Fabric phase sorptive extraction-high performance liquid chromatography-photo diode array detection method for simultaneous monitoring of three inflammatory bowel disease treatment drugs in whole blood, plasma and urine

J Chromatogr B Analyt Technol Biomed Life Sci. 2018 May 1;1084:53-63. doi: 10.1016/j.jchromb.2018.03.028. Epub 2018 Mar 16.


This paper reports a novel fabric phase sorptive extraction-high performance liquid chromatography-photodiode array detection (FPSE-HPLC-PDA) method for the simultaneous extraction and analysis of three drug residues (ciprofloxacin, sulfasalazine, and cortisone) in human whole blood, plasma, and urine samples, generally administered in human patients to treat inflammatory bowel disease (IBD). The drugs of interest were well resolved using a Luna C18 column (250 mm × 4.6 mm; 5 μm particle size) in gradient elution mode within 20 min. The analytical method was optimized and validated in the range 0.05-10 μg/mL for whole blood, 0.25-10 μg/mL for human plasma, and 0.10-10 μg/mL for human urine. Blank human whole blood, plasma, and urine were used as the sample matrix for the method development and validation; while methyl-p-hydroxybenzoate was used as the internal standard (IS). Weighted-matrix matched standard calibration curves showed a good linearity up to a concentration of 10 μg/mL. The intra- and inter-day accuracy values (precision and trueness) were found in the range from -10.9% to 12.3%, and the performances of the validated FPSE-HPLC-PDA were further tested on real IBD patient samples. This is the first FPSE procedure applied simultaneously to whole blood, plasma, and urine samples for the determination of residual IBD drugs, which possess a wide range of polarity (logP values ranging from 2.30 for Ciprofloxacin, to 1.66 for Cortisone, and 2.92 for Sulfasalazine). The new approach exhibits high potential for immediate adoptation as a rapid, robust and green analytical tool for future clinical and pharmaceutical applications.

Keywords: FPSE-HPLC-PDA; Inflammatory bowel disease; Method validation; Sample preparation; Whole blood, plasma and urine.

MeSH terms

  • Adsorption
  • Chromatography, High Pressure Liquid / methods*
  • Female
  • Gastrointestinal Agents / analysis*
  • Gastrointestinal Agents / therapeutic use
  • Humans
  • Inflammatory Bowel Diseases / drug therapy*
  • Limit of Detection
  • Linear Models
  • Liquid-Liquid Extraction
  • Male
  • Middle Aged
  • Reproducibility of Results


  • Gastrointestinal Agents