一种新型西地那非衍生物的Q-TOF-MS鉴定Identificationof-药学学报.PDF

药学学报 Acta Pharmaceutica Sinica 20 14, 49 (4): 513 516 ·513 · 种新型西地那非衍生物的 Q-TOF-MS 鉴定 * 健, 于 泓, 胡 青, 冯 睿, 张 甦, 季 申 (上海市食品 品检验所, 上海 20 1203) 摘要: 非法添加于中成药和保健食品中的西地那非类药物可严重危害健康, 新型衍生物层出不穷。基于高分 辨四级杆串联飞行时间质谱 (Q-TOF-MS) 方法, 在保健食品中检出一种新型西地那非衍生物。该化合物经制备 液相分离纯化, 核磁共振确证结构, 化学名为1-[4-丙氧基-3-[5-(6, 7-二氢- 1-甲基-7-氧代-3-丙基-1H-吡唑并[4, 3d] 嘧啶)]苯磺酰]-4- 甲基哌嗪, 即西地那非苯环上乙氧基衍生为丙氧基, 国内未见报道。总结该结构类型的质谱行为 规律, 可有效帮助此类衍生物的快速结构鉴定。 关键词: 西地那非衍生物; 高分辨四级杆串联飞行时间质谱; 非法添加 中图分类号: R9 17 文献标识码: A 文章编号: 0513-4870 (20 14) 04-0513-04 Identification of a new sildenafil analogue based on Q-TOF-MS * SUN Jian, YU Hong, HU Qing, FENG Rui, ZHANG Su, JI Shen (Shanghai Institutef or Food and Drug Control, Shanghai 201203, China ) Abstract : The drugs such as sildenafil adulterated in herbal products and dietary supplements may endanger human health. The number of the new modified derivatives is increasing recently. Based on Q-TOF-MS, a new sildenafil analogue was found. It was isolated and purified by preparative liquid chromatography. Its structure was determined by NMR, as 1-[4-propoxy-3-(6, 7-dihydro-1-methyl-7-oxo-3-propyl-1H-pyrazolo[4, 3-d] pyrimidin-5-yl)phenylsulfonyl]-4-methylpiperazine. Compared with sildenafil, the ethoxy group of the benzene ring moiety was moved to the propoxy group, which had not been reported in China. The mass spectrometric behavior pattern of the structure type was summarized, which can greatly a