摘要
目的建立同时测定新复方大青叶片中维生素C、对乙酰氨基酚、咖啡因和异戊巴比妥含量的一测多评(QAMS)法。方法色谱柱为Welch Ultimate LP-C18柱(250 mm×4.6 mm,5μm),流动相为乙醇-0.01 mol/L磷酸二氢钾溶液(pH 3.0)、梯度洗脱,流速为0.8 mL/min,检测波长为215 nm(对乙酰氨基酚、咖啡因和异戊巴比妥)和245 nm(维生素C),柱温为40℃,进样量为10μL。以对乙酰氨基酚为参照物,测定维生素C、咖啡因和异戊巴比妥的相对校正因子,以计算维生素C、咖啡因和异戊巴比妥的含量。比较采用外标法与QAMS法时结果的差异。结果维生素C、对乙酰氨基酚、咖啡因和异戊巴比妥进样量分别在0.0643~0.6432μg(r=0.9998)、0.3737~3.7375μg(r=0.9997)、0.0373~0.3732μg(r=0.9999)、0.0379~0.3789μg(r=0.9999)范围内与峰面积线性关系良好;检测限分别为0.03,0.15,0.07,0.24μg/mL,定量限分别为0.09,0.51,0.23,0.79μg/mL;精密度、稳定性、重复性试验结果的RSD均小于2.0%;平均加样回收率分别为101.07%,101.83%,98.04%,98.80%,RSD分别为1.20%,1.73%,1.13%,1.58%(n=6);维生素C、咖啡因和异戊巴比妥的相对校正因子分别为0.5761,0.3732和0.8438,QAMS法与外标法测定结果无显著差异(P>0.05)。结论所建立的方法环保(以乙醇代替甲醇)、经济(只需1种对照品),结果准确且可快速获得,适用于新复方大青叶片的质量评价。
Objective To establish a quantitative analysis of multi-components by single-marker(QAMS)method for the simultaneous determination of vitamin C,paracetamol,caffeine and amobarbital in New Compound Isatidis Folium Tablets.Methods The chromatographic column was Welch Ultimate LP-C18 column(250 mm×4.6 mm,5μm),the mobile phase was ethanol-0.01 mol/L potassium dihydrogen phosphate solution(pH 3.0),with gradient elution,the flow rate was 0.8 mL/min,the detection wavelengths were 215 nm(paracetamol,caffeine and amobarbital)and 245 nm(vitamin C),the column temperature was 40℃,and the injection volume was 10μL.With paracetamol as the reference,the relative correction factors of vitamin C,caffeine and amobarbital were determined to calculate their contents.The differences of content determination by external standard method(ESM)and QAMS were compared.Results The linear ranges of vitamin C,paracetamol,caffeine and amobarbital were 0.0643-0.6432μg(r=0.9998),0.3737-3.7375μg(r=0.9997),0.0373-0.3732μg(r=0.9999)and 0.0379-0.3789μg(r=0.9999)respectively.The limits of detection(LOD)of the above four components were 0.03,0.15,0.07 and 0.24μg/mL respectively,the limits of quantitation(LOD)of the above four components were 0.09,0.51,0.23 and 0.79μg/mL respectively.The RSDs of precision,stability and repeatability tests were all lower than 2.0%.The average recovery rates of the above four components were 101.07%,101.83%,98.04%and 98.80%respectively,with RSDs of 1.20%,1.73%,1.13%and 1.58%(n=6)respectively.The relative correction factors of vitamin C,caffeine and amobarbital were 0.5761,0.3732 and 0.8438 respectively.The results of content determination by QAMS were similar to those by ESM(P>0.05).Conclusion The established method is environmental(replacing methanol with ethanol),economical(with only one reference),accurate and rapid,which is suitable for the quality evaluation of New Compound Isatidis Folium Tablets.
作者
王丽琼
魏长勇
余敏灵
WANG Liqiong;WEI Changyong;YU Minling(Leshan Food and Drug Inspection Center·SCMPA Key Laboratory of Quality Research of Traditional Chinese Medicine,Leshan,Sichuan,China 614000)
出处
《中国药业》
CAS
2023年第10期80-84,共5页
China Pharmaceuticals
基金
四川省药品监督管理局科技计划项目[2021012]。
