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Determination of Tetracycline, Benzimidazole and Quinolone Veterinary Drug Residues in Foodstuffs by High-Throughput Fabric Phase Sorptive Extraction using Titania/Chitosan-Modified Cotton Fabric

Rafiee Parto, Negin | 2025

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  1. Type of Document: M.Sc. Thesis
  2. Language: Farsi
  3. Document No: 57861 (03)
  4. University: Sharif University of Technology
  5. Department: Chemistry
  6. Advisor(s): Bagheri, Habib; Eshaghi, Ali
  7. Abstract:
  8. Veterinary medicines are extensively applied in food producing animals for the treatment of various bacterial infections, so the risk of occurrence of unwanted residues in animal-derived food exists, which may have adverse effects on human health by directly causing disease via low-dose exposure and indirect harm via antibiotic resistance. The major challenges in determination of these residues stem from the complexity of matrix, as well as polar differences and low concentrations of them. This work aimed to develop a screening and quantification method for benzimidazoles, quinolones and tetracyclines residues in egg, milk and chicken muscle. For this, the sample was extracted with acetonitrile, defatted with hexane and cleaned-up on a HLB SPE cartridge. The analytes were identified and quantified by Liquid Chromatography-tandem Mass Spectrometry (LC-MS/MS) after High-Throughput Fabric Phase Sorptive Extraction (HT-FPSE) as a separation and enrichment procedure. The target drug molecules were retained onto the cotton fabric modified by titania/chitosan, in the pH=6-7 medium and back-extracted by acetonitrile before chromatographic determinations. Chemical characterization of the used fabric phase sorptive extraction was studied and experimental variables of FPSE approach were optimized step by step. LC-MS/MS analysis was then carried out by using C8 column, under isocratic conditions with the mobile phase composed of acetonitrile-0.1% FA in water (80:20 v:v), while MS was in the positive ionization mode with Multiple Reaction Monitoring (MRM). The calibration curves showed good linearities with correlation coefficients of 0.9325-0.9993. The relative recoveries were within 85-114.9 % with relative standard deviation of 0.21-9.91 %. The limits of detection and limits of quantification were in the range of 0.01-0.5 and 0.04-1.5 ng mL-1, respectively. Finally, the method has been successfully utilized for the screening of eleven veterinary drug residues in chicken muscle and egg samples from five different provinces of Iran and milk sample from the local markets. Oxytetracycline was detected in both chicken muscle and milk samples with the highest concentrations of 1103 ng g-1 and 1356.38 ng mL-1, respectively. Ciprofloxacin was also detected in egg samples with the highest concentrations of 1349.5 ng g-1
  9. Keywords:
  10. Veterinary Drugs ; Cotton Fabric Modified By Titania/Chitosan ; Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) ; High-Throughput Fabric Phase Sorptive Extraction ; Veterinary Drug Residues

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