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

中文关键词:  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

英文关键词:tylosin A  tylvalosin  erythromycin A  tilmicosin  egg  liquid chromatography-tandem mass spectrometry  antibiotic residue

中文摘要:

      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，乙腈饱和正己烷去脂，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 C18色谱柱进行分离，在电喷雾正离子模式（electrospray ionization, ESI+），多反应离子监测模式（multiple reaction monitoring，MRM）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0.50~50.00 μg/kg的浓度与其相对应的峰面积之间线性关系良好，R2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。

英文摘要:

      Objective To establish a test method for tylosin A, tylvalosin, erythromycin A and tilmicosin in eggs by QuEChERS-liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods The samples were extracted by ultrasonic and vortex of 80% aqueous acetonitrile, the analytical solution was purified by QuEChERS method, saturated with n-hexane, centrifuged and tested on the machine. The acetonitrile and 0.1% formic acid water (containing 5 mmol of ammonium acetate) was used as mobile phase, the flow rate was set to 0.25 mL/min, gradient elution procedure, ACQUITY UPLC BEH C18 column separation, electrospray positive ion mode (ESI +), multiple reaction ion monitoring mode (MRM) 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 50.00 μg/kg, tilmicosin at 0.50 to 50.00 μg/kg and the corresponding peak area was good, and R2 was greater than 0.999. At 3 different levels of addition, the average recovery of tylosin A, tylvalosin, erythromycin A, tilmicosin was 89.05%-109.82%, and the relative standard deviation was 4.95%-11.46%. Conclusion This method has a relatively high accuracy, precision and sensitivity, and is suitable for the detection of tylosin A, tylvalosin, erythromycin A and tilmicosin in fresh eggs.