title: Liquid chromatography and ion trap mass spectrometry for simultaneous and multiclass analysis of antimicrobial residues in feed water.
abstract: This work firstly reported the development of liquid chromatography coupled to an ion trap mass spectrometer (LC-MS ion trap) for the simultaneous determination of nitrofurans (e.g. nitrofurazone (NFZ), nitrofurantoin (NFT), furazolidone (FZD) and furaltadone (FTD)), nitroimidazoles (e.g. metronidazole (MNZ), ronidazole (RNZ) and dimetridazole (DMZ)) and chloramphenicol (CAP) in feed water. Isotope-labeled internal standards for the corresponding target analytes were employed to prevent matrix effects that might lead to signal suppression/enhancement. High performance liquid chromatography (HPLC) analysis was performed on a Prodigy ODS-3 column, 2.0mm×150mm, 5μm with a guard cartridge at a flow rate of 0.2mL/min, column oven temperature of 40°C, and an injection volume of 10μL. Solid phase extraction (SPE) procedures, factors affecting HPLC separation (e.g. buffer pH and concentrations) and mass spectrometry (MS) parameters were optimized. After an off-line SPE by the OASIS HLB cartridges (with an enrichment factor of 400), the eight antimicrobial agents were separated in 18min using a gradient elution of acetonitrile in acidified water (pH 5.0). MS detection was by an ion trap MS coupled with electrospray ionization (ESI) in tandem mass spectrometry mode (MS/MS) using the nebulizer gas at 35psi, drying gas at 9L/min and drying temperature of 325°C. Method linearity was good (r(2)=0.979-0.999) with acceptable precision (% RSDs=3.4-26.6%) and accuracy (%recovery=88.4-110.1%). Very low limits of detection (LOD) and quantitation (LOQ) were achieved in ranges of 0.002-0.06μg/L and 0.005-0.25μg/L, respectively. The established method is successfully employed by the Department of Livestock Development of Thailand for the monitoring of the drug residues in feed waterbecause of its convenience, reliability and high sensitivity.
authors: Bureau of Quality Control of Livestock Products, Department of Livestock Development, Bangkok 10400, Thailand.
authors: Chusak
authors: C
authors: Ardsoongnearn
authors: Bureau of Quality Control of Livestock Products, Department of Livestock Development, Bangkok 10400, Thailand.
authors: Ongart
authors: O
authors: Boonbanlu
authors: Bureau of Quality Control of Livestock Products, Department of Livestock Development, Bangkok 10400, Thailand.
authors: Sunan
authors: S
authors: Kittijaruwattana
authors: Department of Pharmaceutical Chemistry, Faculty of Pharmacy, Mahidol University, Bangkok 10400, Thailand; Center of Excellence for Innovation in Drug Design and Discovery, Faculty of Pharmacy, Mahidol University, Bangkok 10400, Thailand. Electronic address: leena.sun@mahidol.ac.th.
authors: Leena
authors: L
authors: Suntornsuk
mesh_terms: D000890:Anti-Infective Agents / Q000032:analysis*; D002701:Chloramphenicol / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D057230:Limit of Detection; D009581:Nitrofurans / Q000032:analysis*; D009593:Nitroimidazoles / Q000032:analysis*; D015203:Reproducibility of Results; D052616:Solid Phase Extraction / Q000379:methods; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D053719:Tandem Mass Spectrometry; D014867:Water / Q000032:analysis; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D000890:Anti-Infective Agents; D009581:Nitrofurans; D009593:Nitroimidazoles; D014874:Water Pollutants, Chemical; D014867:Water; D002701:Chloramphenicol
keywords: Chloramphenicol; Feed water; HPLC-MS; Nitrofurans; Nitroimidazoles