Journal
FOOD ADDITIVES AND CONTAMINANTS PART A-CHEMISTRY ANALYSIS CONTROL EXPOSURE & RISK ASSESSMENT
Volume 36, Issue 11, Pages 1616-1625Publisher
TAYLOR & FRANCIS LTD
DOI: 10.1080/19440049.2019.1658904
Keywords
Caffeine; direct analysis mass spectrometry; laser diode thermal desorption; energy drinks; quantitative analysis
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A rapid method for quantitative caffeine analysis in carbonated and non-carbonated beverages and liquid dietary supplement products was developed based on the direct sample introduction technique of laser diode thermal desorption atmospheric pressure chemical ionisation with tandem mass spectrometry (LDTD-MS/MS). Product samples were diluted with a mixture of methanol, water, and d(3)-caffeine internal standard. Sample aliquots were filtered, spotted on a metal-lined LDTD microtitre plate, dried, and thermally desorbed for subsequent ionisation and analysis by MS/MS analysis. Each sample required a 6 s desorption, and sample-to-sample analysis time of less than 30 s per sample. Caffeine yielded a linear calibration curve over the range 0.5-100 mu g mL(-1) (R-2 > 0.995). Caffeine recoveries from fortified samples ranged from 97% to 107% with <5% RSD. The caffeine determination was not affected by matrix interferences despite the large range of ingredients, vitamins, sweeteners, extracts, and additives present in the products tested, even though LDTD-MS/MS is a whole-sample desorption technique with no separation of matrix background. The method detection limit was below 0.12 mu g mL(-1). The method was applied to 33 caffeinated products and LDTD-MS/MS quantitative results closely correlated (R-2 > 0.998) with the regulatory standard HPLC-UV method (AOAC Official Method 979.08).
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