万萍,卢岳华,陈波.纸喷雾离子化质谱法快速筛查保健食品中违禁添加的磷酸二酯酶5抑制剂[J].中国食品卫生杂志,2017,29(4):459-463. 本文二维码信息
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纸喷雾离子化质谱法快速筛查保健食品中违禁添加的磷酸二酯酶5抑制剂
Rapid determination of phosphodiesterase 5 inhibitors in invigorative health food by paper spray ionization mass spectrometry method
投稿时间:2017-06-07  
DOI:
中文关键词:  纸喷雾离子化质谱  快速筛查  抗疲劳  保健食品  磷酸二酯酶5抑制剂  西地那非  伐地那非  他达拉非  违法添加物
Key Words:Paper spray ionization mass spectrometry  rapid detection  invigorative  health food  phosphodiesterase 5 inhibitors  sildenafil  vardenafil  tadalafil  adulterant
基金项目:
作者单位E-mail
万萍 湖南师范大学 植化单体开发与利用湖南省重点实验室,湖南 长沙 410081 wanping0903@sina.com,lyh@hunnu.cn 
卢岳华 湖南师范大学 植化单体开发与利用湖南省重点实验室,湖南 长沙 410081 wanping0903@sina.com,lyh@hunnu.cn 
陈波 湖南师范大学 植化单体开发与利用湖南省重点实验室,湖南 长沙 410081  
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中文摘要:
      目的 建立纸喷雾离子化质谱(PSI-MS)法快速检测保健食品中3种非法添加的磷酸二酯酶5(PDE5)抑制剂(西地那非、伐地那非和他达拉非)的方法。方法 利用PSI-MS法对样品中非法添加物进行初步定性鉴别,并通过内标法进行半定量分析。结果 24种包括胶囊、片剂、丸剂、粉末、酒剂、糖浆及口服液等剂型在内的待测市售保健品的PSI-MS检测结果与HPLC-UV检测结果基本一致。各目标物在一定范围内线性关系良好,相关系数r2均>0.99,检出限均在1.0 mg/L以下,相对标准偏差为20%~24%。结论 本方法快速、准确、专属性强,适用于大批量复杂基质样品中PDE5抑制剂的快速筛查。
Abstract:
      Objective A rapid method was constructed for detection of 3 kinds of phosphodiesterase 5 (PDE5) inhibitors (sidenafil, vardalafil, tadalafil) in invigorative health food by paper spray ionization mass spectrometry (PSI-MS method). Methods The characteristic ions of the PDE5 inhibitors could be used for preliminary identification and semiquantitative analysis with internal standard method using PSI-MS method. Results The 24 kinds of commercially available health-care products includes capsule, tablet, pill, powder, wine, syrup and liquid were tested. Results from PSI-MS were consistent with the HPLC-UV date. The calibration curves of PSI-MS has a good linearity in a given range. The linear coefficients of analytes were higher than 0.99. The LODs of 3 kinds of PDE5 inhibitors were lower than 1.0 mg/L. The RSDs of this method ranged from 20% to 24%. Conclusion The PSI-MS method was rapid, accurate and targeted, which is compliant for quickly screening the PDE5 inhibitors in large complex matrix samples.
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