Ostro孔板结合UPLC-MS/MS测定牛奶中的6种喹诺酮类药物残留  

Determination of 6 quinolones drug residues in milk by Ostro orifice plate combined with UPLC-MS/MS

作　　者：王彦鹏 张飙 李鹏 仇建飞[2] WANG Yanpeng;ZHANG Biao;LI Peng;QIU Jianfei(Logistics Support Office,Jilin Agricultural University,Changchun 130118,China;Institute of Agricultural Quality Standard and Testing Technology,Jilin Academy of Agricultural Sciences,Changchun 130033,China)

机构地区：[1]吉林农业大学后勤保障处,吉林长春130118 [2]吉林省农业科学院农业质量标准与检测技术研究所,吉林长春130033

出　　处：《中国酿造》2025年第2期268-272,共5页China Brewing

基　　金：吉林省科技厅技术创新引导项目(20240404079ZP)。

摘　　要：该研究建立牛奶中6种喹诺酮类药物残留的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。牛奶样品用0.2%甲酸-乙腈提取,Ostro样品制备板净化,经C18色谱柱分离,用5 mmol/L甲酸铵(含0.1%甲酸)-乙腈进行梯度洗脱,在电喷雾离子(ESI+)模式下采用多反应监测(MRM)模式采集,内标法定量。结果显示,6种喹诺酮类药物在5~200 ng/mL的质量浓度范围内线性关系良好,相关系数(R)均>0.999,检出限和定量限均分别为0.2μg/kg和0.5μg/kg。3个不同加标浓度下,平均回收率为80.1%~98.9%,精密度试验结果的相对标准偏差(RSD)为1.9%~9.2%,方法稳定性试验结果RSD为2.6%~10.8%。该方法的前处理步骤简单快捷,检测效率和通量高,适用于牛奶中6种喹诺酮类药物的快速筛查和定量定性分析。An ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the determination of 6 quinolones drug residues in milk was established.The milk samples were extracted with 0.2%formic acid-acetonitrile,purified by Ostro sample preparation plate,separated by C18 column,gradient elution was performed with 5 mmol/L ammonium formate(containing 0.1%formic acid)-acetonitrile,collected with multiple reaction monitoring(MRM)mode under electron spray ionization(ESI+)mode,and quantitative by internal standard method.The results showed that the 6 quinolones drug had good linearity in the mass concentration range of 5-200 ng/ml,and the correlation coefficients(R)were all greater than 0.999.The limits of detection and limits of quantification were 0.2μg/kg and 0.5μg/kg,respectively.The average recovery rates were 80.1%-98.9%at 3 different standard concentrations,the relative standard deviation(RSD)of precision tests results were 1.9%-9.2%,and the RSD of the method stability tests results were 2.6%-10.8%.The pre-treatment step of this method was simple and fast,the detection efficiency and throughput were high,and it was suitable for rapid screening,quantitative and qualitative analysis of 6 quinolones drug in milk.

关 键 词：牛奶 Ostro样品制备板 UPLC-MS/MS 喹诺酮类 

分 类 号：TS207.5[轻工技术与工程—食品科学] O657.7[轻工技术与工程—食品科学与工程]