高效液相色谱-高分辨质谱快速筛查和确证保健品中非法添加的壮阳药物  

Rapid screening and confirmation of illegally added antiimpotence preparations in health care products by high performance liquid chromatography-high resolution mass spectrometry

作　　者：胡婷婷[1,2] 曲晓宇[3] 康明芹[1] 宋清莲[1] 杨璐[1] 赵韫慧[1] 张代辉[1] 

机构地区：[1]吉林出入境检验检疫局,吉林长春130062 [2]吉林大学公共卫生学院,吉林长春130021 [3]吉林大学第一医院,吉林长春130021

出　　处：《色谱》2015年第8期897-901,共5页Chinese Journal of Chromatography

基　　金：国家科技支撑计划项目(2012BAK08B01)

摘　　要：采用高效液相色谱-四极杆/飞行时间质谱对中药保健品中红地那非、伐地那非、那红地那非、他达拉非、西地那非、豪莫西地那非、硫代艾地那非、伪伐地那非、羟基豪莫西地那非、育亨宾、达泊西汀等11种非法添加的壮阳类药物进行了快速筛查、确证和定性定量检测。样品经甲醇提取后,采用正离子扫描模式进行检测。结果表明,11种待测物的定量限除那红地那非为25.0 ng/m L外,其他10种壮阳类药物均为5.0 ng/m L,在5.0～200.0 ng/m L（那红地那非在25.0～500.0 ng/m L）范围内,线性相关性较好,相关系数均不小于0.999 0。平均添加回收率为82.0%～105.9%,相对标准偏差为4.7%～16.5%。本方法利用准确质量数匹配和自建标准谱库,通过多级特征碎片离子的比对,实现快速筛查和确证,简单快速,结果可靠。A method was established for rapid screening and quantifying 11 illegally added anti- impotence preparations （yohimbine, acetildenafil, nor-acetildenafil, homosildenafil, hydroxy- homosildenafil, sildenafil, vardenafil, thioaildenafil, tadalafil, pseudovardenafil, dapoxetine） in health care products by high performance liquid chromatography-high resolution mass spec- trometry. The samples were extracted with methanol and analyzed by positive mode in the MS detection. The results showed that the limits of detection were 25.0 ng/mLexcept for nor-acetil- denafil （5.0 ng/mL）, the linear ranges were 5.0-200.0 ng/mL except for nor-acetildenafil （25.0-500.0 ng/mL） with the correlation coefficients not less than 0. 999 0. The recoveries were in the range of 82.0% -105.9% with the relative standard deviations of 4.7% -16. 5%. This method is accurate, simple and rapid, and can be used in rapid screening and quantitative anal- ysis of the ! ! illegally added anti-impotence in health care products.

关 键 词：高效液相色谱-高分辨质谱 壮阳药物 保健品 快速筛查 

分 类 号：O658[理学—分析化学]