The use of a monolithic column to improve the simultaneous determination of four cephalosporin antibiotics in pharmaceuticals and body fluids by HPLC after solid phase extraction--a comparison with a conventional reversed-phase silica-based column.
The use of a monolithic column (Chromolith, SpeedROD RP-18e, by Merck) was studied on the determination of cephalosporin antibiotics. Results were compared with those from a previously developed analytical method using conventional silica-based analytical column. A rapid, accurate and sensitive method has been developed and validated for the quantitative simultaneous determination of four cephalosporins: Cephalexine and Cephadroxil (first generation), Cefaclor (second generation) and Cefotaxim (third generation) in pharmaceuticals as well as in human blood serum and urine. Hydroflumethiazide (HFM) (3,4-dihydro-6(trifluoromethyl)-2H-1,2,4-benzothiadiazine-7-sulfonamide-1,1-dioxide) was used as an internal standard at a concentration of 1.5 ng/microL. A rectilinear relationship was observed up to 5 ng/microL for the four compounds. Analysis time was less than 4 min. The statistical evaluation of the method was examined by means of within-day repeatability (n=8) and day-to-day precision (n=8) and was found to be satisfactory with high accuracy and precision results. The method was applied to the determination of the cephalosporins in commercial pharmaceuticals and in biological fluids: human blood serum after solid phase extraction and urine simply after filtration and dilution. Recovery of analytes in spiked serum samples was in the range from 88.7 to 107.8%, while for urine samples recovery was from 98.0 to 105.6%. By comparing the figures of merit for the monolithic column and the silica-based one, regarding the determination of the four cephalosporins investigated in the present study, the outstanding efficiency of the monolithic column can be noticed.
Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, GR-54124 Thessaloniki, Greece.
V F
VF
Samanidou
A S
AS
Ioannou
I N
IN
Papadoyannis
D001826:Body Fluids / Q000737:chemistry*; D002511:Cephalosporins / Q000032:analysis* / Q000097:blood / Q000652:urine; D002853:Chromatography, Liquid / Q000379:methods*; D006801:Humans; D004364:Pharmaceutical Preparations / Q000737:chemistry*; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013056:Spectrophotometry, Ultraviolet
D002511:Cephalosporins; D004364:Pharmaceutical Preparations