超高效液相色谱串联质谱法分析北京油鸡中2种头孢菌素及其代谢物的消解趋势

Analysis of digestion trends of 2 cephalosporins and their metabolites in Beijing You chicken by ultra performance liquid chromatography-tandem mass spectrometry

目的用超高效液相色谱串联质谱法(ultra performance liquid chromatography tandem mass spectrometry,UPLC-MS/MS)分析北京油鸡中2种头孢菌素及其代谢物的消解趋势。方法样品经乙腈-水溶液(4:1,V:V)提取,PRiME HLB固相萃取柱净化,UPLC-MS/MS的多反应监测(multiple reaction monitoring,MRM)模式进行测定。结果给药后0.5 h内,头孢匹林在北京油鸡体内迅速代谢为去乙酰基头孢匹林,二者均可在停药后48 h内消除。头孢噻肟进入北京油鸡体内,在4 h内转化为去乙酰基头孢噻肟;头孢匹林可在停药后48 h内消除;停药后120 h仍可检测到胸肌肉和肾脏中去乙酰基头孢噻肟浓度为27.2和14.5μg/kg。结论在原药代谢较快,不易检出的情况下,检测主要一级代谢物可作为头孢菌素类抗生素残留的重要指标。

Objective To analyze the digestion trends of 2 cephalosporins and their metabolites in Beijing You chicken by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).Methods The samples were extracted with acetonitrile-water solution(4:1,V:V),purified by PRiME HLB solid phase extraction column,and determined by multiple reaction monitoring(MRM)mode of UPLC-MS/MS.Results Within 0.5 h after dosing,cefpirin was rapidly metabolized to deacetylcefpirin in Beijing You chicken,and both could be eliminated within 48 h after discontinuation.Cefotaxime entered Beijing You chicken and was converted to deacetyl cefotaxime within 4 h;Cefpirin could be eliminated within 48 h after discontinuation.Deacetylcefotaxime concentrations of 27.2 and 14.5μg/kg were still detectable in the chest muscles and kidneys 120 h after discontinuation.Conclusion In the case of rapid metabolism of the original drug,which is not easy to detect,the detection of the primary metabolites can be used as an important indicator of cephalosporin antibiotic residues.