Development and validation method for the determination of selected tetracyclines in animal medicated feedingstuffs with the use of micellar liquid chromatography

Abstract

A chromatographic procedure for the determination of oxytetracycline (OTC), tetracycline (TC), chlorotetracycline (CTC), and doxycycline (DC) in medicated feedingstuffs was developed. Samples were extracted with 0.01 M citric buffer/acetonitrile (pH 3.0) and further purified with 0.45 μm syringe filters. The purified extract was separated on Thermo column C18, 150 × 4 mm, 5 μm and detection was carried out at 360 nm for OTC, and TC, 370 nm for CTC, and 350 nm for DC. TCs were eluted with a mobile phase of 0.03 M SDS/7% 1-butanol/0.02 M oxalic acid/NaOH at pH 2.5. This method provided average recoveries of 80.4% to 100.2%, with CVs of 0.5% to 6.6% in the range of 50 to 1500 mg/kg OTC, TC, CTC, and DC in feeds. The linearity for the four TCs was determined by high-performance liquid chromatography-diode array detector (HPLC-DAD) in the range 10-300 μg/mL (50-1500 mg/kg), with a linear correlation coefficient (R) > 0.99. The LOD and LOQ for TCs in pig and poultry feeds ranged from 4.0 to 10.7 and 4.7 to 12.6 mg/kg, respectively. The methodology was applied to the analysis of animal feedingstuffs collected from poultry and pig farms.

Micellar Liquid Chromatography from Green Analysis Perspective

“…Another interesting application of MLC is the analysis of food samples [81][82][83][84][85][86][87][88][89][90][91][92][93][94][95]. This includes the determination of several compounds in chicken muscles and liver [81][82][83]95]; bovine meat, liver, and kidney [81,82,84,95]; swine kidney [89]; eggs [81,83,93,95]; milk [82,87,93,95]; baby food [82,83,95]; honey [92]; fish sauce [91,94]; feeding staff [86,90]; olive extract samples [85]; and dietetic supplements [88].…”

“…This includes the determination of several compounds in chicken muscles and liver [81][82][83]95]; bovine meat, liver, and kidney [81,82,84,95]; swine kidney [89]; eggs [81,83,93,95]; milk [82,87,93,95]; baby food [82,83,95]; honey [92]; fish sauce [91,94]; feeding staff [86,90]; olive extract samples [85]; and dietetic supplements [88]. MLC has been shown to be a very efficient technique for food analysis, avoiding long and tedious extractions of such complex matrices while providing high percentage recoveries with high accuracy and precision.…”

Methods for the separation, preconcentration, and determination of tetracycline antibiotics

“…A comparatively small number of works [21,24,31,32,46,75,[82][83][84][85] were devoted to the determination of tetracycline antibiotics in feed. Ethyl acetate [24,31,85]; methanol [21,32]; the mixtures of methanol with water [46] or citric acid [83] and acetonitrile with citric acid [84] or formic acid [82]; and a phosphate buffer solution in the presence of trichloroacetic acid [75] were used for the extraction of tetracycline antibi otics from feed.…”

“…Ethyl acetate [24,31,85]; methanol [21,32]; the mixtures of methanol with water [46] or citric acid [83] and acetonitrile with citric acid [84] or formic acid [82]; and a phosphate buffer solution in the presence of trichloroacetic acid [75] were used for the extraction of tetracycline antibi otics from feed. The additional cleaning and precon centration of the extracts are carried out by SPE with the use of an HLB column [83] or a Varian MP1 car tridge [75].…”

Analytical procedure for the determination of tetracyclines in medicated feedingstuffs by liquid chromatography-mass spectrometry

“…There are several analytical techniques used to quantify TCs in feeds: TLC (15), HPLC (4,11,16,17,20), HPCE (11,22), LC/MS, LC-MS/MS (6,8,10), and microbiological assays (15). Nowadays, liquidchromatography coupled with mass spectrometry and tandem mass spectrometry seem to be the techniques of choice for analysis of these groups of antibiotics.…”