Residue Determination Of Sulfonamides, Fluoroquinolones And Rodenticides Drugs By High Performance Liquid Chromatography With Accelerated Solvent Extraction

The residue of drug has structured potential harm to the consumers’ health and safety. Toensure food safety, the European Community, and China Agriculture Department have laiddown the maximum residue level (MRL) of sulfonamides (SAs) and fluoroquinolones (FQs).Therefore, there is an urgent need to develope rapid，sensitive and veracious method forsimultaneous determination of the drug residues at the low concentrations in animal originfoods. In addition, anticoagulant rodenticides (ARs) with the characteristics of broadspectrum, high efficiency, toxic effect slowly are widely used in indoor and field deratization.Anticoagulant rodenticides poisoning cases occur repeatedly, intimidating human health. Thispaper focalize on methodology for the determination of SAs, FQs and ARs residues in foodand body fluid. The paper is divided into three chapters:Chapter1: The high performance liquid chromatography (HPLC) technique, acceleratedsolvent extraction and their application are introduced briefly. The analytical research anddevelopment status of sulfonamides, fluoroquinolones and rodenticides were reviewed.Chapter2: A new accelerated solvent extraction (ASE)-solid phase extraction (SPE)-highperformance liquid chromatography (HPLC) method is developed for determination ofsulfonamides and fluoroquinolones in pork and chicken muscle. Under the optimizedconditions, The chalibration cueves for the determination of sulfadiazine, sulfamerazine,sulfametoxydiazine and sarafloxacin have a good linearity (r＞0.9999). The method limits ofquantification (LOQs) were4~12μg/kg. Intra-and inter-day precisions (RSDs) were0.3~1.5%and0.7~1.8%, respectively. Their average recoveries with four spiked levels rangedfrom83%to108%with the RSD of0.3~1.5%. This method provides an effective extractionprocedure and high sensitivity, and can be applied for the determination of4residual drugs inpork and chicken muscle at lower than their MRL levels.Chapter3: A new accelerated solvent extraction (ASE)-high performance liquidchromatography (HPLC) method is developed for determination of anticoagulants rodenticides in foodstuff and body fluids. Under the optimized conditions, crimidine,bromadiolone, warfarin, and coumatetralyl were determined. Good linearity was achievedwith a correlation coefficient (r) of0.9999. The limits of quantification for the fourrodenticides ranged from2.2μg/kg (crimidine) to13μg/kg (bromadiolone) for solid samplesand from0.02μg/mL (crimidine) to0.15μg/mL (bromadiolone) for liquid samples. Theproposed method has the characteristic of high precision, sensitivity and accuracy as well aslow consumption of reagents. The proposed HPLC method was successfully applied for theanalysis of the four anticoagulant rodenticides in rice, corn, whole blood, and urine samples.