Switchable-hydrophilicity solvent liquid-liquid microextraction versus dispersive liquid-liquid microextraction prior to HPLC-UV for the determination and isolation of piperine from Piper nigrum L

J Sep Sci. 2020 Aug;43(15):3053-3060. doi: 10.1002/jssc.202000152. Epub 2020 Jun 4.

Abstract

Switchable-hydrophilicity solvent liquid-liquid microextraction and dispersive liquid-liquid microextraction were compared for the extraction of piperine from Piper nigrum L. prior to its analysis by using high-performance liquid chromatography with UV detection. Under optimum conditions, limits of detection and quantitation were found as 0.2-0.6 and 0.7-2.0 μg/mg with the two methods, respectively. Calibration graphs showed good linearity with coefficients of determination (R2 ) higher than 0.9962 and percentage relative standard deviations lower than 6.8%. Both methods were efficiently used for the extraction of piperine from black and white pepper samples from different origins and percentage relative recoveries ranged between 90.0 and 106.0%. The results showed that switchable-hydrophilicity solvent liquid-liquid microextraction is a better alternative to dispersive liquid-liquid microextraction for the routine analysis of piperine in food samples. A novel scaled-up dispersive liquid-liquid microextraction method was also proposed for the isolation of piperine providing a yield of 102.9 ± 4.9% and purity higher than 98.0% as revealed by NMR spectroscopy.

Keywords: black pepper; dispersive liquid-liquid microextraction; piperine; switchable-hydrophilicity solvent; white pepper.

MeSH terms

  • Alkaloids / analysis*
  • Benzodioxoles / analysis*
  • Chromatography, High Pressure Liquid
  • Cyclohexylamines / chemistry*
  • Ethylamines / chemistry*
  • Food Contamination / analysis*
  • Hydrophobic and Hydrophilic Interactions
  • Liquid Phase Microextraction*
  • Piper nigrum / chemistry*
  • Piperidines / analysis*
  • Polyunsaturated Alkamides / analysis*
  • Solvents / chemistry
  • Spectrophotometry, Ultraviolet
  • Ultraviolet Rays

Substances

  • Alkaloids
  • Benzodioxoles
  • Cyclohexylamines
  • Ethylamines
  • Piperidines
  • Polyunsaturated Alkamides
  • Solvents
  • piperine
  • triethylamine

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