UPLC法同时测定乙肝宁颗粒中的10种指标成分  

Simultaneous determination of 10 active ingredients in Yiganning Granules by UPLC

作　　者：王蕾[1,2] 李果果 韩旭 WANG Lei;LI Guo-guo;HAN Xu(Tianjin Second People's Hospital,Tianjin 300192,China;Tianjin Institute of Hepatology,Tianjin 300192,China;Tianjin University of Traditional Chinese Medicine,Tianjin 301617,China)

机构地区：[1]天津市第二人民医院,天津300192 [2]天津市肝病医学研究所,天津300192 [3]天津中医药大学,天津301617

出　　处：《中草药》2020年第22期5754-5759,共6页Chinese Traditional and Herbal Drugs

基　　金：天津市科技计划项目(No.18YFZCSY00015)。

摘　　要：目的建立同时测定乙肝宁颗粒中10种指标成分的UPLC方法,为乙肝宁颗粒的质量控制提供科学依据。方法采用UPLC-DAD法,色谱柱为Acquity UPLC BEH C18(100 mm×2.1 mm,1.7μm);流动相为乙腈-甲醇-0.15%磷酸水溶液,梯度洗脱,体积流量0.3 mL/min,柱温45℃,进样量2μL。结果同时测定了乙肝宁颗粒中绿原酸、白术内酯I、芍药苷、毛蕊异黄酮苷、二苯乙烯苷、咖啡酸、川楝素、山柰素、丹皮酚、丹参酮IIA 10种有效成分,各成分在考察的质量浓度范围内线性关系良好(r≥0.9990),检测限与定量限分别为0.006~0.017μg/mL和0.017~0.510μg/mL,平均加样回收率为98.8%~102.5%,RSD为1.13%~5.37%。通过对16个批次样品的测定,上述10种成分的平均质量浓度依次为(5.724±0.017)、(0.273±0.003)、(0.854±0.005)、(1.228±0.004)、(0.496±0.003)、(1.287±0.004)、(0.137±0.004)、(3.624±0.014)、(7.366±0.032)、(1.754±0.005)mg/g。结论所建立的UPLC方法简单、专属、灵敏,可用于乙肝宁颗粒质量控制和评价。Objective To establish a UPLC method to simultaneously determine 10 active ingredients in Yiganning Granules(YG)and provide scientific basis for the quality control,evaluation and standard revision of YG preparations.Methods A UPLC method was used with an Acquity UPLC BEH C18 column(100 mm×2.1 mm,1.7μm).The mobile phase was acetonitrile-mehanol-0.15%phosphoric acid solution with gradient elution.The flow rate was 0.3 mL/min.The column temperature was 45℃.The injection volume was 2μL.Results Ten active ingredients(chlorogenic acid,atractylenolide I,paeoniflorin,calycosin 7-O-β-Dglucopyranoside,stilbene glycoside,caffeic acid,toosendanin,kaempferol,paeonol and tanshinoneⅡA)in YG were simultaneously determined.The linearity was good(r≥0.9990),the limit of detection and quantification were 0.006—0.017μg/mL and 0.017—0.510μg/mL.The average recoveries were 98.8%—102.5%with RSDs of 1.13%—5.37%.Through the determination of 16 batches of samples,the average content of the above 10 ingredients was in turn(5.724±0.017),(0.273±0.003),(0.854±0.005),(1.228±0.004),(0.496±0.003),(1.287±0.004),(0.137±0.004),(3.624±0.014),(7.366±0.032)and(1.754±0.005)mg/g,respectively.Conclusion The established UPLC method is simple,specific,sensitive,stable,precise,accurate,and reproducible,which can be used for quality control and evaluation of YG.

关 键 词：乙肝宁颗粒 UPLC 绿原酸 白术内酯I 芍药苷 毛蕊异黄酮苷 二苯乙烯苷 咖啡酸 川楝素 山柰素 丹皮酚 丹参酮IIA 

分 类 号：R286.02[医药卫生—中药学]