液相色谱-串联质谱法测定牛奶中米尔贝霉素类 药物残留

Determination of milbemycins residues in milk by liquid chromatography-tandem mass spectrometry

中文关键词:  米尔贝霉素  牛奶  液相色谱-串联质谱法  残留

英文关键词:milbemycin  milk  liquid chromatography-tandem mass spectrometry  residues

中文摘要:

      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 10~100 μg/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。

英文摘要:

      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). Methods The 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). Results The 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- sion The method is suitable for the determination of milbemycins residues in milk due to its high sensitivity and good reproducibility.