QuEChERS EMR-Lipid结合LC-MS/MS测定鸡蛋中磺胺类和喹诺酮类药物残留

Determination of Sulfonamides and Quinolones in Eggs by QuEChERS EMR-Lipid and High Performance Liquid Chromatography-Tandem Mass Spectrometry

摘要:

采用QuEChERS EMR-Lipid技术处理样品，建立快速检测鸡蛋中14种磺胺类药物和16种喹诺酮类药物残留的液质联用检测方法。将鸡蛋样品用2%甲酸乙腈8 mL提取，再加入0.5 mL pH 7.0、0.1 mol/L的EDTA缓冲液震荡，用QuEChERS EMR-Lipid快速样品提取技术净化，最后用0.2%甲酸溶液（A相）和乙腈溶液（B相）作为流动相进行梯度洗脱，采用电喷雾离子源的动态多反应监测模式(dynamic MRM)对30种磺胺类药物和喹诺酮类药物进行定性和定量分析。结果显示，30种抗生素添加水平在8~32 μg/kg的回收率为50.09%~102.11%，相对标准偏差小于15.66%，方法检出限为0.00131~0.09717 μg/kg。建立的鸡蛋中磺胺类药物和喹诺酮类药物残留检测的检测方法前处理简单易行，便于操作，方法精密度高，可以满足对鸡蛋中磺胺类药物和喹诺酮类药物快速、准确的检测要求，并适合大批量样品的准确定性和定量分析检测。

Abstract:

A sensitive liquid chromatography-tandem mass spectrometry(LC-MS/MS) method has been developed for assaying fourteen sulfonamides and sixteen quinolone antibiotics in egg samples. The egg samples were extracted with 8 mL 2% formic acid acetonitrile, shaked in 0.5 mL 0.1 mol/L EDTA buffer (pH 7). The extract was purified with QuEChERS EMR-Lipid-based rapid sample treatment method, and gradiently eluted with 0.2% formic acid (A) and acetonitrile (B) as the mobile phase. The electrospray ion source was applied with multiple reaction monitoring (MRM) for qualitative and quantitative analysis of 30 sulfonamides and quinolones. The results showed that the recoveries were 50.09%~102.11% for the 30 antibiotics at spiked levels of 8~32 μg/kg, and the relative standard deviation(RSD) was less than 15.66%. The limit of detection (LOD) for the 30 antibiotics was 0.00131~0.09717 μg/kg. The method of determinating sulfonamides and quinolones is simple, easy, and reliable, which can meet the rapid and accurate detection requirements of sulfonamides and quinolones in eggs.