title: High-performance liquid chromatography with fluorescence detection for the determination of nitrofuran metabolites in pork muscle.
abstract: A simple and sensitive HPLC method with fluorescence detection (HPLC-FLD) is reported for the simultaneous determination of metabolites of four nitrofuran drugs (furazolidone, furaltadone, nitrofurantoin and nitrofurazone) in pork muscle. The method involves acid hydrolysis of the protein-bound drug metabolites and the conjugation of the released side-chains with a novel fluorescence agent 2-hydroxy-1-naphthaldehyde. After liquid-liquid extraction and effective separation of the derivatives on a YMC-Pack Polymer C18 column at 40°C under alkaline conditions, the high fluorescence intensity of these derivatives at emission wavelength λem = 463 nm enables their simultaneous determination in pork muscle at concentrations as low as 1 µg kg⁻¹. The method was validated using blank pork muscle fortified with all four metabolites at 0.5, 1.0 and 2.0 µg kg⁻¹. Recoveries were > 92.3% with RSDs < 8.5% for all four metabolites. The results obtained with HPLC-FLD and LC-MS/MS methods showed very good agreement for pork muscle samples.
authors.affiliation: a College of Chemistry and Chemical Engineering, Fuyang Normal College , Fuyang, Anhui , China.
authors.forename: Liang-Quan
authors.initials: LQ
authors.lastname: Sheng
authors.forename: Ming-Ming
authors.initials: MM
authors.lastname: Chen
authors.forename: Shui-Sheng
authors.initials: SS
authors.lastname: Chen
authors.forename: Na-Na
authors.initials: NN
authors.lastname: Du
authors.forename: Zhao-Di
authors.initials: ZD
authors.lastname: Liu
authors.forename: Chong-Fu
authors.initials: CF
authors.lastname: Song
authors.forename: Rui
authors.initials: R
authors.lastname: Qiao
mesh_terms: D053000:Analytic Sample Preparation Methods; D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis* / Q000737:chemistry / Q000378:metabolism; D001711:Biotransformation; D002273:Carcinogens / Q000032:analysis* / Q000737:chemistry / Q000378:metabolism; D002681:China; D002851:Chromatography, High Pressure Liquid; D004350:Drug Residues / Q000032:analysis* / Q000737:chemistry / Q000378:metabolism; D005456:Fluorescent Dyes / Q000737:chemistry; D005506:Food Contamination; D005513:Food Inspection / Q000379:methods*; D057230:Limit of Detection; D008460:Meat / Q000032:analysis* / Q000191:economics; D018482:Muscle, Skeletal / Q000737:chemistry / Q000378:metabolism; D009153:Mutagens / Q000032:analysis / Q000737:chemistry / Q000378:metabolism; D009281:Naphthalenes / Q000737:chemistry; D009581:Nitrofurans / Q000032:analysis* / Q000737:chemistry / Q000378:metabolism; D015203:Reproducibility of Results; D013050:Spectrometry, Fluorescence; D034421:Sus scrofa
chemical_list: D000900:Anti-Bacterial Agents; D002273:Carcinogens; D005456:Fluorescent Dyes; D009153:Mutagens; D009281:Naphthalenes; D009581:Nitrofurans; C062247:2-hydroxy-1-naphthaldehyde