固相萃取-高效液相色谱-串联质谱法测定禽畜和水产品中沃尼妙林和泰妙菌素

Determination of valnemulin and tiamulin antibiotics residues in domestic animal and aquatic product by solid Phase extraction with liquid chromatography-tandem mass spectrometry

建立了固相萃取-高效液相色谱-串联质谱法测定禽畜和水产品中沃尼妙林、泰妙菌素残留量的分析方法。匀浆样品用乙腈水提取,经盐析和乙腈饱和正己烷除脂后过Oasis MCX SPE小柱净化,采用LC-MS/MS电喷雾电离（ESI）和多反应监测模式（MRM）检测,外标法定量。沃尼妙林和泰妙菌素的检出限均为1.0μg/kg,在1.0～100μg/kg范围内线性关系良好,相关系数r均大于0.99。在1.0～50.0μg/kg的加标水平内的回收率为80.9%～104.3%,RSD为4.7%～7.8%。

A method for simultaneous analysis of valnemulin and tiamulin antibiotics residues in domestic animal and aquatic product was developed by a liquid chromatography tandem mass spectrometry.The sample was extracted with acetonitrile water solution,cleaned up by n-hexane and purified by solid phase extraction（SPE） using oasis MCX extraction catridges.The residues were dissolved with 30% methanol solution and were detected by UPLC-MS/MS.The separation was achieved on a Waters acquity BEH C18 column,and was detected by the MRM mode of the mass spectrometry. The calibration curve was good linear from 1.0μ g/kg to 100 μg/kg with the correlation coefficient more than 0.99. The recoveries for added level in the range of 1.0 - 50.0 μg/kg were 80.9% - 104.3%, and the relative standard deviations were 4.7% - 7.8%. The limit of quantification is 1.0 μg/kg.