UPLC-MS/MS法快速测定奶粉中17种喹诺酮类药物

Rapid determination of 17 quinolone residues in milk powder by UPLC-MS/MS

建立了超高效液相色谱质谱联用(UPLC-MS/MS)同时测定奶粉中17种喹诺酮类药物残留的检测方法。研究了适用于不同脂肪含量奶粉的前处理方法和上机条件。样品溶解后,加入甲醇/乙腈混合溶液提取,通过Oasis Prime HLB固相萃取柱直接进行净化,氮吹定容后,采用电喷雾正离子多反应监测模式进行检测,外标法定量。17种喹诺酮类药物定量限为3.0μg/kg。当喹诺酮类药物添加范围3.0～60μg/kg时,基质效应57.4%～130.2%,回收率65.3%～104.8%,相对标准偏差0.6%～8.9%。该方法具有简单方便,快速高效,适用于不同脂肪含量奶粉产品检测的特点。

A ultra performance liquid chromatography-aandem mass spectrometry(UPLC-MS/MS)method for simultaneous determination of seventeen quinolone residues in milk powder has been developed.Pretreatment method,liquid phase condition and mass spectrometry for high fat milk powder and others were studied.The sample was dissolved by water,and then extracted by the mixture of methanol and acetonitrile,followed by cleanup of the extract through a Oasis Prime HLB solid phase extraction column directly.After the filtrate was dried by nitrogen blowing method and redissolved.The analysis was carried out by a positive electrospray ion multiple reaction monitoring mode and An external standard method was applied for quantification.The limits of quantification(LOQ)were 3.0μg/kg for seventeen quinolones.The ranges of the matrix effects,the recovery values,and the relative standard deviation were 57.4%-130.2%,65.3%-104.8%and 0.6%-8.9%respectively at fortification levels of 3.0~60μg/kg for seventeen quinolones.This method was simple,convenient,fast,efficient and suitable for the quantification and confirmation of quinolone residues in milk powder products with different fat contents.