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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。

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 11 illegally added anti-impotence in health care products.

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