保健食品中非法添加西地那非类似物的分析鉴定  

Analysis and identification of illegally added sildenafil analogue in health food

作　　者：黄朝辉 蔡丹丹[2] 陈仲益 

机构地区：[1]宁波市药品检验所,宁波315048 [2]宁波戒毒研究中心,宁波315010

出　　处：《药物分析杂志》2015年第4期694-698,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:鉴定保健食品中非法添加的1个未知结构的西地那非类似物。方法:采用HPLC-DAD进行补肾壮阳类保健食品非法添加筛查时发现1个未知结构的西地那非类似物,经过正相硅胶薄层色谱分离纯化得到目标化合物后,用UPLC-MS/MS获得其相对分子质量和结构碎片,用核磁共振得到氢谱数据,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1个新的西地那非类似物:5-[2-丙氧基-5-(4-羟乙基哌嗪-1-基磺基)苯基]-1-甲基-3-正丙基-1,6-二氢-7H-吡唑并[4,3-d]嘧啶-7-酮(甲羟基豪莫西地那非)。结论:首次在保健品食中检出该化合物。该化合物不在现有补肾壮阳类保健食品非法添加检验标准11种目标化合物范围内,因此有必要对现有标准进行补充,以惩治非法添加者。Objective： To identify an unknown sildenafil analogue illegally adulterated in health food. Methods：An unknown sildenafil analogue was observed during a routine screening by HPLC- DAD for illegal adulteration in heath food for invigorating the kidney and strengthening Yang. The target compound was isolated and purified by silica gel thin layer chromatography（ TLC）. Its molecular weight and structural fragments were gained by UPLC-MS / MS1 and H- NMR spectum was also obtained by using nuclear magnetic resonance（ NMR）. Its structure was finally elucidated through literature analysis. Results： A new sildenafil analogue,5-[2- propoxy- 5-（ 4- hydroxyethyl- piperazin- 1- ylsulfonyl） phenyl]- 1- methyl- 3- propyl- 1,6- dihydro- 7H- pyrazolo[4,3- d]pyrimidin- 7- one（ methylhydroxyhomosildenafil）,was detected in health food. Conclusion： This is the first time that this compound was detected as illegally adulterated in health food. It is very necessary to supplement the current inspection standard of health food for invigorating the kidney and strengthening Yang,as the current standard lists 11 target compounds not including this compound methylhydroxyhomosildenafil,so as to punish the illegal producers in time.

关 键 词：保健食品 非法添加药物鉴定 西地那非类似物 甲羟基豪莫西地那非 超高效液相色谱-串联质谱 

分 类 号：R917[医药卫生—药物分析学]