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http://dx.doi.org/10.5806/AST.2012.25.1.025

Analysis of sorbic acid in tea-drink using isotope dilution liquid chromatography tandem mass spectrometry (ID-LC/MS/MS)  

Ahn, Seong-Hee (Division of Metrology for Quality Life, Korea Research Institute of Standards and Science)
Lee, In-Sun (Dong-il SHIMAZU Corp. R&D center)
Kim, Byung-Joo (Division of Metrology for Quality Life, Korea Research Institute of Standards and Science)
Publication Information
Analytical Science and Technology / v.25, no.1, 2012 , pp. 25-32 More about this Journal
Abstract
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, $^{13}C_2$-sorbic acid, was obtained by custom synthesis. MS was operated in the negative mode with selected reaction monitoring (SRM) mode of $[M-H]^-$ ${\rightarrow}$ $[M-CO_2H]^-$ channel at m/z 111 ${\rightarrow}$ 67 for sorbic acid and at m/z 113 ${\rightarrow}$ 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.
Keywords
sorbic acid; ID-LC/MS; reference materials; expanded uncertainty;
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