论文部分内容阅读
目的应用液相色谱-串联质谱技术,建立牛奶中奈马克丁、米尔贝霉素A3、米尔贝霉素A4、米尔贝霉素D和莫西丁克等5种米尔贝霉素类药物残留检测方法。方法用乙腈提取牛奶样品中的目标物,C18固相萃取柱净化,Agilent Poroshell 120 EC-C18色谱柱分离,以0.1%甲酸水溶液和甲醇为流动相梯度洗脱,然后用液相色谱-串联质谱仪在正离子多反应监测(MRM)模式下测定。结果 5种化合物在10~100μg/kg范围内线性良好,相关系数大于0.99,平均回收率为77.5%~100%,相对标准偏差小于11.6%。结论 本方法灵敏度高,重现性好,适用于牛奶中米尔贝霉素类药物残留检测。
OBJECTIVE To establish a method for the determination of 5 milbemycins residues in milk by nematicide, milbemycin A3, milbemycin A4, milbemycin D and moxibutin using liquid chromatography-tandem mass spectrometry . Methods The target compounds in milk samples were extracted with acetonitrile and purified on a C18 solid phase extraction column. The residue was separated on an Agilent Poroshell 120 EC-C18 column. The mobile phase was eluted with 0.1% formic acid in water and methanol as mobile phase. The instrument was tested in positive ion multiple reaction monitoring (MRM) mode. Results The five compounds showed a good linearity in the range of 10-100 μg / kg with the correlation coefficient greater than 0.99, the average recovery of 77.5% -100% and the relative standard deviation of less than 11.6%. Conclusion The method has high sensitivity and reproducibility and is suitable for the determination of milbemycin residues in milk.