Journal
ANALYTICA CHIMICA ACTA
Volume 608, Issue 2, Pages 165-177Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.aca.2007.12.010
Keywords
liquid chromatography; time-of-flight mass spectrometry; synthetic preservative; screening; beverage
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In this study, liquid chromatography time-of-flight mass spectrometry (HPLC/TOF-MS) is applied to qualitation and quantitation of 18 synthetic preservatives in beverage. The identification by HPLC/TOF-MS is accomplished with the accurate mass (the subsequent generated empirical formula) of the protonated molecules [M + H]+ or the deprotonated molecules [M - H]-, along with the accurate mass of their main fragment ions. In order to obtain sufficient sensitivity for quantitation purposes (using the protonated or deprotonated molecule) and additional qualitative mass spectrum information provided by the fragments ions, segment program of fragmentor voltages is designed in positive and negative ion mode, respectively. Accurate mass measurements are highly useful in the complex sample analyses since they allow us to achieve a high degree of specificity, often needed when other interferents are present in the matrix. The mass accuracy typically obtained is routinely better than 3 ppm. The 18 compounds behave linearly in the 0.005-5.0 mg center dot kg(-1) concentration range, with correlation coefficient > 0.996. The recoveries at the tested concentrations of 1.0 mg center dot kg(-1)-100 mg center dot kg(-1) are 81-106%, with coefficients of variation < 7.5%. Limits of detection (LODs) range from 0.0005 to 0.05 mg center dot kg(-1), which are far below the required maximum residue level (MRL) for these preservatives in foodstuff. The method is suitable for routine quantitative and qualitative analyses of synthetic preservatives in foodstuff. (c) 2007 Elsevier B.V. All rights reserved.
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