超高效液相色谱-高分辨质谱法筛查婴幼儿配方奶粉中17种头孢菌素类药物残留

建立了一种快速筛查婴幼儿配方奶粉中17种头孢菌素类药物残留的超高效液相色谱-四极杆/静电场轨道阱高分辨质谱（UHPLC-Q-Orbitrap HRMS）分析方法。奶粉样品经水溶解后，使用乙腈提取除去蛋白质等杂质，经低温高速离心后可达到净化样品的目的。选用C8色谱柱对待测物进行分离，在Q Exactive高分辨质谱Full MS/dd-MS²（data-dependent MS²）扫描模式下采集数据进行定性定量分析。17种目标物在5~200 μg/L范围内线性关系良好，相关系数（r²）均大于0.99，检出限0.0060~0.040 μg/L，定量限0.71~4.6 μg/kg，平均回收率69.6%~101.4%，相对标准偏差（RSDs）均小于10%。该法操作简单，重现性好，分辨率高，适用于婴幼儿配方奶粉中17种头孢菌素类药物残留的定性、定量筛查。

Screening of 17 cephalosporin residues in infant formula milk powder by ultra-high performance liquid chromatography-high resolution mass spectrometry

A method for the simultaneous determination of 17 cephalosporinsin milk powder by ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) has been developed. After dissolution in water, the homogenized milk powder samples were extracted with acetonitrile to remove impurities such as proteins and the extract was further purified by high-speed centrifugation at low temperature. A C8 chromatographic column was employed to separate the analytes. Quantitative and qualitative analyses were performed in Q Exactive Full-MS/dd-MS² scan mode. The results revealed an excellent linear correlation over a wide range of analyte mass concentrations (5-200 μg/L) with coefficients of determination (r²) greater than 0.99 in all cases. The limits of detection (LODs) and quantitation (LOQs) were in the range of 0.0060-0.014 μg/L and 0.71-4.62 μg/kg, respectively. The overall average recoveries were 69.6%-101.4% with RSDs<10%. This method presents the advantages of simple operation, good repeatability, and high resolution, being suitable for the qualitative and quantitative screening of 17 cephalosporin residues in infant formula milk powder.