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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r~2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。
Objective To establish a rapid method for the determination of three illicitly added phosphodiesterase 5 (PDE5) inhibitors (sildenafil, vardenafil and tadalafil) in health food by paper spray ionization mass spectrometry (PSI-MS) method. Methods The initial qualitative identification of illicit additives in samples by PSI-MS method was carried out and semi-quantitative analysis was performed by internal standard method. Results The results of PSI-MS of 24 commercially available health products, including capsules, tablets, pills, powders, wine, syrup and oral solution, were basically consistent with those of HPLC-UV. The linear correlation between each target in a certain range, the correlation coefficient r ~ 2 were> 0.99, the detection limits were below 1.0 mg / L, the relative standard deviation of 20% to 24%. Conclusion The method is rapid, accurate and specific. It is suitable for the rapid screening of PDE5 inhibitors in a large number of complex matrix samples.