Separation and determination of seven fluoroquinolones by pressurized capillary electrochromatography

• Published in: Journal of separation science Vol. 28; no. 16; pp. 2210 - 2217
• Main Authors: Lü, Haixia, Wu, Xiaoping, Xie, Zenghong, Lin, Xucong, Guo, Liangqia, Yan, Chao, Chen, Guonan
• Format: Journal Article
• Language: English
• Published: Weinheim WILEY-VCH Verlag 01.11.2005; WILEY‐VCH Verlag; Wiley
• Subjects: Animals; Biological and medical sciences; Buffers; Chromatography; Ciprofloxacin; Electrochemistry; Enoxacin; Ethylamines; Fish and seafood industries; Fishes - metabolism; Fleroxacin; Fluoroquinolones - analysis; Fluoroquinolones - isolation & purification; Fluoroquinolones - metabolism; Food industries; Fundamental and applied biological sciences. Psychology; Gatifloxacin; Hydrogen-Ion Concentration; Lomefloxacin; Muscle, Skeletal - metabolism; Norfloxacin; Ofloxacin; Pressurized capillary electrochromatography (pCEC); Sensitivity and Specificity; Sodium Dodecyl Sulfate; Fleroxacin; Chemical analysis; Enoxacin; Fleroxacin; Lomefloxacin; Enoxacin; Pressurized capillary electrochromatography (pCEC); Fish fillet; Veterinary medicine; Norfloxacin; Ofloxacin; Contamination; Operating conditions; Fluoroquinolone derivatives; Ultraviolet detector; Pressure effect; Gatifloxacin; Residue; Electrochromatography; Gatifloxacin; Lomefloxacin; Norfloxacin; Ofloxacin; Antibacterial agent; Ciprofloxacin; Quinolone derivatives; Quantitative analysis
• ISSN: 1615-9306; 1615-9314
• DOI: 10.1002/jssc.200500175

In this paper, pressurized CEC was used for the separation and determination of seven fluoroquinolones (FQs). The effect of different experimental conditions, such as the concentration and pH of the buffer, the organic modifier concentration, the surfactant and ion‐paring agents added to the electrolyte, and applied voltage were studied. All the seven FQs were baseline separated using mobile phase containing 27% v/v ACN, 5 mmol/L Na2HPO4 buffer (pH 4.0 adjusted using citric acid), 11 mmol/L SDS, and 0.01% TEA v/v at detection wavelength of 287 nm and at an applied voltage of –10 kV. The calibration curves were linear (r >0.9991) over a concentration range of 1.0–50.0 mg/L for norfloxacin (NFLX); 2.5–50.0 mg/L for fleroxacin (FLX), ciprofloxacin (CPFX), and lomefloxacin (LMX); and 5.0–50.0 mg/L for enoxacin (ENX), ofloxacin (OFLX), and gatifloxacin (GFLX). The detection limits (S/N = 3) for ENX, OFLX, FLX, NFLX, CPFX, LMX, and GFLX were 0.5, 0.8, 0.4, 0.2, 0.4, 0.5, and 1.0 mg/L, respectively. The method is simple, rapid, and reproducible. It was successfully applied to the analysis of fish muscle samples spiked with FQs. Mean recoveries ranged from 81.6 to 97.6%.