基于液相色谱-飞行时间质谱建立的非法添加物广谱筛查方法

Wide-scope screening of illegal additives by HPLC-QTOF

关键词:  非法添加  靶向筛查  非靶向筛查

Key words:  illegal additive  target screening  non-target screening

摘要:

目的 基于液相色谱-飞行时间质谱建立了非法添加物的广谱筛查方法,包括了基于数据库搜索的靶向筛查策略和基于特征离子的非靶向筛查策略。方法 利用HPLC-QTOF通过243种对照品分类建立筛查数据库,通过MassHunter软件的Find By Formular 算法匹配保留时间、一级和二级质谱图进行靶向筛查。总结裂解规律,选择特征离子,利用Find By Auto MS/MS算法结合裂解规律进行非靶向筛查。结果 筛查了100批样品,其中既检出了对乙酰氨基酚、双氯芬酸、西地那非、酚酞、西布曲明等靶向物质,也筛查出二乙氨基前他达拉非等非靶向物质。结论 该方法具有快速、高通量等特点,为多种非法添加物的高通量广谱筛查提供了新的思路。

Abstract:

ABSTRACT: OBJECTIVE A method for comprehensive screening of illegal additives was developed based on HPLC-QTOF high resolution mass spectrometry including target and non-target screening. METHODS 243 compounds were selected to build an in-house database. Identification were conducted by comparing the retention times, the exact masses of precursor ions and fragmentations. According to the structural similarity of diverse illegal additives the diagnostic common ions of class-specific compounds were found, which were used as non-target screening. RESULTS The method was applied to analyze 100 samples, among which 4-Acetamidophenol, Diclofenac, Sildenafil, Phenolphthalein, Sibutramine were found. In particular, Diethylaminopretadalafil were detected out of the in-house database using non-target screening strategy. CONCLUSION In this studying a target and non-target screening method for illegally added medicines was established, which was useful in the high-throughput screening of illegal additives.