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  

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

作　　者：程建桥 张峰[1] 许秀丽[1] 洪云鹤 吴寒秋 王传胜 CHENG Jianqiao;ZHANG Feng;XU Xiuli;HONG Yunhe;WU Hanqiu;WANG Chuansheng(Institute of Food Safety,Chinese Academy of Inspection&Quarantine,Beijing 100176,China;College of Applied Chemistry,Shenyang University of Chemical Technology,Shenyang 110142,China)

机构地区：[1]中国检验检疫科学研究院食品安全研究所,北京100176 [2]沈阳化工大学应用化学学院,辽宁沈阳110142

出　　处：《色谱》2018年第8期809-816,共8页Chinese Journal of Chromatography

基　　金：中央级科研院所社会公益研究专项资金项目(2017JK003);应对国际贸易食品安全法规精准检测关键技术研究(2017YFC1601600)~~

摘　　要：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/ddMS2(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5~200μg/L范围内线性关系良好,相关系数(r^2)均大于0.99,检出限0.006 0~0.040μg/L,定量限0.71~4.6μg/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。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-MS 2 scan mode.The results revealed an excellent linear correlation over a wide range of analyte mass concentrations(5-200μg/L)with coefficients of determination(r 2)greater than 0.99 in all cases.The limits of detection(LODs)and quantitation(LOQs)were in the range of 0.006 0-0.014μg/L and 0.71-4.62μg/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.The results showed an exceptional linear relationship with the concentrations of analytes over wide concentration ranges(5-200μg/L)as all the fitting coefficients of determination(r 2)were greater than 0.99.All the limits of detection(LODs)and quantification(LOQs)were in the respective range of 0.006-0.04μg/L and 0.71-4.6μg/kg.Overall average recoveries were 69.6%-101.4%with RSDs<10%.The method has the advantages of simple operation,good repeatability and high resolution.It is suitable for the qualitative and quantitative screening of the 17 cephalosporin residues in infant formula milk powder.

关 键 词：超高效液相色谱 高分辨质谱 头孢菌素 婴幼儿配方奶粉 高通量筛查 食品安全 

分 类 号：O658[理学—分析化学]