小柴胡胶囊中间体和制剂的色谱检测方法研究(2)——中间体的多成分含量测定方法  

Study on Chromatographic Detection Methods of Intermediates and Preparations of Xiaochaihu Capsules(2)--The Method for Determining the Multi-component Contents of Intermediates

作　　者：丁丰 吴革林[2,3] 钱俊回 刘思含 司徒倩彤 邢冷 瞿海斌 谢永建[2] 龚平 周鹏 龚行楚 DING Feng;WU Ge-lin;QIAN Jun-hui;LIU Si-han;SITU Qian-tong;XING Leng;QU Hai-bin;XIE Yong-jian;GONG Ping;ZHOU Peng;GONG Xing-chu(College of Pharmaceutical Sciences,Zhejiang University,Hangzhou 310058,China;Zhejiang Pralife Pharmaceutical Co.,Ltd.,Taizhou 318000,China;Hangzhou Zansheng Pharmaceutical Co.,Ltd.,Hangzhou 310052,China;Jinhua Institute of Zhejiang University,Jinhua 321016,China;National Key Laboratory of Chinese Medicine Modernization,Hangzhou 310058,China)

机构地区：[1]浙江大学药学院,浙江杭州310058 [2]浙江赞生药业有限公司,浙江台州318000 [3]杭州赞生医药有限公司,浙江杭州310052 [4]浙江大学金华研究院,浙江金华321016 [5]现代中药创制全国重点实验室,浙江杭州310058

出　　处：《分析测试学报》2024年第11期1764-1773,共10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(ZYYCXTD-D-202002);浙江大学科研项目(XY2023024);中央高校基本科研业务费专项资金(226-2022-00226)。

摘　　要：建立了适用于小柴胡胶囊提取浓缩液、稠膏、浸膏粉和制粒药粉4种中间体的分析方法,其中含量测定包括甘草苷、党参炔苷、黄芩苷、汉黄芩苷、黄芩素、甘草皂苷G_(2)、甘草酸、汉黄芩素、柴胡皂苷B_(2)、柴胡皂苷B_(1)共10种成分。采用超高效液相色谱(UHPLC)方法检测,色谱柱为HSS T3柱(100 mm×2.1 mm,1.8μm),以0.05%磷酸水溶液-乙腈为流动相进行梯度洗脱,利用二极管阵列检测器(DAD)在215 nm和254 nm两个波长下进行检测。10种成分在一定质量浓度范围内线性关系良好,r^(2)>0.999;4种中间体供试品溶液的进样精密度、方法重复性符合药典规定,且在24 h内稳定,各成分的加标回收率均符合药典规定。与缺味中间体所得图谱比对后,判断了23个色谱峰的归属。利用所建方法对8批次小柴胡胶囊生产过程中的4种中间体进行了检测。所建立的分析方法稳定、准确、可靠,能为深入了解小柴胡胶囊的制药过程提供技术支持。A quantitative content determination method was established for four intermediates for the extraction of concentrate,thick paste,extract powder and granulation powder from Xiaochaihu Capsules.The quantitative content were including liquiritin,lobetyolin,baicalin,wogonoside,baicalein,licoricesaponin G_(2),glycyrrhizin,wogonin,saikosaponin B_(2) and saikosaponin B_(1).The detected substances were analyzed by ultra-high performance liquid chromatography(UHPLC).HSS T3 chromatographic column(100 mm×2.1 mm,1.8μm)was used.The mobile phase was consisted of 0.05% phosphoric acid solution and acetonitrile.The elution mode was gradient elution.The detection wavelength was set at 215 nm and 254 nm.The linear relationship of 10 quantitative components was good within the certain mass concentration ranges and the correlation coefficients(r^(2))were all more than 0.999.Relative standard deviations(RSDs)of injection precision and method repeatability met the requirements of the pharmacopoeia.The sample solution was stable within 24 hours,and the recoveries of each component met the requirements of the pharmacopoeia.The method was used to determine the attribution of 23 chromatographic peaks after comparing with the obtained by lack of herb intermediates.4 intermediates in 8 batches were used to analyze Xiaochaihu Capsule intermediates by the established method.The established analytical method is stable,accurate and reliable.It provides technical support for the improvement of the pharmaceutical process of Xiaochaihu Capsules.

关 键 词：小柴胡胶囊 中间体 含量测定 浓缩液 超高效液相色谱 

分 类 号：O657.7[理学—分析化学] R284[理学—化学]