色谱2018，Vol.36Issue(4)：345-350,6.DOI:10.3724/SP.J.1123.2017.11007
QuEChERS-超高效液相色谱-串联质谱法测定牛奶中6种头孢菌素类抗生素残留
Determination of six cephalosporin residues in milk by QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry
摘要
Abstract
A simple,rapid and sensitive method for the simultaneous determination of six cephalosporin(cephalexin,cephapirin,cefotaxime,cefazolin,cefalonium and cefquinome) residues in milk was developed by QuEChERS coupled with ultra high performance liquid chro-matography-tandem mass spectrometry(UPLC-MS/MS). The milk samples were extracted with 10 mL acetonitrile containing 1%(v/v)acetic acid,and then centrifuged for 10 min. The super-natant was cleaned up with 100 mg C18 adsorbent powder. The analytes were separated on a reversed phase HSS T3 column(100 mm×2.1 mm,1.8 μm)using acetonitrile and water con-taining 0.1%(v/v)formic acid as mobile phases with gradient elution. An electrospray ioniza-tion(ESI)source was used in the multiple reaction monitoring(MRM)mode. The analytes were quantified using an external standard method. The linear relationships of the six cephalo-sporins were good and the correlation coefficients(r)were greater than 0.999. The limits of detection(LODs)and the limits of quantification(LOQs)for the analytes were in the range of 0.2-0.6 μg/kg and 0.8-2 μg/kg,respectively. The recoveries of the target analytes were between 75.1% and 94.4%at spiked levels of 8,16,80 μg/kg. The relative standard deviations (RSDs)were no more than 8.3%(n=6). The method is simple and sensitive,and can be suit-able for the analysis of the cephalosporin residues in milk.关键词
超高效液相色谱-串联质谱/QuEChERS/头孢菌素类抗生素/牛奶Key words
ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)/QuEChERS/cephalosporins/milk分类
化学化工引用本文复制引用
张小刚,王霞,戴春风,陈美莲..QuEChERS-超高效液相色谱-串联质谱法测定牛奶中6种头孢菌素类抗生素残留[J].色谱,2018,36(4):345-350,6.基金项目
公益性行业(农业)科研专项(201403071).Special Public Welfare Industry(Agriculture)Research(No.201403071). （农业）
