元胡止痛口服液药材、中间体及制剂的定量指纹图谱方法研究  

Study on Quantitative Fingerprints for Raw Medicinal Materials,Intermediates and Preparations of Yuanhu Zhitong Koufuye

作　　者：颉佳乐 兰婧 曹智铭 关建丽 王毅[1,2,4] 龚行楚 XIE Jia-le;LAN Jing;CAO Zhi-ming;GUAN Jian-li;WANG Yi;GONG Xing-chu(College of Pharmaceutical Sciences,Zhejiang University,Hangzhou 310058,China;Innovation Institute for Artificial Intelligence in Medicine,Zhejiang University,Hangzhou 310018,China;Henan Fusen Pharmaceutical Co.,Ltd.,Nanyang 474450,China;State Key Laboratory of Component-Based Chinese Medicine,Innovation Center in Zhejiang University,Hangzhou 310058,China)

机构地区：[1]浙江大学药学院,浙江杭州310058 [2]浙江大学智能创新药物研究院,浙江杭州310018 [3]河南福森药业有限公司,河南南阳474450 [4]组分中药国家重点实验室浙江大学交叉创新中心,浙江杭州310058

出　　处：《分析测试学报》2023年第8期984-991,共8页Journal of Instrumental Analysis

基　　金：国家中医药管理局创新团队与人才支持计划项目(ZYYCXTD-D-202002);河南省重大科技专项项目(201111310800);中央高校基本科研业务费专项资金资助项目(226-2022-00226)。

摘　　要：建立了适用于元胡止痛口服液原料药材、中间体及制剂中若干生物碱类成分的定量指纹图谱方法。采用DIKMA Diamonsil Plus C18-A色谱柱(4.6 mm×250 mm,5μm),以0.04%乙酸铵溶液(冰醋酸调至pH4.0,A)-乙腈(B)为流动相进行梯度洗脱,在280 nm下进行检测。指纹图谱中含共有峰7个,其精密度、重复性、稳定性的相对标准偏差(RSD)均小于5.0%。对延胡索乙素、去氢延胡索甲素进行定量分析,其分别在6.15~123μg/mL和10.15~203μg/mL范围内线性关系良好,相关系数(r^(2))> 0.999,进样精密度、方法重复性的RSD均小于5.0%,供试品溶液在24 h内稳定。延胡索乙素、去氢延胡索甲素在低、中、高3个加标水平下的平均回收率为89.6%~107%,RSD小于3.0%。所建立的分析方法稳定、准确、可靠,能够对药材、中间体及制剂中的中等极性成分进行检测,可用于考察工业生产中元胡成分的量值传递情况,从而为改进元胡止痛口服液制药过程控制水平提供技术支持。A quantitative fingerprint method was established for several alkaloids in the raw medicinal materials,intermediates and preparations of Yuanhu Zhitong Koufuye.A DIKMA Diamonsil Plus C18-A chromatographic column(4.6 mm×250 mm,5µm)was used for separation with gradient elution.The mobile phase was consisted of solvent A(0.04%ammonium acetate solution,glacial acetic acid was used to regulate the pH value to 4.0)and solvent B(acetonitrile).The detection wavelength was 280 nm.There were 7 common peaks in the fingerprint.The relative standard deviations(RSDs)of precision,re-peatability and stability were all less than 5.0%.The linear relationships of tetrahydropalmatine and dehy-drocorydaline were good within the range of 6.15-123µg/mL and 10.15-203µg/mL,respectively.The correlation coefficients(r^(2))were more than 0.999,and RSDs for injection precision and method re-peatability were less than 5.0%.The sample solution was stable within 24 h.The average recoveries for tetrahydropalmatine and dehydrocorydaline at low,medium and high levels ranged from 89.6%to 107%,with RSDs less than 3.0%.The established method is stable,accurate and reliable,and could be used to detect the medium polar components in the medicinal materials,intermediates and preparations,in-vestigating the quantity and measure value transfer of the components in Corydalis Rhizoma during indus-trial production.The method provides a technical support for improving the control level for pharmaceutical process of Yuanhu Zhitong Koufuye.

关 键 词：定量指纹图谱 含量测定 元胡止痛口服液 延胡索乙素 去氢延胡索甲素 

分 类 号：O657.63[理学—分析化学] R283[理学—化学]