Switchable-hydrophilicity solvent liquid-liquid microextraction of non-steroidal anti-inflammatory drugs from biological fluids prior to HPLC-DAD determination

J Pharm Biomed Anal. 2019 Sep 10:174:509-517. doi: 10.1016/j.jpba.2019.06.023. Epub 2019 Jun 20.

Abstract

Switchable-hydrophilicity solvent liquid-liquid microextraction was used prior to high-performance liquid chromatography with diode-array detector (HPLC-DAD) for the determination of four non-steroidal anti-inflammatory drugs [i.e., ketoprofen, etodolac, flurbiprofen and ibuprofen] in human urine, saliva and milk. Optimum extraction conditions were as follows: 500 μL switched-on N,N-dimethylcyclohexylamine as the extraction solvent, 9.5 mL of the aqueous phase, 500 μL 20 M sodium hydroxide as a switching-off trigger, and within 30 s extraction time. A portion of the final extract was directly injected into HPLC. Under optimized extraction and chromatographic conditions, limits of detection ranged between 0.04 and 0.18 μg mL-1 in all matrices analyzed. Good linearity with coefficients of determination (R2) ranging between 0.9955 and 0.9998, and percentage relative standard deviations (%RSD) of 0.9-7.7% were obtained. The proposed method was efficiently used for the extraction of the analytes in the biological fluids with percentage relative recoveries (%RR) ranging between 95.7 and 109.2%.

Keywords: Biological fluids; Liquid–liquid microextraction; Non-steroidal anti-inflammatory drugs; Switchable-hydrophilicity solvent.

MeSH terms

  • Anti-Inflammatory Agents, Non-Steroidal / analysis*
  • Anti-Inflammatory Agents, Non-Steroidal / urine*
  • Centrifugation
  • Chromatography, High Pressure Liquid*
  • Etodolac / urine
  • Flurbiprofen / urine
  • Humans
  • Hydrophobic and Hydrophilic Interactions
  • Ibuprofen / urine
  • Ketoprofen / urine
  • Linear Models
  • Liquid Phase Microextraction*
  • Milk, Human / chemistry*
  • Organic Chemicals
  • Reproducibility of Results
  • Saliva / chemistry*
  • Sodium Hydroxide / chemistry
  • Solvents / chemistry

Substances

  • Anti-Inflammatory Agents, Non-Steroidal
  • Organic Chemicals
  • Solvents
  • Etodolac
  • Sodium Hydroxide
  • Flurbiprofen
  • Ketoprofen
  • Ibuprofen