicine(2012 edition)was used for the establishment of HPLC characteristic chromatogram and similarity analysis;the chromatographic peaks were identified by comparing with the chromatogram of the reference substance.The contents of matrine,oxymatrine,scopoletin and isoazinopyridine were determined by HPLC.RESULTS Totally 18 common characteristic peaks were demarcated for 11 batches of samples,4 of them were identified,i.e.peak 2(matrine),peak 3(oxymatrine),peak 6(scopoletin),peak 7(isoazinopyridine).The similarity between the characteristic chromatogram of 11 batches of samples and the control characteristic chromatogram R was ≥0.990.The results of content determination methodology conformed to the relevant requirements.The contents of matrine,oxymatrine,scopoletin and isoazinopyridine in 11 batches of Shangkeling spray were14.48-44.86,32.53-69.76,11.28-20.96 and 10.36-22.49 μg/m L,respectively.CONCLUSIONS HPLC characteristic chromatogram and quantitative analysis method of 4 indicator components are successfully established in this study,which can be used to evaluate the quality of this preparation.

关 键 词：伤科灵喷雾剂 高效液相色谱法 特征图谱 苦参碱 氧化苦参碱 东莨菪内酯 异嗪皮啶 

分 类 号：R917[医药卫生—药物分析学]