一测多评法同时测定玳玳果黄酮滴丸中4个活性成分的含量  

Determination of four active components in Daidaiguo Huangtong dropping pills by QAMS

作　　者：连赟芳[1] 陈丹[1] 蔡韦炜[1] 曾华平[1] 林伊莉 廖淑彬 

机构地区：[1]福建中医药大学药学院,福州350122

出　　处：《药物分析杂志》2015年第6期974-978,共5页Chinese Journal of Pharmaceutical Analysis

基　　金：福建省发展和改革委员会产业技术开发项目(闽发改高技[2011]1598号;福建省自然科学基金(2012J01386);福建省科技计划项目(2010Y2004)

摘　　要：目的：建立一测多评法同时测定玳玳果黄酮滴丸中活性成分柚皮苷、新橙皮苷、橙皮内酯水合物及枳属苷的含量。方法：采用高效液相色谱法,使用250-4 lichrocart C18（250 mm×4.6 mm,5μm）色谱柱,流动相为乙腈（A）-0.2%醋酸水溶液（B）,线性梯度洗脱（0-10 min,22%A;10-20 min,22%A→35%A;20-25 min,35%A→48%A;25-30 min,48%A→22%A）,流速1.0 m L·min-1,检测波长284 nm,柱温25℃,进样量20μL。柚皮苷、新橙皮苷、橙皮内酯水合物及枳属苷的色谱峰分离度R〉1.5,理论塔板数按柚皮苷计〉3 000。建立测定代表性成分柚皮苷含量并以其为内参物,通过柚皮苷与新橙皮苷、橙皮内酯水合物和枳属苷的相对校正因子计算新橙皮苷、橙皮内酯水合物和枳属苷含量的一测多评法,实现多指标成分的同步测定;同时与外标法分别测定玳玳果黄酮滴丸上述4个成分含量的结果比较。结果：柚皮苷质量浓度在119.40-477.60μg·m L-1、新橙皮苷质量浓度在122.20-488.80μg·m L-1、橙皮内酯水合物质量浓度在7.62-22.86μg·m L-1、枳属苷质量浓度在3.00-21.00μg·m L-1范围内线性关系良好;柚皮苷、新橙皮苷、橙皮内酯水合物、枳属苷平均加样回收率（n=3）分别为98.67%（RSD=1.5%）、98.20%（RSD=0.50%）、101.9%（RSD=1.7%）、100.9%（RSD=0.35%）;柚皮苷与新橙皮苷、橙皮内酯水合物、枳属苷的相对校正因子分别为1.153、0.434、0.893,RSD（n=6）分别为2.7%、3.1%、1.2%;外标法与一测多评法含量测定结果无显著性差异。结论：以柚皮苷为内参物,利用相对校正因子一测多评法同时测定玳玳果黄酮滴丸活性成分柚皮苷、新橙皮苷、橙皮内酯水合物与枳属苷含量的结果准确,为以中药有效部位为原料制备的中药制剂实现多指标成分群质量控制评价提供了可借鉴的方法。Objective：To establish a method for simultaneous determination of active components including naringin,neohesperidin,meranzin hydrate and poncirin in Daidaiguo Huangtong dropping pills by quantitative analysis of multi-components by single-marker（QAMS）.Methods：Using the method of HPLC,the 250-4 lichrocart C18column（250 mm × 4.6 mm,5 μm） was used.The mobile phase was composed of acetonitrile（A）-0.2% acetic acid（B） with linear gradient elution（0-10 min,22% A;10-20 min,22% A→35% A;20-25 min,35% A→48% A;25-30 min,48% A→22% A） at the flow rate of 1.0 m L·min-1.The detection wavelength was 284 nm,the column temperature was 25 ℃ and the sample size was 20 μL.The chromatographic resolution of naringin,neohesperidin,meranzin hydrate and poncirin was greater than 1.5,and the theoretical plate number of naringin was greater than3 000.The naringin was used as an internal standard to establish the relative correction factors of neohesperidin,meranzin hydrate and poncirin with reference to naringin so as to achieve simultaneous determination of multi-indexed components.Meanwhile,the external standard method for determination was used to compare with the results of QAMS method.Results：There were good linearities in the range of 119.40-477.60 μg·m L-1for naringin,122.20-488.80 μg·m L-1for neohesperidin,7.62-22.86 μg·m L-1for meranzin hydrate and 3.00-21.00 μg·m L-1for poncirin.The average recoveries（n = 3） were 98.67%（RSD = 1.5%） for naringin,98.20%（RSD = 0.50%） for neohesperidin,101.9%（RSD = 1.7%） for meranzin hydrate and 100.9%（RSD = 0.35%） for poncirin,respectively.The relative correction factors of neohesperidin,meranzin hydrate and poncirin with reference to naringin were1.153,0.434 and 0.893 with RSDs of 2.7%,3.1%,1.2%（n = 6）,respectively in Daidaiguo Huangtong dropping pills.The quantitative results of the external standard method and the QAMS method had no significant difference.Conclusion：Naringin was used as the internal standard for the relative c

关 键 词：一测多评法 玳玳果黄酮滴丸 相对校正因子 柚皮苷 新橙皮苷 橙皮内酯水合物 枳属苷 多成分同步监控 

分 类 号：R917[医药卫生—药物分析学]