Determination of nine high-intensity sweeteners in various foods by high-performance liquid chromatography with mass spectrometric detection |
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Authors: | Agata Zygler Andrzej Wasik Agata Kot-Wasik Jacek Namieśnik |
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Institution: | (1) Department of Analytical Chemistry, Chemical Faculty, Gdańsk University of Technology, ul. G. Narutowicza 11/12, 80–233 Gdańsk, Poland; |
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Abstract: | An analytical procedure involving solid-phase extraction (SPE) and high-performance liquid chromatography-mass spectrometry
has been developed for the determination of nine high-intensity sweeteners authorised in the EU; acesulfame-K (ACS-K), aspartame
(ASP), alitame (ALI), cyclamate (CYC), dulcin (DUL), neohesperidin dihydrochalcone (NHDC), neotame (NEO), saccharin (SAC)
and sucralose (SCL) in a variety of food samples (i.e. beverages, dairy and fish products). After extraction with a buffer
composed of formic acid and N,N-diisopropylethylamine at pH 4.5 in ultrasonic bath, extracts were cleaned up using Strata-X 33 μm Polymeric SPE column. The
analytes were separated in gradient elution mode on C18 column and detected by mass spectrometer working with an electrospray source in negative ion mode. To confirm that analytical
method is suitable for its intended use, several validation parameters, such as linearity, limits of detection and quantification,
trueness and repeatibilty were evaluated. Calibration curves were linear within a studied range of concentrations (r
2
≥ 0.999) for six investigated sweeteners (CYC, ASP, ALI, DUL, NHDC, NEO). Three compounds (ACS-K, SAC, SCL) gave non-linear
response in the investigated concentration range. The method detection limits (corresponding to signal-to-noise (S/N) ratio
of 3) were below 0.25 μg mL−1 (μg g−1), whereas the method quantitation limits (corresponding to S/N ratio of 10) were below 2.5 μg mL−1 (μg g−1). The recoveries at the tested concentrations (50%, 100% and 125% of maximum usable dose) for all sweeteners were in the
range of 84.2 ÷ 106.7%, with relative standard deviations <10% regardless of the type of sample matrix (i.e. beverage, yoghurt,
fish product) and the spiking level. The proposed method has been successfully applied to the determination of the nine sweeteners
in drinks, yoghurts and fish products. The procedure described here is simple, accurate and precise and is suitable for routine
quality control analysis of foodstuffs. |
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