engleski

Determination of cyanuric acid in whey powder using HILIC-MS/MS

A hydrophilic liquid chromatography-tandem mass spectrometry method was developed for determination of cyanuric acid in whey powder samples in the mass fraction range from 1.00 to 10.00 mg kg-1. The cyanuric acid was extracted from whey powder with an acetonitrile:water (60:40, v/v) extraction solution. Separation was performed on a XBridge Amide column 3.5µm using acetonitrile:water (90:10, v/v) as the mobile phase at a flow rate of 0.2 mL min. Detection was achieved by triple quadrupole mass spectrometry using heated electrospray ionization interface. The analysis was performed in the negative ionization mode using the SRM transitions combinations of m/z 128→ 42 and m/z 128→ 85 for quantitative and qualitative detection of cyanuric acid, respectively and m/z 134→ 44 and m/z 134→ 89 for isotope-labelled cyanuric acid (13C3, 15N3 – CYA) detection, used to correct for matrix effects. The developed and optimized method was validated by determing following validation parameters: selectivity, linearity, precision, recovery (accuracy), limits of detection and quantification and stability of cyanuric acid in whey powder extract. The recoveries of cyanuric acid from whey powder fortified at 1.00, 2.50 and 7.00 mg kg-1 were within the 100.9-112.2% range, intra-day precision was ≤ 6.45% and inter-day precision was ≤ 9.13%. The limit of detection and quantification was 0.30 mg kg-1 and 1.00 mg kg-1 respectively. The suitabilityof the developed method for use in routine determination was confirmed through analysis of whey powder samples from dairy industry and supermarkets.

cyanuric acid ; whey powder ; hydrophilic interaction liquid chromatography ; tandem mass spectrometry

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