同时测定制剂中添加3种卡波地那非类似物的研究

Simultaneous Determination of Three Carbodenafil Analogues Adulterated in Herbal Wine and Tablets

目的建立制剂中添加3种卡波地那非类似物的分析方法。方法以乙腈为提取溶剂,样品经Agilent Eclipse Plus C_(18)(4.6 mm×250 mm,5μm)色谱柱分离,高效液相色谱仪-二级管阵列(DAD)检测器定性、定量检测3种制剂中的3种卡波地那非类似物(去甲基卡波地那非、二硫去甲基卡波地那非、二甲基哌嗪二硫去甲基卡波地那非)。用Dikma Spursil C_(18)(2.1 mm×150 mm,3μm)色谱柱分离,高效液相色谱-质谱联用仪以一级及二级质谱定性确证3种卡波地那非类似物。结果3种卡波地那非类似物检测的线性相关系数r≥0.9958;方法精密度相对标准偏差(RSD)为2.2%~4.3%;3个添加水平的方法回收率为95.3%~102.8%;定量限为22~58 ng。结论本方法准确,操作简单、快捷,可作为3种制剂中卡波地那非类似物化学成分的定性、定量检测方法。

OBJECTIVE To develop a high performance liquid chromatography(HPLC)preliminary screening method and a high performance liquid chromatography coupled with mass spectrometry(HPLC-MS/MS)confirmatory determination method for three carbodenafil analogues(desmethylcarbodenafil,dithiodesmethylcarbodenafil and 3,5-dimethylpiperazinyldithiodesmethylcarbodenafil)adulterated in herbal wine and tablets.METHODS Acetonitrile was used as the extraction solvent,Agilent Eclipse Plus C_(18)(4.6 mm×250 mm,5μm)column was used for chromatographic separation,and DAD detector was used for quantitative determination of the three carbodenafil analogues adulterated in plant wine and tablets.HPLC-MS/MS was used for qualitative analysis,using Dikma Spursil C_(18)(2.1 mm×150 mm,3μm)column for chromatographic separation.RESULTS The linear correlation coefficients for the detection of three carbodenafil analogs were greater than 0.9958.The precision of the method was showed by RSDs(n=6)ranging from 2.2%to 4.3%.The method recovery rates of the three addition levels were 95.3%-102.8%.The limits of quantification were 22-58 ng.CONCLUSION The established methods are accurate,simple and quick to operate,and can be used as quantitative and qualitative detection methods for three carbodenafil analogues adulterated in herbal wine and tablets.