Dispersive liquid-liquid microextraction coupled to liquid chromatography tandem mass spectrometry for the determination of phenolic compounds in human milk

Food Chem. 2020 Oct 15:327:126996. doi: 10.1016/j.foodchem.2020.126996. Epub 2020 May 6.


This work describes a novel approach for the analysis of 11 phenolic compounds (naringenin, hesperetin, kaempferol, quercetin, epicatechin, epicatechin gallate, epigallocatechin gallate, genistein, daidzein, caffeic acid, gallic acid) in human milk. Clean-up of the sample and extraction of 11 analytes from milk was performed by dispersive liquid-liquid microextraction (DLLME). Under the optimal conditions, the extraction recoveries of 11 analytes were in a range from 94.3% to 108%. For determination of phenolic compounds in extracts, LC-ESI-MS/MS method was used. The calibration curves showed linearity in the concentration ranges from 0.01 to 1500 ng mL-1 and the limits of detection were in a range from 0.18 ng L-1 to 74 ng mL-1. The repeatability and intermediate precision expressed as the relative standard deviations were below 7.6% and 9.9%, respectively. The DLLME-LC-ESI-MS/MS method was successfully applied to the determination of phenolic compounds present in breast milk.

Keywords: Caffeic acid (PubChem CID: 689043); Daidzein (PubChem CID: 5281708); Dispersive liquid–liquid microextraction; Epicatechin (PubChem CID: 72276); Epicatechin gallate (PubChem CID: 107905); Epigallocatechin gallate (PubChem CID: 65064); Gallic acid (PubChem CID: 370); Genistein (PubChem CID: 5280961); Hesperetin (PubChem CID: 72281); Human milk; Kaempferol (PubChem CID: 5280863); LC-ESI-MS/MS; Naringenin (PubChem CID: 932); Phenolic compounds; Quercetin (PubChem CID: 5280343).

MeSH terms

  • Calibration
  • Chromatography, Liquid / methods*
  • Female
  • Food Analysis / methods
  • Humans
  • Liquid Phase Microextraction / methods*
  • Milk, Human / chemistry*
  • Phenols / analysis*
  • Poland
  • Tandem Mass Spectrometry / methods*


  • Phenols