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[高效液相色谱-高分辨率质谱法快速筛查与确证保健品中非法添加的抗阳痿制剂]

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

作者信息

Hu Tingting, Qu Xiaoyu, Kang Mingqin, Song Qinglian, Yang Lu, Zhao Yunhui, Zhang Daihui

出版信息

Se Pu. 2015 Aug;33(8):897-901. doi: 10.3724/sp.j.1123.2015.03020.

DOI:10.3724/sp.j.1123.2015.03020
PMID:26749869
Abstract

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 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/mLexcept 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 0.999 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 analysis of the 11 illegally added anti-impotence in health care products.

摘要

建立了一种利用高效液相色谱-高分辨质谱法快速筛查和定量保健品中11种非法添加的抗阳痿制剂(育亨宾、乙酰西地那非、去甲乙酰西地那非、同型西地那非、羟基同型西地那非、西地那非、伐地那非、硫代艾地那非、他达拉非、伪伐地那非、达泊西汀)的方法。样品用甲醇提取,在质谱检测中采用正离子模式进行分析。结果表明,除去甲乙酰西地那非(检测限为5.0 ng/mL)外,其余10种的检测限均为25.0 ng/mL;除去甲乙酰西地那非(线性范围为25.0 - 500.0 ng/mL)外,其余10种的线性范围为5.0 - 200.0 ng/mL,相关系数均不小于0.999 0。回收率在82.0% - 105.9%之间,相对标准偏差为4.7% - 16.5%。该方法准确、简便、快速,可用于保健品中11种非法添加抗阳痿制剂的快速筛查和定量分析。

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