Development and validation of Analysis Method for Determination of Quinolone Drug Residues in Meat by HPLC-FLD

Abstract

       Quinolone antibacterials are employed and allowed for treatment of infectious diseases in food-producing animals. Drug residues in edible tissues are resulted from improperly using. High levels of residues in food could cause side efects and drug resistances in human. Method for determination of 6 quinolones such as danoloxacin, diloxacin, enroloxacin, saraloxacin, lumiquine and oxolinic acid by HPLC-FLD technique was developed and validated. These analytes were extracted with 0.3% metaphosphoric acid and acetonitrile at ratio 1:10 v/v, fat was removed by liquid-liquid extraction technique with hexane saturated with acetonitrile and then cleaned up by solid phase extraction with HLBC-18 cartridges. Afterwards, qualitative and quantitative analysis of these compounds was conducted by HPLC-FLD. As a result of method validation, limit of detection (LOD) and limit of quantitation (LOQ) were 5 and 10 μg/kg respectively. The linearity of working range was 10-100 μg/kg with coeicient of determination (R²) more than 0.95. The accuracy expressed as mean of %recovery and the precision as HORRAT at concentration level 10, 50 and 100 μg/kg were 65.1-97.8% and 0.3-0.9 respectively. The matrix efect was tested by paired t-test and found that there was non-signiicant diference at level of conidence 95% (μ = 0.05). Participation in proiciency testing program by interlaboratory comparison showed that |Z| less than 2. The characteristics of this method were it for intended use in testing laboratory for requirement of the notiication of Ministry of Public Health (Vol.303) B.E.2550. Moreover, the survey of quinolone drug residues in 60 samples of chicken, pork and beef from 11 markets in Bangkok and Nonthaburi province was performed. It showed that 1 chicken sample was found oxolinic acid 29.59 μg/kg, and 2 samples were found enroloxacin 16.1 and 16.9 μg/kg.