保健食品中新型二硫代卡地那非类似物的分析鉴定

Analysis and Identification of A New Dithio-carbodenafil Analogue in Health Foods

关键词:  保健食品  二硫代卡地那非类似物  3,5-二甲基哌嗪基二硫代去甲卡地那非  非法添加  液相色谱-质谱联用  结构鉴定

Key words:  health food  dithio-carbodenafil analogue  3,5-dimethylpiperazinyl dithio-desmethyl carbodenafil  illegal addition  LC-MS/MS  structural identification

摘要:

目的 鉴定保健食品中非法添加的一个未知结构的二硫代卡地那非类似物。方法 采用高效液相色谱-二极管阵列检测器联用（HPLC-DAD）技术进行补肾壮阳类保健食品非法添加筛查时发现一个未知结构的二硫代卡地那非类似物，经过正相硅胶薄层色谱分离纯化得到目标化合物后，用超高效液相色谱-二级质谱联用（UPLC-MS/MS）技术获得其准分子离子和二级质谱图，用核磁共振得到碳谱和氢谱数据，结合文献分析，最终鉴定该化合物的结构。结果 在保健食品中发现了一个新型二硫代卡地那非类似物，结构为3，5-二甲基哌嗪基二硫代去甲卡地那非。结论 该化合物不在现有补肾壮阳类中成药检验标准的13种目标化合物范围内，是一种新的非法添加化学物质。

Abstract:

OBJECTIVE To identify an unknown dithio-carbodenafil analogue illegally adulterated in health foods. METHODS An unknown dithio-carbodenafil analogue was observed in a routine screening for compounds illegally adulterated in heath foods by HPLC-DAD. The compound of interest was isolated by silica gel TLC. Its quasi-molecular ion and MS² fragmentation spectrum were obtained by UPLC-MS/MS, and its ¹³C-NMR and ¹H-NMR spectum were also obtained using nuclear magnetic resonance. Its structure was elucidated by analysis of these data in combination of the literature. RESULTS A new dithio-carbodenafil analogue, which structural was 3,5-dimethylpiperazinyl dithio-desmethyl carbodenafil, was detected in health foods. CONCLUSION It is a new compound illegally adulterated in health foods. The current inspection standard, which lists 13 target compounds, does not include this compound.