HPLC和LC-MS/MS鉴定锁阳固精丸中非法添加的西地那非衍生物  

Identification of Sildenafil Analog Illegally Added in Dietary Supplement using HPLC and LC-MS/MS

作　　者：向智敏[1] 张骊[2] 祝明[1] 郑成[1] 

机构地区：[1]浙江省药品检验所,杭州310004 [2]浙江工商大学食品与生物工程学院,杭州310035

出　　处：《中国现代应用药学》2010年第2期167-171,共5页Chinese Journal of Modern Applied Pharmacy

摘　　要：目的鉴定中成药中非法掺入的西地那非衍生物。方法采用高效液相色谱-二极管阵列检测器法(HPLC-DAD)和液相色谱-电喷雾电离-质谱联用法(LC-ESI-MS/MS),定性分析锁阳固精丸中非法掺入的西地那非衍生物。结果通过比较被测样品成分和西地那非对照品的紫外吸收光谱图,并对两者的质谱碎片数据进行解析和研究,确认西地那非的一种衍生物羟甲基西地那非(hydroxyhomosildenafil)。结论利用液相色谱-质谱联用法(LC-MS/MS),结合质谱分子结构解析技术,具有专属性强的特点,可以准确分析中成药中非法添加的西地那非衍生物。OBJECTIVE To establish a method based on mass spectrometry structural assignments for identification of sildenafil analog added illegally in herbal product.METHODS A high-performance liquid chromatography-diode array detection（HPLC-DAD） method and a liquid chromatography-electrospray ionization tandem mass spectrometry（LC-ESI-MS/MS） method were applied.RESULTS Identification of hydroxyhomosildenafil,an analog of sildenafil was achieved by comparing UV spectrum and mass fragmentation results of the samples with those of sildenafil.Three batches of Suoyang Gujing Wan,a dietary supplement,were found containing hydroxyhomosildenafil.CONCLUSION Based on structural assignments of mass fragments,analog of sildenafil could be rapidly and accurately determined in herbal product.

关 键 词：西地那非衍生物 羟甲基西地那非 液相色谱-质谱-质谱法 

分 类 号：R917.101[医药卫生—药物分析学]