title: Determination of nitrofuran metabolites in shrimp by high performance liquid chromatography with fluorescence detection and liquid chromatography-tandem mass spectrometry using a new derivatization reagent.
abstract: A high performance liquid chromatography with fluorescence detection (HPLC-FLD) method for the simultaneous determination of total nitrofuran metabolite residues (furazolidone, furaltadone, nitrofurantoin, and nitrofurazone) in shrimp was developed. The method involves the acid hydrolysis of protein-bound metabolites, followed by the derivatization of the freed metabolites with the new fluorescent derivatization reagent 2-hydroxy-1-naphthaldehyde (HN) and subsequent liquid-liquid extraction (LLE). Separation is achieved on a YMC-Pack Polymer C18 column under alkaline conditions, and the high fluorescence intensity of the derivatives at an emission wavelength Em=463nm (Ex=395nm) enables, for the first time, their simultaneous determination in shrimp at concentrations as low as 1μg/kg by HPLC-FLD. The method was validated using blank shrimp fortified with all four metabolites at 0.5, 1.0 and 2.0μg/kg. Recoveries were >87% with relative standard deviations of <8.1% for all four metabolites. Furthermore, the results obtained by HPLC-FLD were in very good agreement with those obtained by LC-MS/MS analysis.
authors.affiliation: College of Chemistry and Chemical Engineering, Fuyang Normal College, Fuyang, Anhui 236041, China.
authors.forename: Na-Na
authors.initials: NN
authors.lastname: Du
authors.affiliation: College of Chemistry and Chemical Engineering, Fuyang Normal College, Fuyang, Anhui 236041, China; College of Chemistry and Chemical Engineering, Anhui University, Hefei, Anhui 230039, China.
authors.forename: Ming-Ming
authors.initials: MM
authors.lastname: Chen
authors.affiliation: College of Chemistry and Chemical Engineering, Fuyang Normal College, Fuyang, Anhui 236041, China; College of Chemistry and Chemical Engineering, Anhui University, Hefei, Anhui 230039, China. Electronic address: shenglq@fync.edu.cn.
authors.forename: Liang-Quan
authors.initials: LQ
authors.lastname: Sheng
authors.affiliation: College of Chemistry and Chemical Engineering, Fuyang Normal College, Fuyang, Anhui 236041, China. Electronic address: chenss@fync.edu.cn.
authors.forename: Shui-Sheng
authors.initials: SS
authors.lastname: Chen
authors.affiliation: College of Chemistry and Chemical Engineering, Fuyang Normal College, Fuyang, Anhui 236041, China.
authors.forename: Hua-Jie
authors.initials: HJ
authors.lastname: Xu
authors.affiliation: College of Chemistry and Chemical Engineering, Fuyang Normal College, Fuyang, Anhui 236041, China.
authors.forename: Zhao-Di
authors.initials: ZD
authors.lastname: Liu
authors.affiliation: College of Chemistry and Chemical Engineering, Fuyang Normal College, Fuyang, Anhui 236041, China.
authors.forename: Chong-Fu
authors.initials: CF
authors.lastname: Song
authors.affiliation: College of Chemistry and Chemical Engineering, Fuyang Normal College, Fuyang, Anhui 236041, China.
authors.forename: Rui
authors.initials: R
authors.lastname: Qiao
mesh_terms: D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D002853:Chromatography, Liquid / Q000379:methods; D005470:Fluorometry; D059625:Liquid-Liquid Extraction; D009581:Nitrofurans / Q000032:analysis* / Q000378:metabolism; D033561:Penaeidae / Q000737:chemistry*; D053719:Tandem Mass Spectrometry / Q000379:methods
chemical_list: D009581:Nitrofurans
keywords: HPLC–FLD; LC–MS/MS; Nitrofuran metabolites; Shrimp