摘要
采用超高效液相色谱串联四级杆-飞行时间高分辨质谱(UHPLC/Q-TOF HRMS)法,从两种宣称具有缓解疲劳、增强免疫力的保健食品中发现了一种他达拉非衍生物。该化合物与2-羟丙基去甲他达拉非的质谱图特征非常相似,但保留时间却略有差异。采用制备液相色谱仪对该衍生物进行分离纯化,经质谱和氢核磁共振分析鉴定为3-羟丙基去甲他达拉非(3-hydroxypropylnortadalafil),为国内首次报道。
A tadalafil analogue was detected during routine screenings from two"fatigue reliever,immunity enhancer"dietary supplements by using UHPLC/Q-TOF HRMS.The MS2 spectrum of this compound was almost identical to that of 2-hydroxypropylnortadalafil.However,the retention time of this analogue was different from that of the 2-hydroxypropylnortadalafil isomers.The analogue was purified by using preparative HPLC and the structure was elucidated by mass spectrometric and NMR spectroscopic experiments.The spectral data suggested that the analogue bore a 3-hydroxypropyl group instead of the N-methyl group in tadalafil.The structure was further confirmed by comparison of the1 H NMR spectra data with those of the reference standard,and thus named as 3-hydroxypropylnortadalafil.The structure is first reported in China.
作者
冯亭亭
孙健
张静娴
于泓
冯睿
张甦
毛秀红
胡青
季申
FENG Ting-ting;SUN Jian;ZHANG Jing-xian;YU Hong;FENG Rui;ZHANG Su;MAO Xiu-hong;HU Qing;JI Shen(China State Institute of Pharmaceutical Industry,Shanghai 201203,China;Shanghai Institute for Food and Drug Control,NMPA Key Laboratory for Quality Control of Traditional Chinese Medicine,Shanghai 201203,China;Hebei North University,Zhangjiakou 075000,China)
出处
《药学学报》
CAS
CSCD
北大核心
2020年第8期1877-1881,共5页
Acta Pharmaceutica Sinica
基金
国家科技部重点研发计划(2017YFC1700800)
上海市科委研发平台专项(18DZ2292200)
上海市科委仪器专项(18142202300)
上海科委长三角合作项目(18395810300)。