UPLC-MS/MS快速测定貉组织中4种硝基呋喃代谢物残留量的研究

Study on Rapid Determination of Nitrofuran Metabolites in Racoon Dog Tissues by UPLC-MS/MS

为了解皮用貉子胴体中硝基呋喃类药物残留情况,建立貉组织中硝基呋喃代谢物残留量准确、快速测定的超高效液相-串联质谱法(UPLC-MS/MS),采用貉子肌肉样品,在酸性条件下,经60℃高温衍生1 h,调节pH值7~8后用乙酸乙酯提取,水浴浓缩后,经正己烷除脂净化,由超高效液相色谱-串联质谱仪在正离子模式下检测,内标法定量。结果表明:4种硝基呋喃代谢物在0.25~50μg/kg范围内线性良好,相关系数r>0.999。貉肌肉组织中4种硝基呋喃代谢物检出限(LOD)均为0.1μg/kg,定量限(LOQ)均为0.25μg/kg。在0.25~2μg/kg范围内的四个添加水平4种硝基呋喃代谢物的回收率为89.7%~108%,相对标准偏差为1.32%~10.5%(n=6)。说明该方法操作简单,灵敏度高、准确性好,适用于貉组织中硝基呋喃类代谢物残留的检测。

A method for rapid and accurate determination of nitrofuran metabolite residues in raccoon dog was developed using ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The samples of raccoon dog muscle were hydrolyzed derivatization at 60℃for 1 h under acidic conditions,adjusting pH 7~8,and then concentrated in water bath,and purified with n-hexane.The samples were detected by UPLC-MS/MS in positive ion mode,and quantified by internal standard method.The limit of detection(LOD)was 0.1μg/kg,and the limit of quantification(LOQ)was 0.25μg/kg.The correlation coefficent was greater than 0.999(r>0.999)within 0.25~50.0μg/kg linear ranges.The recoveries of four nitrofuran metabolites at four levels in the range of 0.25~2μg/kg were between 89.7%~108%,and the relative standard deviations(RSD)were between 1.32%~10.5%(n=6).The method is simple,sensitive and accurate.It is suitable for the determination of nitrofuran metabolic residues in raccoon dog tissue.