Simultaneous determination of seven nitroimidazole residues in meat by using HPLC-UV detection with solid-phase extraction.
A method was developed for the determination of the seven nitroimidazoles including metronidazole (MNZ), ronidazole (RNZ), dimetridazole (DMZ), tinidazole (TNZ), ornidazole (ONZ), secnidazole (SNZ) and the common metabolite of RNZ and hydroxydimetridazole (DMOHZ) in poultry and pork muscles by high-performance liquid chromatography (HPLC) with ultraviolet detection (UV). After extraction with ethyl acetate and evaporation, the nitroimidazoles were redissolved in ethyl acetate and purified using strong cation exchange (SCX) solid-phase extraction (SPE) column. The HPLC separation was carried through on a C(18) bonded silica column with a deionized water-methanol-acetonitrile mobile phase using a gradient elution procedure. The limit of detection of all the seven nitroimidazoles was 0.2 microg/kg. The recoveries of the seven nitroimidazoles for chicken, pork and bacon samples spiked with 1-20 microg/kg were in the range of 71.4-99.5%. The linearity is satisfactory with a correlation coefficient of >0.998 at concentrations ranging from 0.7 to 60 microg/kg. The relative standard deviations of 10 measurements for spiked chicken, pork and bacon samples at the concentration of 1 and 20 microg/kg were in the range of 6.2-13.9% and 4.0-8.7%, respectively. The intra-day precision (n=5) for nitroimidazoles residues in chicken spiked at 20 microg/kg is 6.9%, and the inter-day precision for 5 days (n=25) is 11%. The method is capable of identifying nitroimidazole residues at > or =0.7 microg/kg levels and was applied in the determination of nitroimidazole residues in meat sample.
Sun
Han-Wen
HW
College of Chemistry and Environmental Science, Hebei University, Key Laboratory of Analytical Science and Technology of Hebei Province, Baoding 071002, China. hanwen@mail.hbu.edu.cn
Wang
Feng-Chi
FC
Ai
Lian-Feng
LF
D000818:Animals; D002851:Chromatography, High Pressure Liquid; D008460:Meat / Q000032:analysis*; D009593:Nitroimidazoles / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D012015:Reference Standards; D015203:Reproducibility of Results; D052616:Solid Phase Extraction / Q000379:methods*; D012996:Solutions; D013056:Spectrophotometry, Ultraviolet; D013997:Time Factors
D009593:Nitroimidazoles; D012996:Solutions