QuEChERS-液相色谱-串联质谱法检测鲜蛋中4种大环内酯类抗生素残留  

Determination of 4 kinds of macrolide antibiotics residues in fresh eggs by QuEChERS-liquid chromatography-tandem mass spectrometry

作　　者：李瑶菲 陈冬东[2] 贾景建 余丽波 王一名 李存 彭涛[2] LI Yao-Fei;CHEN Dong-Dong;JIA Jing-Jian;YU Li-Bo;WANG Yi-Ming;LI Cun;PENG Tao(School of Animal Science and Animal Medicine,Tianjin University of Agriculture,Tianjin 300384,China;Chinese Academy of Inspection and Quarantine,Beijing 100176,China;China Inspection Department(Beijing)Test and certification Co.,Ltd.,Beijing 100176,China)

机构地区：[1]天津农学院动物科学与动物医学学院,天津300384 [2]中国检验检疫科学研究院,北京100176 [3]中检科(北京)测试认证有限公司,北京100176

出　　处：《食品安全质量检测学报》2024年第19期20-27,共8页Journal of Food Safety and Quality

基　　金：国家重点研发计划项目(2022YFF1100804)。

摘　　要：目的建立QuEChERS-液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)测定鲜蛋中泰乐菌素A、泰万菌素、红霉素A、替米考星的残留方法。方法样品经80%乙腈水溶液超声涡旋提取,分析液经QuEChERS方法净化,乙腈饱和正己烷去除脂肪,以乙腈与0.1%甲酸水(含5 mmol乙酸铵)为流动相进行梯度洗脱,采用ACQUITY UPLC BEH C_(18)色谱柱进行分离,在电喷雾正离子(electrospray ionization,ESI+)模式,多反应离子监测(multiple reaction monitoring,MRM)模式下检测,基质匹配内标法进行定量。结果对于鲜蛋基质,泰乐菌素A、泰万菌素、红霉素A在0.25~50.00μg/kg,替米考星在0.50~50.00μg/kg的浓度与其相对应的峰面积之间线性关系良好,r^(2)均大于0.999,在3种不同浓度添加水平下,泰乐菌素A、泰万菌素、红霉素A、替米考星的平均回收率为89.05%~109.82%,相对标准偏差为4.59%~11.46%。结论该方法具有较高的准确度、精密度和灵敏度,适用于检测鲜蛋中的泰乐菌素A、泰万菌素、红霉素A、替米考星。Objective To establish a method for determination the residues of tylosin A,tylvalosin,erythromycin A and tilmicosin in fresh eggs by QuEChERS-liquid chromatography-tandem mass spectrometry(LC-MS/MS).Methods The samples were extracted by ultrasonic vortex of 80%acetonitrile solution,the analytical solution was purified by QuEChERS method,and the fat was removed by acetonitrile saturated with n-hexane.The acetonitrile and 0.1%formic acid water(containing 5 mmol ammonium acetate)was used as mobile phase,the flow rate was set to 0.25 mL/min,gradient elution procedure,ACQUITY UPLC BEH C_(18)column separation,electrospray positive ion(ESI+)mode,multiple reaction ion monitoring(MRM)mode detection,and matrix matching internal standard method for quantification.Results For egg matrix,the linear relationship between tylosin A,tylvalosin,erythromycin A at 0.25 to 50.00μg/kg,tilmicosin at 0.50 to 50.00μg/kg and the corresponding peak area was good,and r^(2)was greater than 0.999.At 3 different levels of addition,the average recoveries of tylosin A,tylvalosin,erythromycin A,tilmicosin were 89.05%-109.82%,and the relative standard deviations were 4.95%-11.46%.Conclusion The method exhibits a relatively high accuracy,precision and sensitivity,and is suitable for the detection of tylosin A,tylvalosin,erythromycin A and tilmicosin in fresh eggs.

关 键 词：泰乐菌素A 泰万菌素 红霉素A 替米考星 鲜蛋 液相色谱-串联质谱法 抗生素残留 

分 类 号：O657.63[理学—分析化学] TS253.7[理学—化学]