解吸附电晕束电离质谱法快速筛选保健食品中非法添加的5型磷酸二酯酶抑制剂

建立了解吸附电晕束离子源(DCBI)结合离子阱质谱快速检测保健食品中非法添加的3种磷酸二酯酶5(PDE5)抑制剂(伐地那非、西地那非、他达拉非)的方法。采用一级质谱筛选,二级质谱确证,对样品中非法添加物进行定性鉴别;通过二级特征碎片离子进行半定量分析,并与传统高效液相色谱-紫外(HPLC-UV)定量检测法对比。对12个市售保健品进行检测,DCBI-MS定性检测结果与HPLC-UV检测结果一致,有7个样品检出他达拉非,3个样品检出西地那非,1个样品检出伐地那非。通过研究3种PDE5抑制剂的二级质谱裂解规律,推测一个样品中含有羟基豪莫西地那非。本方法快速准确,适用于大批量复杂基质样品中PDE5抑制剂的筛查。

Rapid Determination of Illegally Added Phonphodiesterase 5 Inhibitors in Health Food by Desorption Corona Beam Ionization-Tandem Mass Spectrometry

A rapid method using desorption corona beam ionization-ion trap mass spectrometry(DCBI-MS) was developed for the determination of three phosphodiesterase 5(PDE5) inhibitors,i.e.,vardenafil,sildenafil,tadalafil in health food.The MS spectra and MS2 spectra of the inhibitors were used for prescreening and confirmation respectively.The characteristic ions of the PDE5 inhibitors were chosen for semi-quantitative.Precise quantification of the PDE5 inhibitors was carried out by high performance liquid chromatography-ultraviolet(HPLC-UV).Vardenafil,sildenafil and tadalafil were detected in one sample,three samples,and seven samples,respectively.These results were in accordance with those obtained by HPLC-UV.The fragmentation pathways of the PDE5 inhibitors were studied and based on it one sample was figured out to contain hydroxyhomosidenafil.The DCBI-MS method is rapid and accurate,which had more advantages to screen the illegally added PDE5 inhibitors in samples with complex matrix and the semiquantitative results could provide basis for HPLC analysis.