摘要
以LC-MS为分析手段,建立了中药复方制剂维C银翘片中有效组分对乙酰氨基酚和马来酸氯苯那敏的定性和定量检测方法。在样品分离阶段,采用等梯度洗脱方式在Hypsil-ODS色谱柱(4.6 mm×250 mm,5.0μm,Agilent)上进行分离;在定性和定量方法上,确定了每个分析物的保留时间和一级质谱特征离子为定性参数,以紫外色谱峰面积为定量参数。结果表明:该方法对于2种有效组分对乙酰氨基酚和马来酸氯苯那敏的线性相关系数(r)分别为0.99990和0.99998,平均加标回收率分别为99.6%和98.0%,相对标准偏差(RSD)分别为0.36%和0.72%,最低检测限(LOD)分别为0.02μg.mL-1和0.05μg.mL-1。同时,该方法对维C银翘片中另外两种有效组分绿原酸和连翘苷也可以进行定性鉴定。
Two pharmaceutical systems were studied by means of LC-MS.An qualitative and quantitative analytical method was developed for the determination of effective constituents in Chinese traditional medicine compound preperation Vitamin C Yinqiao Tablet.In the LC separation step,Hypsil-ODS chromatographic column(4.6 mm×250 mm,5.0 μm,Agilent) was used for the separation of sample by constant gradent mode,for the qualitative and the quantitative method,the retention time and characteristic ions of every analyte were choosed to be qualitative parameters,the peak area of UV chromatogram was confirmed to be the quantitative parameter.The research results showed that the linear correlation coefficients(r) of the proposed method for two effective constituents,4-acetamino phenol and chlorpheniramine maleate were 0.99990 and 0.99998,respectively,the mean recoveries were 99.6% and 98.0% with relative standard deviations(RSD) 0.36% and 0.72%,the limits of detection(LOD) were 0.02 μg·mL-1 and 0.05 μg·mL-1,and other two effective constituents,chlorogenic acid and forsythin were identified by the analytical method.
出处
《广州化工》
CAS
2012年第15期142-144,147,共4页
GuangZhou Chemical Industry
基金
广东石油化工学院自然科学基金(510009)
关键词
LC-MS法
维C银翘片
药物分析
LC-MS
Vitamin C Yinqiao Tablet
pharmaceutical analysis