生发片HPLC-DAD 指纹图谱及指标性成分定量研究  

HPLC-DAD fingerprint and quantitative determination of characteristic components in Shengfa tablets

作　　者：司徒文辉 谢诗婷 刘颖 王永刚[1] 彭维[1] 姚宏亮[1,3] SITU Wen-hui;XIE Shi-ting;LIU Ying;WANG Yong-gang;PENG Wei;YAO Hong-liang(School of Life Sciences,Sun Yat-sen University,Guangdong Engineering and Technology Research Center for Quality and Efficacy Re-Evaluation of Post-Marketed Traditional Chinese Medicine,Guangdong Key Laboratory of Plant Resources,Guangzhou 510275;Guangxi Nanning Baihui Pharmaceutical Group Co.Ltd,Nanning 530032;Guangdong Key Laboratory of Animal Conservation and Resource Utilization,Guangdong Public Laboratory of Wild Animal Conservation and Utilization,Institute of Zoology,Guangdong Academy of Sciences,Guangzhou 510260)

机构地区：[1]中山大学生命科学学院,广东省中药上市后质量与药效再评价工程技术研究中心,广东省热带亚热带植物资源与利用重点实验室,广州510275 [2]广西南宁百会药业集团有限公司,南宁530032 [3]广东省科学院动物研究所,广东省动物保护与资源利用重点实验室,广东省野生动物保护与利用公共实验室,广州510260

出　　处：《中南药学》2022年第1期165-170,共6页Central South Pharmacy

基　　金：广东省科学院科技发展专项(No.2016GDASRC-0104)。

摘　　要：目的建立生发片HPLC-DAD指纹图谱,对其主要特征峰进行归属和指证;同时测定指标性成分二苯乙烯苷、特女贞苷、大豆苷的含量,为更全面评价生发片的质量提供科学依据。方法采用Welch Ultimate XB-C_(18)(4.6 mm×250 mm,5μm)色谱柱,流动相:甲醇(A)-0.1%磷酸(B),梯度洗脱(0~105 min,5%~60%A);柱温:25℃;流速:1.0 mL·min^(-1);进样量:10μL。共收集了28批生发片样品,其中20批生发片用于构建对照指纹图谱,8批生发片用于验证;对指纹图谱10个共有峰成分进行了确证和指认;另外,测定了28批生发片中二苯乙烯苷、特女贞苷、大豆苷的含量。结果10个共有峰分别归属于5味药材:牡丹皮、墨旱莲、黑豆、何首乌、女贞子,通过对照品确证了其中4个成分,采用HPLC-MS法指认了其中6个化学成分;二苯乙烯苷、特女贞苷和大豆苷的含量分别为0.0449~0.3113 mg/片、0.1277~0.8124 mg/片、0.0204~0.0512 mg/片。结论该方法专属性强,操作简便,结果准确,重复性好,可为生发片的质量控制提供可靠的科学依据。Objective To establish an HPLC-DAD fingerprint of Shengfa tablets,identify the main characteristic peaks,and simultaneous quantify 3 major components(stilbene glycoside,specnuezhenide and daidzin),to provide a scientific basis for a more comprehensive evaluation of the quality of Shengfa tablets.Methods Chromatographic fingerprint was obtained with a Welch Ultimate XB-C_(18)(4.6 mm×250 mm,5μm)column,eluted at 25℃with a flow rate of 1.0 mL·min^(-1).The solvent system was composed of methanol(A)-0.1%phosphoric acid(B).The gradient elution program was:0-105 min,5%-60%A.The injection volume was 10μL.Totally 28 batches of Shengfa tablets were collected,20 of which were used as the control fingerprint,and the other 8 for the validation.Ten common peaks were identified or tentatively characterized.The content of stilbene glycoside,specnuezhenide,and daidzin in the 28 batches of Shengfa tablets was determined.Results The 10 common peaks were respectively attributed to moutan cortex,ecliptae herba,sojae semen nigrum,polygoni multiflori radix and ligustri lucidi fructus.Four components were clearly identified by reference substance,and 6 were tentatively characterized by HPLC-MS.The content determination of stilbene glycoside,specnuezhenide and daidzin was between 0.0449~0.3113 mg per tablet,0.1277~0.8124 mg per tablet,and 0.0204~0.0512 mg per tablet,respectively.Conclusion The method is highly specific,accurate and reproducible,which provides a reliable scientific basis for the quality control of Shengfa tablets.

关 键 词：生发片 高效液相色谱法 指纹图谱 含量测定 

分 类 号：R286[医药卫生—中药学] O657.72[医药卫生—中医学]