色谱

色谱 ›› 2015, Vol. 33 ›› Issue (8): 897-901.DOI: 10.3724/SP.J.1123.2015.03020

• 技术与应用 • 上一篇    

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

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   

  1. 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
  • 收稿日期:2015-03-16 出版日期:2015-08-08 发布日期:2015-07-27
  • 通讯作者: 张代辉
  • 基金资助:

    国家科技支撑计划项目(2012BAK08B01).

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

HU Tingting1,2, QU Xiaoyu3, KANG Mingqin1, SONG Qinglian1, YANG Lu1, ZHAO Yunhui1, ZHANG Daihui1   

  1. 1. Jilin Entry-Exit Inspection and Quarantine Bureau, Changchun 130062, China;
    2. Public Health College of Jilin University, Changchun 130021, China;
    3. The First Hospital of Jilin University, Changchun 130021, China
  • Received:2015-03-16 Online:2015-08-08 Published:2015-07-27

PDF

170

被引次数

6

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/mL外,其他10种壮阳类药物均为5.0 ng/mL,在5.0~200.0 ng/mL(那红地那非在25.0~500.0 ng/mL)范围内,线性相关性较好,相关系数均不小于0.9990。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。

关键词: 保健品, 高效液相色谱-高分辨质谱, 快速筛查, 壮阳药物

Abstract:

A method was established for rapid screening and quantifying 11 illegally added anti-impotence preparations (yohimbine, acetildenafil, nor-acetildenafil, homosildenafil, hydroxyhomosildenafil, sildenafil, vardenafil, thioaildenafil, tadalafil, pseudovardenafil, dapoxetine) in health care products by high performance liquid chromatography-high resolution mass spectrometry. 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/mL except for nor-acetildenafil (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 0.9990. 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 analysis of the 11 illegally added anti-impotence in health care products.

Key words: anti-impotence preparations, health care products, high performance liquid chromatography-high resolution mass spectrometry (HPLC-HRMS), rapid screening

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