高效液相色谱-电喷雾电离三级四极杆质谱检测动物源食品中氯霉素、甲砜霉素、氟苯尼考残留量

Determination of chloramphenicol,thiamphenicol and florfenicol residue in original animal food by HPLC-ESI-MS/MS

建立了动物源产品中氯霉素、甲砜霉素、氟苯尼考残留量的高效液相色谱-电喷雾电离三级四极杆质谱（LC—ESI—MS／MS）的方法。前处理方法包括添加同位素内标氯霉素-d5，碱化乙酸乙酯提取，C18小柱净化。该方法采用负离子．多反应监测氯霉素四对离子（321．0／151．9，321．0／256．6，321．0／194．2，321．0／175．4），甲砜霉素两对离子（354．1／185．0，354．1／290．0），氟苯尼考两对离子（356．0／335．9，356．0／185．1）和同位素内标氯霉素-d5（326．0／157．1）。该方法线性范围为0．1-1．6μg／kg；对不同基质样品的加标回收率为80％-112．5％；相对标准偏差小于11％；方法的测定低限为0．1μg／kg。

A method for the determination of chloramphenicol, thiamphenicol and florfenicol residues in original animal food by HPLC- ESI- MS/MS was developed. In sample pretreatment, an isotope internal standard （CAP- d5） was added, and the samples were extracted with basic ethyl acetate and cleaned up with C18 calumn. Mass spectrometry was performed in negative ion mode with multiple reaction monitoring of four precursor/product ion transitions for chloramphenicol （321.0/151.9, 321.0/256.6, 321.0/194.2, 321.0/175.4）, two precursor/product ion transitions for thiamphenicol （354.1/185.0, 354.1/290.0） and florfenicol （356.0/335.9, 356.0/185.1 ）, and one precursor/product ion transition for isotope intemal standard CAP- d5 （326.0/157.1）. Recoveries were between 80% - 112.5% in different matrix. Relative standard deviations was below 11%. The detection limit was 0.1 μg/kg.