一种新型西地那非衍生物的q-tof-ms鉴定.pdfVIP

一种新型西地那非衍生物的Q-TOF-MS 鉴定 孙健，于泓，胡青，冯睿，张甦，季申* (上海市食品药品检验所，上海201203) 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- 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 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 accelerate the structural analysis of novel analogues. Keywords sildenafil analogue ；Q-TOF-MS ；adulteration 以西地那非（结构见图1）为代表的磷酸二酯酶5（phosphodiesterase 5 ，PDE-5 ） 抑制剂被广泛用于治疗勃起功能障碍（ED ），但该类药物的心血管等副作用也屡 [1] 见报道 。近年来，一些宣称具有增强性功能及抗疲劳等功效的中成药及保健食 品中被检出含该类化合物，且未见报道的新型衍生物层出不穷，给监管工作造成 一定困难。西地那非衍生物结构修饰主要为嘧啶环上氧替 为硫，如硫代西地那 [2] [3] 非 ；吡唑环1 位、3 位的结构修饰，如mirodenafil ；苯环上氧取代基的修饰， [4] [5] 如udenafil ；哌嗪环上结构修饰，如艾地那非 。 ________________________________ *通讯作者Tel：021 Email: j ishen2013@ 163.com