基于双标多测法辅助HPLC的肿节风配方颗粒的多组分分析  

Multi-component analysis of Herba Sarcandrae dispensing granules based on TRSDMC assisted HPLC

作　　者：林燕翔 黄博 罗轶 孙磊[2] 马双成[2] 谢培德 LIN Yan-xiang;HUANG Bo;LUO Yi;SUN Lei;MA Shuang-cheng;XIE Pei-de(Guangxi Institute for Food and Drug Control,Key Laboratory of Quality Detection and Evaluation of Chinese Medicinal Materials,National Medical Products Administration,Nanning 530021,China;National Institutesfor Food and Drug Control Beijing 100050,China)

机构地区：[1]广西壮族自治区食品药品检验所,国家药品监督管理局中药材质量检测与评价重点实验室,南宁530021 [2]中国食品药品检定研究院,北京100050

出　　处：《药物分析杂志》2022年第3期402-410,共9页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立肿节风配方颗粒中新绿原酸、绿原酸、隐绿原酸、咖啡酸、异嗪皮啶、迷迭香酸等6个多指标成分含量测定方法,探索双标线性多测法在色谱峰定性及采用相对校正因子定量的可行性。方法:采用十八烷基键合硅胶为填充剂的液相色谱柱,以乙腈-0.1%磷酸水溶液为流动相梯度洗脱。在17根不同的C_(18)色谱柱上测定肿节风配方颗粒6个成分的实际保留时间,计算各成分在各色谱柱保留时间的平均值,得到各成分的标准保留时间,选取绿原酸和异嗪皮啶2个成分作为双标化合物,使用双标线性校正法准确定位各成分色谱峰,预测成分在未知色谱柱的保留时间并进行方法学验证。以绿原酸为参照物,计算绿原酸与其余各成分的相对校正因子,对各成分进行定量。结果:不同企业的样品中新绿原酸、绿原酸、隐绿原酸、咖啡酸、异嗪皮啶、迷迭香酸的含量范围分别为0.482~0.625、0.44~1.30、0.298~0.452、0.808~1.502、1.24~2.79、1.10~3.54 mg·g^(-1)。双标线性校正法能够准确地预测待测成分在未知色谱柱上的保留时间,且预测结果与实际值的偏差小于相对保留时间法,对色谱峰的定位比相对保留时间法更加精准;以相对校正因子法和常规外标法的定量结果显示二者无显著性差异。结论:双标多测法作为一种新的替代对照品方法,能较好地运用于肿节风配方颗粒多成分的测定中,值得进一步研究完善和推广。Objective:To establish a multi-component analysis method of Herba Sarcandrae dispensing granules for determination of six ingredients including neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,caffeic acid,isofraxidin and rosmarinic acid by HPLC,and to explore the feasibility of the method of two referencesubstances for determination of multiple components(TRSDMC)in chromatographic peak characterization and relative correction factor quantification.Methods:A liquid chromatography column using octadecyl bonded silica gel was adopted as the solid phase,with acetonitrile-0.1%phosphoric acid as the mobile phase in gradient elution.The retention time of the five ingredients in Herba Sarcandrae dispensing granules was determined on 17 different C_(18) columns by HPLC.The standard retention time(SRT)was calculated.Both chlorogenic acid and isofraxidin were taken as the linear calibration standards.Two reference substances were used for accurately locating the peaks of each ingredient,forecasting the retention time of the other three ingredients when the method was established and validated.Meanwhile,chlorogenic acid was chosen as reference substance for the determination of relative correction factor in order to calculate the content of each component.Results:The content ranges of neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,caffeic acid,isofraxidin and rosmarinic acid in samples from different enterprises were 0.482-0.625 mg·g^(-1),0.44-1.30 mg·g^(-1),0.808-1.502 mg·g^(-1),0.298-0.452 mg·g^(-1),1.24-2.79 mg·g^(-1) and 1.10-3.54 mg·g^(-1),respectively.Conclusion:TRSDMC can be used in the determination of multiple components of Herba Sarcandrae dispensing granules as a new replacement method of chemical reference substance and is worth further research and improvement.

关 键 词：肿节风配方颗粒 隐绿原酸 绿原酸 新绿原酸 咖啡酸 异嗪皮啶 迷迭香酸 双标线性校正法 替代对照品 多组分分析 含量测定 

分 类 号：R917[医药卫生—药物分析学]