液相色谱-高分辨率四级杆飞行时间质谱联用法测定保健食品中非法添加的N-去甲基他达拉非

Determination of N-Desmethyltadalafil Illegally Added in Dietary Supplements by HPLC-QTOF

目的基于高分辨率四级杆飞行时间质谱(QTOF),建立保健食品中N-去甲基他达拉非的检测方法。方法色谱柱为Agilent Poroshell EC-C_(18)柱(100 mm×4.6 mm,2.7μm),流动相为乙腈-0.1%醋酸,梯度洗脱,流速为0.3 mL/min,柱温为35℃;电喷雾电离(ESI),正离子模式,根据保留时间、精确相对分子质量和二级碎片比对定性。由提取离子流图峰面积与质量浓度关系定量分析N-去甲基他达拉非ESI质谱的裂解途径。结果 N-去甲基他达拉非进样质量浓度在53~1 060 ng/mL范围内与峰面积线性关系良好(r=0.999 6),检出限为10.6 ng/mL,定量限为35.0 ng/mL,平均回收率大于97.2%。结论该方法准确、可靠,适用于N-去甲基他达拉非的快速鉴别和定量测定。

Objective To establish the high-resolution quadrupole-time-of-flight mass spectrometry （QTOF） method for determining the N-Desmethyltadalfi illegally added in dietary supplements. Methods The analysis was performed on an Agilent Poroshell EC-C18 column（100 mm x 4. 6 mm,2. 7 μm）with 0. 1% acetic acid-acetonitrile as mobile phase,and the flow rate was 0. 3 mL/min,gradient elution,with the column temperature 35 ℃. QTOF MS equipped with ESI ion source was performed in positive ionization mode. Qualitative analysis was based on the retention time,accurate mass,and the product ions. Quantitative analysis was performed by using the peak area and concentration. Results The ESI-MS fragmentation behavior was characterized. Good linearity was obtained in the range of 53-1060 ng/mL（r=0. 9996）. The LOD was 10. 6 ng/mL and LOQ was 35. 0 ng/mL,the recoveries were more than 97. 2%. Conclusion The method is sensitive,accurate,and can be used in the qualitative and quantitative analysis of N-Desmethyltadalafil illegally added in dietary supplements.