首页|双标多测法在枣仁安神颗粒6个成分含量测定中的应用

双标多测法在枣仁安神颗粒6个成分含量测定中的应用

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目的 建立枣仁安神颗粒中斯皮诺素、6'''-阿魏酰斯皮诺素、迷迭香酸、五味子醇甲、五味子乙素和丹酚酸B 6个成分的双标多测法,验证该方法在枣仁安神颗粒质量评价中应用的准确性和可行性.方法 采用HPLC法,以乙腈为流动相A,0.2%冰醋酸溶液为流动相B,梯度洗脱,流速为1.0 mL·min-1,切换波长320 nm(斯皮诺素、6'''-阿魏酰斯皮诺素、迷迭香酸、丹酚酸B)、250 nm(五味子醇甲、五味子乙素),柱温28 ℃.采用5根不同的C18色谱柱,测定枣仁安神颗粒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,选取斯皮诺素(峰1)、五味子乙素(峰6)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.以五味子乙素为参照物,计算其余各成分的相对校正因子,对各成分进行定量.结果 双标线性校正法能够准确地预测待测组分在未知色谱柱上的保留时间;斯皮诺素、6'''-阿魏酰斯皮诺素、迷迭香酸、五味子醇甲和丹酚酸B相对于五味子乙素的相对校正因子分别为0.7342、0.6063、0.5664、0.9975及0.7773,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枣仁安神颗粒中6个成分可行且准确.
Application of Two Reference Substances for Determination of Multiple Components Method for the Determination of Six Components in ZaoRen AnShen Granules
OBJECTIVE To establish a two reference substances for determination of multiple components method(TRSDMC)for the determination of six components(spinosin,6'''-feruloylspinosin,rosmarinic acid,schisan-drin,γ-schisandrin and salvianolic acid B)of ZaoRen AnShen granules,and to verify the accuracy and feasibility of the method in the quality evaluation of ZaoRen AnShen granules.METHODS HPLC method was used with aceto-nitrile as mobile phase A and 0.2%glacial acetic acid as mobile phase B in gradient elution mode,and the flow rate was 1.0 mL·min-1,the determination wavelengths were 320 nm for spinosin,6'''-feruloylspinosin,rosmarinic acid,salvianolic acid B,250 nm for schisandrin and γ-schisandrin;the column temperature was 28 ℃.The actual retention time of six components in ZaoRen AnShen granules was determined on five different types of C18 chromatographic col-umns.The average retention time of each component in each column was calculated to obtain the standard retention time of each component.Spinosin(peak 1)and γ-schisandrin(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 in the same method.The methodology was validated.Taking γ-schisandrin as reference,the content of each compo-nent was determinated.At the same time,the contents of cinnamaldehyde,schizandrin and schisandrin A in ZaoRen AnShen granules were determined by external standard method,and the contents obtained by TRSDMC and external standard method were compared to verify the scientificity and feasibility of TRSDMC.RESULTS The linear calibra-tion using two reference substances can accurately predict the retention time of the tested components on the unknown column.The relative correction factors of spinosin,6'''-feruloylspinosin,rosmarinic acid,schisandrin and salvianolic acid B were 0.7342,0.6063,0.5664,0.9975 and 0.7773,respectively,with RSD values less than 1%.There was no significant difference between the contents obtained by TRSDMC and external standard method for each compo-nent.CONCLUSION TRSDMC for simultaneous determination of 5 components in ZaoRen AnShen granules is fea-sible and accurate.

ZaoRen AnShen granulesTwo reference substances for determination of multiple components method(TRSDM)Ela-tive correction factor quantificationSpinosinγ-schisandrin6'''-feruloylspinosinSalvianolic acid BSchisandrinRosmarinic acid

陈颖、刘智勇、郑时桢

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福建中医药大学附属人民医院,福建 福州 350000

枣仁安神颗粒 双标多测法 相对校正因子定量 斯皮诺素 五味子乙素 6'''-阿魏酰斯皮诺素 丹酚酸B 五味子醇甲 迷迭香酸

2024

海峡药学
中国药学会福建分会

海峡药学

影响因子:0.643
ISSN:1006-3765
年,卷(期):2024.36(8)