一测多评法同时测定芒果止咳片中6种药效成分的含量  

Simultaneous Determination of 6 Medicinal Components in Mango Zhike Tablets by Quantitative Analysis of Multi-components by Single Marker Method

作　　者：梁梓敏 覃洁萍 郭海姣 罗宇东 胡华 LIANG Zimin;QIN Jieping;GUO Haijiao;LUO Yudong;HU Hua(College of Pharmacy,Guangxi University of TCM,Nanning 530001,China;Pharmaceutical Factory,Guangxi University of TCM,Nanning 530023,China)

机构地区：[1]广西中医药大学药学院,南宁530001 [2]广西中医药大学制药厂,南宁530023

出　　处：《中国药房》2020年第8期963-968,共6页China Pharmacy

基　　金：广西创新驱动发展专项资金项目(No.桂科AA172040-73);广西教育厅高校中药提取纯化与质量分析重点实验室项目(No.桂教科研〔2014〕6号);广西中医药大学2019年研究生教育创新计划项目(No.YCSY2019030)。

摘　　要：目的:建立同时测定芒果止咳片中没食子酸、原儿茶酸、芒果苷、高芒果苷、金丝桃苷和异槲皮苷含量的方法。方法:采用高效液相色谱法。色谱柱为Phenomenex Gemini C18,流动相为0.1%磷酸水溶液-乙腈(梯度洗脱),流速为1.0 mL/min,检测波长为258 nm,柱温为30℃,进样量为5μL。以没食子酸为内参物,计算原儿茶酸、芒果苷、高芒果苷、金丝桃苷和异槲皮苷的相对校正因子,并将一测多评法与外标法测定结果进行比较。结果:没食子酸、原儿茶酸、芒果苷、高芒果苷、金丝桃苷和异槲皮苷检测质量浓度的线性范围分别为45.75~1 830μg/m L(r=0.999 9)、2.525~101.0μg/mL(r=0.999 9)、65.33~2 613μg/m L(r=0.999 6)、9.058~362.3μg/mL(r=0.999 9)、3.885~155.4μg/mL(r=0.999 9)、1.870~74.8μg/mL(r=0.999 9);定量限分别为0.571、0.643、1.053、0.854、0.830、1.500μg/mL,检测限分别为0.171、0.193、0.316、0.256、0.249、0.450μg/mL;精密度、稳定性、重复性试验RSD均小于3%;加样回收率分别为98.8%~101.9%(RSD=1.3%,n=6)、94.3%~101.5%(RSD=3.3%,n=6)、97.9%~100.5%(RSD=0.9%,n=6)、98.2%~101.6%(RSD=1.2%,n=6)、102.3%~106.1%%(RSD=1.3%,n=6)、96.6%~99.3%(RSD=1.0%,n=6)。以没食子酸为内参物,原儿茶酸、芒果苷、高芒果苷、金丝桃苷、异槲皮苷的相对校正因子分别为0.568 3、0.500 3、0.687 6、0.939 1、0.826 3;一测多评法测得原儿茶酸等5种成分的含量范围分别为0.197~0.440、3.263~11.250、0.201~1.196、0.168~0.381、0.115~0.293 mg/片,外标法测得的含量范围分别为0.198~0.441、3.329~11.570、0.206~1.194、0.171~0.380、0.119~0.298 mg/片,两种方法测量结果的相对误差为-3.80%~0.74%,且差异无统计学意义(P>0.05)。结论:所建一测多评含量测定方法准确、可靠、重复性好,可用于同时测定芒果止咳片中6种药效成分的含量。OBJECTIVE:To establish a method for simultaneous determination of gallic acid,protocatechuic acid,mangiferin,homomangiferin,hyperoside and isoquercetin in Mangguo zhike tablets. METHODS:HPLC was adopted. The determination was performed on Phenomenex Gemini C18 column with mobile phase consisted of 0.1% phosphoric acid water solution-acetonitrile(gradient elution)at the flow rate of 1.0 m L/min. The detection wavelength was set at 258 nm. The column temperature was set at30 ℃,and sample size was 5 μ L. Gallic acid was used as the internal substance,and the correction factors of gallic acid,protocatechuic acid,mangiferin,homomangiferin,hyperoside and isoquercetin were calculated;the results of quantitative analysis of multi-components by single marker method(QAMS) were compared with those of external standard method(ESM).RESULTS:The linear range of gallic acid,protocatechuic acid,mangiferin,homomangiferin,hyperoside and isoquercetin were45.75-183 0 μg/mL(r=0.999 9),2.525-101.0 μg/mL(r=0.999 9),65.33-261 3 μg/mL(r=0.999 6),9.058-362.3 μg/mL(r=0.999 9),3.885-155.4 μg/mL(r=0.999 9),1.870-74.8 μg/mL(r=0.999 9),respectively. The limits of quantification were 0.571,0.643,1.053,0.854,0.830,1.500 μg/m L,respectively. The limits of detection were 0.171,0.193,0.316,0.256,0.249,0.450 μg/m L,respectively. RSDs of precision, stability and reproducibility tests were all lower than 3%. The average recoveries were98.8%-101.9%(RSD=1.3%,n=6),94.3%-101.5%(RSD=3.3%,n=6),97.9%-100.5%(RSD=0.9%,n=6),98.2%-101.6%(RSD=1.2%,n=6),102.3%-106.1%(RSD=1.3%,n=6),96.6%-99.3%(RSD=1.0%,n=6),respectively. RCFs of protocate-chuic acid, mangiferin, homomangiferin,hyperoside and isoquercetin were 0.568 3,0.500 3,0.687 6,0.939 1 and 0.826 3,using gallic acid as internal substance.The content ranges of protocatechuic acid and other 4 components measured by QAMS were 0.197-0.440,3.262-11.250,0.201-1.196,0.168-0.381,0.115-0.293 mg/tablet,respectively.The content ranges measured by ESM were 0.198-0.441, 3.239-11.570, 0.206-1.194, 0.171-0.380, 0.11

关 键 词：芒果止咳片 高效液相色谱法 一测多评法 没食子酸 原儿茶酸 芒果苷 高芒果苷 金丝桃苷 异槲皮苷 含量测定 

分 类 号：R286[医药卫生—中药学]