title: Development and validation of an ultra high performance liquid chromatography tandem mass spectrometry method for determination of 10 cephalosporins and desacetylcefapirin in milk.
abstract: A simple, sensitive and reliable analytical method was developed for the simultaneous determination of 10 cephalosporins and desacetylcefapirin in bovine milk by ultra high performance liquid chromatography-positive electrospray ionization tandem mass spectrometry (UHPLC-ESI-MS/MS). Samples were directly purified through HLB cartridge after dilution with 50mM phosphate buffer solution (pH 8.5). Then the eluate was dried under nitrogen and the residue was redissolved in mobile phase. Samples were analyzed by LC-MS/MS on an Acquity UPLC BEH Shield RP18 column with gradient elution. The samples were quantified using ceftiofur-D3 as internal standard. The proposed method was validated according to the European Commission Decision 2002/657/EC. The CCα values were 111, 0.04, 140, 55, 55, 67, 23, 23, 68, 0.10 and 113μg/kg for cefalexin, cefradine, cefacetrile, cefazolin, cefoperazone, cefapirin, cefalonium, cefquinome, desacetylcefapirin, cefotaxime and ceftiofur, respectively. The mean recoveries, repeatability (expressed as coefficient of variation, CVr), and reproducibility (CVR) varied from 94.6% to 117.1%, from 5.6% to 13.6% (CVr), and from 5.9% to 27.9% (CVR), respectively. The method is demonstrated to be suitable for the determination of 10 cephalosporins and desacetylcefapirin in bovine milk. The total time required for the analysis of one sample, including sample preparation, was about 40min.
authors.affiliation: Animal Science and Technology College, Beijing University of Agriculture, Beijing 102206, PR China.
authors.forename: Xiao-Lin
authors.initials: XL
authors.lastname: Hou
authors.forename: Yin-Liang
authors.initials: YL
authors.lastname: Wu
authors.forename: Yan
authors.initials: Y
authors.lastname: Lv
authors.forename: Xiu-Qin
authors.initials: XQ
authors.lastname: Xu
authors.forename: Jian
authors.initials: J
authors.lastname: Zhao
authors.forename: Ting
authors.initials: T
authors.lastname: Yang
mesh_terms: D000818:Animals; D002417:Cattle; D002511:Cephalosporins / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D002514:Cephapirin / Q000031:analogs & derivatives* / Q000032:analysis / Q000737:chemistry / Q000302:isolation & purification; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004355:Drug Stability; D016014:Linear Models; D008892:Milk / Q000737:chemistry*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D002511:Cephalosporins; D002514:Cephapirin; C049805:desacetyl cephapirin