Spectrophotometric flow-injection analysis assay of tetracycline antibiotics using a dual light-emitting diode based detector

In this paper, a small dual light-emitting diode (LED)-based detector for FIA process analyser has been designed. The detector’s optical parts comprise a flow-through cell, a dual-blue LED and a photodiode. Neither mirrors nor lenses are used. The optical path for the first LED detects the blank, while the other LED detects the sample. The detector’s electronic components including a signal amplifier and an A/D converter are integrated on one small board connected to a PC for measuring the results. The designed spectrophotometric detector was used for the determination of tetracycline antibiotics. Uranyl acetate was used as a reagent forming orange-red complexes with the drugs in N,N– dimethylformamide. The complexes show absorption maxima at 410, 416 and 408 nm for tetracycline hydrochloride (TCH), chlortetracycline hydrochloride (CTCH), and doxycycline hydrochloride (DCH), respectively. The detection limit was found to be 0.38, 0.75, 1.44 µg mL-1 and the linear range was obtained at 1.0-3.0, 3.0-5.0, and 3.0-10.0 µg mL-1 for TCH, CTCH and DCH, respectively. The proposed method has been successfully applied to the determination of tetracycline antibiotic residues in milk samples. Moreover, this method is an environmentally friendly approach and suitable for routine analysis

On-line preconcentration and determination of tetracycline residues in milk using solid-phase extraction in conjunction with flow injection spectrophotometry

A simple, cheap and highly sensitive system with on-line preconcentration using solid-phase extraction in conjunction with flow injection spectrophotometry for the determination of tetracycline residues in milk samples is described. C18 was used as packing material in a designed minicolumn used for preconcentration of tetracyclines. Tetracycline standard or sample solutions were dissolved in a mixed buffer solution of pH 4.0 containing boric acid, citric acid and sodium phosphate, then loaded to the minicolumn for 6 min followed by elution with a solution containing methanol : mixed buffer solution (40:60 by volume) of pH 6.5 The absorbance of the eluate was measured at 370 nm. The calibration graph was linear in the range of 0.20-1.00, 0.20-4.00, and 0.20-1.00 mg L-1 for tetracycline (TC), oxytetracycline (OTC), and chlortetracycline (CTC) respectively. The limits of detection were 0.08, 0.10, and 0.09mg L-1 for TC, OTC, and CTC respectively. Relative standard deviations for 20 replicated determinations of 0.20, 0.40, and 0.60 mg L-1 of TC were 7.03, 7.23, and 6.55 % respectively. Per cent recoveries for four commercial types of milk: U.H.T., pasteurised, raw, and sterilised milk were in the range of 86–109 (TC), 90–109 (OTC), and 89–108 (CTC). The sample throughput was 6 h-1