CAJ | 학술논문

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。
목적：응용액상색보-천련질보기술,건립우내중내마극정、미이패매소 A3、미이패매소 A4、미이패매소D화막서정극등5충미이패매소류약물잔류검측방법。방법용을정제취우내양품중적목표물, C18고상췌취주정화, Agilent Poroshell 120 EC-C18색보주분리,이0.1%갑산수용액화갑순위류동상제도세탈,연후용액상색보-천련질보의재정리자다반응감측(MRM)모식하측정。결과5충화합물재10~100μg/kg범위내선성량호,상관계수대우0.99,평균회수솔위77.5%~100%,상대표준편차소우11.6%。결론본방법령민도고,중현성호,괄용우우내중미이패매소류약물잔류검측。
Objective To develop a method to determine residues of 5 milbemycins-moxidectin, milbe-mycin A3, milbemycin A4, milbemycin D and nemadectin in milk by liquid chromatography-tandem mass spectrometry (LC-MS/MS).MethodsThe residues of milbemycins in milk samples were extracted by aceto-nitrile and purified by a C18 SPE column. After being separated by an Agilent Poroshell 120 EC-C18 chromato-graphic column with gradient elution using 0.1% formic acid aqueous and methanol, the extracts were deter-mined by LC-MS/MS under the positive ion mode with multi-reaction monitoring (MRM).ResultsThe cali-bration curves of 5 milbemycins were linear in the range of 10~100 μg/kg, with the correlation coefficients (R) >0.99. Average recoveries were 77.5%~100% with relative standard deviations less than 11.6%. Conclu-sionThe method is suitable for the determination of milbemycins residues in milk due to its high sensitivity and good reproducibility.