摘要
采用了牛肉中头孢噻呋残留检测的超高效液相色谱方法(UPLC).样品中残留的头孢噻呋,用二硫赤藓醇溶液提取,使头孢噻呋及去呋喃甲酰头孢噻呋(DFC)有关代谢物从蛋白或含硫化合物中分离,产生DFC.DFC与碘乙酰胺反应,生成稳定的DFC乙酰胺衍生物(DCA).用C18固相萃取柱对衍生物进行提取.强阴离子交换(SAX)柱纯化,再用强阳离子交换(SCX)柱净化后,进行UPLC分析.头孢噻呋在0.06～10.0μg/mL的质量浓度范围内,呈良好的线性关系;在牛肉组织中添加量分别为500、1 000、2 000μg/kg,添加回收率在80.0%～102%,批内、批间RSD均﹤10%.本方法定量准确,结果重复性好,适用于牛肉中头孢噻呋残留定量分析.
A UPLC method was established for the determination of Ceftiofur in beef. The residual ceftiofur in the sample was extracted with disulfide erythritol solution, and the related metabolites of ceftiofur and DFC were separated from protein or sulfur compounds to produce DFC. DFC was reacted with iodine acetamide to form a stable DFC acetamide derivative(DCA).C18 solid phase extraction column was used to extract the derivatives. Strong anion exchange(SAX) column purification, and then strong cation exchange(SCX) column purification, UPLC analysis. The calibration curves were good linear between the peak areas and concentrations from 0.06～10.0 μ g/mL, the dosage of ceftiofur in beef tissue was 500 g/kg, 1 000 g/kg, 2 000 g/kg,the recovery was 80.0%～102%, RSD was less than 10% in batch and between batches. The method is accurate and reproducible for the determination of ceftiofur residues in beef.
引文
[1]赵静,刘鹏,钱镭.UPLC-MS/MS检测原料奶中脱呋喃甲酰基头孢噻呋残留方法的建立[J].食品工业科技,2014(16):35-37.
[2]李帅鹏,黄显会,孔祥凯.头孢噻呋在猪组织中残留消除规律.畜牧兽医学报,2013,44(8):1311-1316.
[3]刘明生,甘辉群,刘俊栋,等.鸡蛋中头孢噻呋的残留检测技术研究[J].江苏农业科学,2013,41(7):305-306.
[4]董晓云,王静,程林丽,等.超高效液相色谱-串联质谱法测定牛肉中非衍生化的脱呋喃甲酰基头孢噻呋残留量[J].分析试验室,2012(6):42-45.
