中国药业2017，Vol.26Issue(4)：22-26,5.DOI:10.3969/j.issn.1006-4931.2017.04.006
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
舒展 1王琤帅1
作者信息
- 1. 浙江省金华市食品药品检验检测研究院,浙江金华 321000
- 折叠
摘要
Abstract
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 × 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-Desmethyltadalafil illegally added in dietary supplements.关键词
液相色谱-四级杆飞行时间质谱/非法添加/N-去甲基他达拉非Key words
HPLC-QTOF/illegal additives/N-desmethyltadalafil分类
医药卫生引用本文复制引用
舒展,王琤帅..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[J].中国药业,2017,26(4):22-26,5.
