同时测定制剂中添加3种卡波地那非类似物的研究

宋金玉, 董培智, 王珂, 刘晓普, 张禄, 项新华

中国药学杂志 ›› 2022, Vol. 57 ›› Issue (19) : 1673-1678.

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中国药学杂志
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中国药学杂志 ›› 2022, Vol. 57 ›› Issue (19) : 1673-1678. DOI: 10.11669/cpj.2022.19.012
论著

同时测定制剂中添加3种卡波地那非类似物的研究

  • 宋金玉1, 董培智2*, 王珂3, 刘晓普2, 张禄2, 项新华4*
作者信息 +

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

  • SONG Jin-yu1, DONG Pei-zhi2*, WANG Ke3, LIU Xiao-pu2, ZHANG Lu2, XIANG Xin-hua4*
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文章历史 +

摘要

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 C18(4.6 mm×250 mm,5 μm) 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 C18(2.1 mm×150 mm,3 μm)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≥0.995 8;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。

Abstract

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 C18(4.6 mm×250 mm, 5 μm) 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 C18(2.1 mm×150 mm, 3 μm) column for chromatographic separation. RESULTS The linear correlation coefficients for the detection of three carbodenafil analogs were greater than 0.995 8. 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.

关键词

卡波地那非类似物 / 非法添加 / 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

Key words

carbodenafil analogues / illegal addition / desmethylcarbodenafil / dithiodesmethylcarbodenafil / 3,5-dimethylpiperazinyldithiodesmethylcarbodenafil

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宋金玉, 董培智, 王珂, 刘晓普, 张禄, 项新华. 同时测定制剂中添加3种卡波地那非类似物的研究[J]. 中国药学杂志, 2022, 57(19): 1673-1678 https://doi.org/10.11669/cpj.2022.19.012
SONG Jin-yu, DONG Pei-zhi, WANG Ke, LIU Xiao-pu, ZHANG Lu, XIANG Xin-hua. Simultaneous Determination of Three Carbodenafil Analogues Adulterated in Herbal Wine and Tablets[J]. Chinese Pharmaceutical Journal, 2022, 57(19): 1673-1678 https://doi.org/10.11669/cpj.2022.19.012
中图分类号： R917   

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基金

山西省重点研发计划项目资助(201903D321011);山西省2020年度职业院校教师素质提高计划中高职教师素质协同提升项目资助(CXTD2020-11)
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