超高效液相色谱-串联质谱法测定鸡组织中泰乐菌素的残留量

建立了鸡组织中泰乐菌素残留的超高效液相色谱-串联质谱法检测方法,样品用甲醇(含2%氨水)提取,经C18固相萃取柱净化,洗脱液氮气吹干,残渣用甲醇:乙腈(20∶80,V/V)复溶,超高效液相色谱-串联质谱法检测,基质添加标准溶液外标法定量。结果表明泰乐菌素在5~1000μg/kg的浓度范围内呈现良好的线性关系。在鸡组织中中泰乐菌素的检测限为4μg/kg,定量限为10μg/kg。在10~200μg/kg添加浓度范围内,泰乐菌素在鸡组织中的回收率均在85.9%~110.4%之间,批内批间变异系数在1.2%~4.0%之间。该方法各项技术指标均能满足残留检测要求,且方法的重现性良好,满足国内外兽药残留相关法规规定。

Determination of tylosin residues in chicken tissues by liquid chromatography-tandem mass spectrometry

A liquid chromatography-tandem mass spectrometry (LC-MS / MS method for the determination of tylosin residues in chicken tissues was developed. The samples were extracted with methanol (containing 2% ammonia) , purified by C18 solid phase extraction column, and the eluted liquid was dried by nitrogen. The residue was redissolved with methanol: Acetonitrile (20:80, V / V),determination by High-performance liquid chromatography-tandem mass spectrometry and quantitative analysis by external standard solution added to Matrix. The results showed that tylosin showed a good linear relationship in the concentration range of 5 ng / mL ~ 1000 ng / mL. The detection limit of tylosin in chicken tissues was 4 g / kg and the quantitative limit was 10 g / kg. In the range of 10 G / kg ~ 200 G / kg, the recoveries of tylosin in the tissues of and chickens were 60% ~ 120% , and the coefficient of variation between batches was less than 20% . All the technical indexes of the method can meet the requirements of residue detection, and the reproducibility of the method is good, which can meet the requirements of relevant laws and regulations of veterinary drug residue at home and abroad.