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

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。

Rapid determination of phosphodiesterase 5 inhibitors in invigorative health food by paper spray ionization mass spectrometry method

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.