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

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

Key words:  sildenafil analog  hydroxyhomosildenafil  LC-MS/MS

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。

Abstract:

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.