RAPID ANALYSIS OF MELAMINE IN POWDERED MILK USING SPECIFIC SOLID PHASE EXTRACTION FOLLOWED BY ULTRAHIGH PERFORMANCE LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY


TÜRKÖZ BAKIRCI G., Yaman-Acay D. B., Karakaya S.

FRESENIUS ENVIRONMENTAL BULLETIN, vol.28, pp.1281-1286, 2019 (SCI-Expanded) identifier

  • Publication Type: Article / Article
  • Volume: 28
  • Publication Date: 2019
  • Journal Name: FRESENIUS ENVIRONMENTAL BULLETIN
  • Journal Indexes: Science Citation Index Expanded (SCI-EXPANDED)
  • Page Numbers: pp.1281-1286
  • Keywords: Melamine, solid phase extraction, powdered milk, UPLC/MS/MS
  • Dokuz Eylül University Affiliated: Yes

Abstract

An extraction and analytical method for the determination of melamine in powdered milk using ultrahigh performance liquid chromatography coupled to tandem mass spectrometry (UPLC/MS/MS) has been developed. In the method, the melamine was extracted using a perchloric acid (HCLO4), clean up sample supernatant using Oasis (R) MCX cartridge (3 cc 60 mg, P/N 186000254), and the final extract was analyzed in a single injection by UPLC/MS/MS. Limit of quantification (LOQ) value of melamine was found to be lower than the maximum residue limits (MRL). Matrix-matched calibration curves were applied and correlation coefficients (R-2) was greater than 0.99. The recovery values were found to be between 70 and 100% with relative standard deviations less than 20%. Based on these results, the proposed method is suitable for the routine determination of the concentration of melamine in powdered milk.