双标多测法在脑心通胶囊5个成分含量测定中的应用  

Assay of Five Components in Naoxintong Capsules by Method Using Two Reference Substances for Determination of Multiple Components

作　　者：唐玉洁 高原 TANG Yu-jie;GAO Yuan(Affiliated Hospital of Hubei University of Arts and Science(Xiangyang Central Hospital),Xiangyang 441021,China)

机构地区：[1]湖北文理学院附属医院(襄阳市中心医院),湖北襄阳441021

出　　处：《食品与药品》2022年第6期560-566,共7页Food and Drug

摘　　要：目的 建立脑心通胶囊中羟基红花黄色素A、芍药苷、阿魏酸、丹酚酸B和藁本内酯5个成分的双标多测法,验证该方法在脑心通胶囊质量评价中应用的准确性和可行性。方法 采用高效液相色谱(HPLC)法,以乙腈为流动相A,0.5%甲酸溶液为流动相B,梯度洗脱,流速为1 ml/min,检测波长403 nm(羟基红花黄色素A)、240 nm(芍药苷)、280 nm(丹酚酸B)、324 nm(阿魏酸和藁本内酯),柱温35℃。采用6根不同型号的C18色谱柱,测定脑心通胶囊5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,选取羟基红花黄色素A(峰1)、藁本内酯(峰5)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,预测各成分在未知色谱柱的保留时间并进行方法学验证。以阿魏酸为参照物,计算其余各成分的相对校正因子,对各成分进行定量。结果 双标线性校正法能准确地预测待测组分在未知色谱柱上的保留时间。羟基红花黄色素A、芍药苷、丹酚酸B和藁本内酯对于阿魏酸的相对校正因子分别为0.728,1.094,1.553和1.339,其RSD均小于1%。各成分含量计算值和实测值无显著差异。结论 双标多测法同时测定脑心通胶囊中5个成分可行且准确。Objective To establish a method using two reference substances for determination of multiple components(TRSDMC) and determine five components(hydroxyl-saffior yellowyellow A,ferulic acid,paeonifiorin,salvianolic acid B and ligustilide) of Naoxintong Capsules,and to verify the accuracy and feasibility of the method in the quality evaluation of Naoxintong Capsules.Methods HPLC was used,using acetonitrile as mobile phase A and 0.5 %formic acid aqueous solution as mobile phase B of gradient elution.The fiow rate was 1 ml/min.The determination wavelengths were 403 nm for hydroxyl-safflor yellow A,240 nm for paeoniflorin,280 nm for salvianolic acid B,and 324 nm for ferulic acid and ligustilide.The column temperature was 35 ℃.The actual retention time of five components in Naoxintong Capsules on six different types of C18 chromatographic columns was determined.The average retention time of each component on each column was calculated to obtain the standard retention time of each component.Hydroxyl-safflor yellow A(peak 1) and ligustilide(peak 5) were selected as the reference substances for the determination.The chromatographic peaks of each component were accurately located by linear calibration using two reference substances,and the position of each component in unknown chromatographic column could be predicted by the same method.The methodological validation was conducted.Taking ferulic acid as reference,the relative correction factors of the other components were calculated and the components were quantified.Results TRSDMC can accurately predict the retention time of the components to be tested on unknown columns.The relative correction factors of hydroxyl-saffior yellow A,paeonifiorin,salvianolic acid B and ligustilide for ferulic acid were 0.728,1.094,1.553 and 1.339,respectively,with RSDs less than 1 %.There was no significant difference between the contents obtained by TRSDMC and external standard method for each component.Conclusion TRSDMC for simultaneous determination of five components in Naoxintong Capsul

关 键 词：脑心通胶囊 双标多测法 色谱峰 相对校正因子 羟基红花黄色素A 芍药苷 阿魏酸 丹酚酸B 藁本内酯 

分 类 号：R284.1[医药卫生—中药学]