KMID : 0385520120250010025
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Analytical Science & Technology 2012 Volume.25 No. 1 p.25 ~ p.32
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Analysis of sorbic acid in tea-drink using isotope dilution liquid chromatography tandem mass spectrometry (ID-LC/MS/MS)
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Ahn Seong-Hee
Kim Byung-Joo Lee In-sun
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Abstract
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Isotope dilution mass spectrometry (ID-MS) based on liquid chromatography tandem mass spectrometry (LC/MS/MS) was developed for the accurate determination of sorbic acid in tea-drink. An isotope analogue of sorbic acid, 13C2-sorbic acid, was obtained by custom synthesis. MS was operated in the negative mode with selected reaction monitoring (SRM) mode of [M-H]- ¡æ [M-CO2H]- channel at m/z 111 ¡æ 67 for sorbic acid and at m/z 113 ¡æ 68 for its isotope analogue. Chromatographic separation was accomplished with a C18 column and an isocratic mobile phase of 55% of 50 mM ammonium acetate (pH 4.5) and 45% of methanol. Homogeneous reference materials were prepared for validation of this method, including repeatability and reproducibility tests, by fortifying tea-drink with sorbic acid in our laboratory. Repeatability and reproducibility studies showed that the ID-LC/MS method is a reliable and reproducible method which provides less than 3.8% of relative standard deviation (RSD) for the analysis of sorbic acid.
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KEYWORD
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sorbic acid, ID-LC/MS, reference materials, expanded uncertainty,
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