Detection and confirmation of milk adulteration with cheese whey using proteomic-like sample preparation and liquid chromatography-electrospray-tandem mass spectrometry analysis

Talanta. 2014 Mar:120:498-505. doi: 10.1016/j.talanta.2013.11.093. Epub 2013 Dec 11.

Abstract

Caseinomacropeptide (CMP) is a peptide released by chymosin in cheese production, remaining in whey. Thus, CMP can be used as a biomarker to fluid milk adulteration through whey addition. Commonly, CMP is analyzed by reversed phase (RP-HPLC) or size-exclusion chromatography (SEC). However, some psychrotropic microorganisms - specially Pseudomonas fluorescens - when present in storaged milk, can produce, by enzymatic pathway, a CMP-like peptide generally called pseudo-CMP. These two peptides differ from each other only by one amino acid. RP-HPLC and SEC methods are unable to distinguish these two peptides, which demand development of a confirmatory method with high selectivity. Considering the several degrees of glycosilation and phosphorylation sites in CMP, allied with possible genetic variation (CMP A and CMP B), analytical methods able to differentiate these peptides are extremely complex. In the present work, we developed a proteomic-like technique for separation and characterization of these peptides, using liquid chromatography coupled to mass spectrometry with electrospray ionization able to differentiate and subsequently quantify CMP and pseudo-CMP in milk samples in order to identify adulteration or contamination of these products. The method shows satisfactory precision (<11%) with a detection limit of 1.0 µg mL(-1) and quantification limit of 5.0 µg mL(-1). Specificity, matrix effects and applicability to real samples analysis were also performed and discussed.

Keywords: Caseinomacropeptide; Food adulteration; Mass spectrometry; Milk proteins; Pepsin digestion.

Publication types

  • Evaluation Study
  • Research Support, Non-U.S. Gov't

MeSH terms

  • Animals
  • Caseins / analysis*
  • Cheese / analysis
  • Chromatography, High Pressure Liquid / methods
  • Food Analysis / methods*
  • Food Quality
  • Limit of Detection
  • Milk / chemistry*
  • Peptide Fragments / analysis*
  • Proteomics
  • Spectrometry, Mass, Electrospray Ionization / methods*
  • Tandem Mass Spectrometry / methods

Substances

  • Caseins
  • Peptide Fragments
  • caseinomacropeptide