摘要
目的:建立同时测定复方罗布麻片Ⅰ中8个活性成分含量的一测多评法(QAMS)。方法:采用HPLC法,以氢氯噻嗪为内参物,分别计算其与金丝桃苷、粉防己碱、防己诺林碱、绿原酸、蒙花苷、盐酸异丙嗪、硫酸双肼屈嗪的相对校正因子,通过相对校正因子计算复方罗布麻片Ⅰ中7个活性成分的含量(计算值),同时采用外标法测定8个活性成分的含量(实测值),比较计算值与实测值的差异。色谱柱为Kromasil C18(250 mm×4.6 mm,5μm),流动相为乙腈-0.5%磷酸溶液(梯度洗脱),流速0.7 mL·min^-1,检测波长260 nm(氢氯噻嗪、盐酸异丙嗪、硫酸双肼屈嗪、金丝桃苷)、280 nm(粉防己碱、防己诺林碱)、325 nm(绿原酸、蒙花苷),柱温30℃,进样量10μL。结果:金丝桃苷、粉防己碱、防己诺林碱、绿原酸、蒙花苷、氢氯噻嗪、盐酸异丙嗪、硫酸双肼屈嗪检测质量浓度的线性范围分别为1.082~19.48、3.016~54.29、1.350~24.30、1.102~19.84、1.623~29.21、19.49~350.8、11.04~198.7、13.03~234.5μg·m L^-1(r为0.999 5~0.999 8);平均加样回收率分别为98.3%、99.1%、98.3%、97.5%、97.9%、96.5%、96.3%、97.8%(RSD<2.0%,n=9);检测下限分别为3.05、2.96、4.25、3.21、2.62、2.95、3.26、4.08 ng,定量下限分别为9.18、8.94、12.95、9.71、7.95、8.81、9.86、12.24 ng;精密度、重复性、稳定性(48 h)试验的RSD<2.0%(n=6)。金丝桃苷、粉防己碱、防己诺林碱、绿原酸、蒙花苷、盐酸异丙嗪、硫酸双肼屈嗪的相对校正因子分别为0.662、1.253、1.548、1.190、0.979、1.236、1.654,其计算值和实测值之间无显著性差异。结论:该方法简单、有效,结果准确,节约成本,可用于复方罗布麻片Ⅰ中上述8个活性成分的同时测定。
Objective:To establish the quantitative analysis of multi-components by single marker(QAMS)for simultaneous determination of 8 active constituents in Kendir leaves tabletsⅠ. Methods:Using hydrochlorothiazide as internal standard,HPLC method was used to calculate relative correction factor(RCF)of hyperoside,tetrandrine,fangchinoline,chlorogenicacid,buddleodide,promethazine,dihydralazine sulfate. The contents of above-mentioned 7 active components in Kendir leaves tablets Ⅰ were calculated by using RCF(calculation value). The external standard method(ESM)was used to determine the contents of 8 constituents(measured value). The differences between calculation value and measured value were compared. The determination was performed on Kromasil C18(250 mm×4.6 mm,5 μm) column with mobile phase consisted of acetonitrile-0.5%phosphoric acid(gradient elution)at the flow rate of 0.7 mL·min^-1. The detection wavelength was set at 260 nm for hyperoside,hydrochlorothiazide;promethazine;dihydralazine sulfate,280 nm for tetrandrine,fangchinoline,325 nm for chlorogenic acid,buddleodide.The column temperature was set at 30 ℃ and the injection volume was 10μL. Results:The linear range was 1.082-19.48 μg·mL^-1 for hyperoside,3.016-54.29 μg·mL^-1 for tetrandrine,1.350-24.30 μg·mL^-1 for fangchinoline,1.102-19.84 μg·mL^-1 chlorogenicacid,1.623-29.21 μg·mL^-1 forbuddleodide,19.49-350.8 μg·mL^-1 for hydrochlorothiazide,11.04-198.7 μg·mL^-1 forpromethazine,13.03-234.5 μg·mL^-1 for dihydralazine sulfate(r=0.999 5-0.999 8),respectively. Average recoveries were 98.3%,99.1%,98.3%,97.5%,97.9%,96.5%,96.3%,97.8%(RSD<2.0%,n=9). Limits of detection were 3.05,2.96,4.25,3.21,2.62,2.95,3.26,4.08 ng;limits of quantitation were 9.18,8.94,12.95,9.71,7.95,8.81,9.86,12.24 ng. RSDs of precision,reproducibility and stability tests(48 h)were lower than 2.0%(n=6). RCFs of hyperoside,tetrandrine,fangchinoline,chlorogenicacid,buddleodide,promethazine,dihydralazinesulfate were 0.662,1.253,1.548,1.190,0.979,1.236,1.654. There was no sta
作者
杨晶
夏新华
张雁
YANG Jing;XIA Xin-hua;ZHANG Yan(Hunan University of Chinese Medicine,Pharmaceutical Teaching and Research Department of Pharmacy College,Changsha 410208,China;Xiangtan Institute for Food and Drug Control,Xiangtan 411100,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2019年第8期1433-1442,共10页
Chinese Journal of Pharmaceutical Analysis
基金
湖南中医药大学一流学科项目(201803)
国家自然科学基金面上项目(81573621)
关键词
高效液相色谱-一测多评法
复方罗布麻片Ⅰ
金丝桃苷
粉防己碱
防己诺林碱
绿原酸
蒙花苷
氢氯噻嗪
盐酸异丙嗪
硫酸双肼屈嗪
high performance liquid chromatography-quantitative analysis of multi-components by single-marker(HPLC-QAMS)
Kendir leaves tablets Ⅰ
hyperoside
tetrandrine
fangchinoline
chlorogenic acid
buddleodide
hydrochlorothiazide
promethazine
dihydralazine sulfate
