Method development for the quantitative determination of lactulose in heat-treated milks by HPAEC with pulsed amperometric detection

Anal Chem. 1999 Nov 1;71(21):4919-25. doi: 10.1021/ac990493u.

Abstract

A robust, rapid, and sensitive high-performance anion-exchange chromatographic method for the separation and quantitative determination of lactulose in heated milks, along with other common milk carbohydrates, has been developed. Complete separation of galactose, glucose, N-acetylgalactosamine, lactose, lactulose, and epilactose was isocratically accomplished in about 22 min by an anion-exchange column eluted with 10 mM NaOH spiked with 2 mM Ba(OAc)2. The within-day repeatability was lower than 2.1% for 10 repetitive injections. Under optimized conditions, there was no need either of post-column addition of strong bases to the eluent for enhancing detection sensitivity or, even more important, for column regeneration between chromatographic runs. Upon 100-fold sample dilution, the amperometric response of lactulose in milk samples was found to be linear up to 100 microM (r = 0.99935) with a limit of detection equal to 1.2 microM (S/N = 3). The lactulose content in ultrahigh-temperature (UHT) and sterilized milks was evaluated by a calibration graph using 2-deoxyglucose as the internal standard, making the proposed method very useful in discriminating among heat-treated milks. Whereas the mean value of lactulose in skimmed, partially skimmed, and whole UHT milks ranged from 10 to 90 mg/100 mL, lactulose content in bottle-sterilized whole milk (two samples) was higher than 140 mg/100 mL. The presence of epilactose, which is another isomer of lactose, was also ascertained in sterilized milk.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Animals
  • Barium Compounds / chemistry
  • Carbohydrates / analysis
  • Chromatography, Ion Exchange / methods*
  • Electrochemistry / methods*
  • Hot Temperature
  • Lactose / chemistry
  • Lactose / metabolism
  • Lactulose / analysis*
  • Milk / chemistry*
  • Reproducibility of Results
  • Sensitivity and Specificity
  • Sterilization

Substances

  • Barium Compounds
  • Carbohydrates
  • Lactulose
  • Lactose