TL;DR: The trueness of the HPLC-ELSD method was satisfactory with recoveries ranging from 93 to 109% for concentration levels around the maximum usable dosages for authorised sweeteners and from 100 to 112% for unauthorised compounds at concentration levels close to the limit of quantification (LOQs).
TL;DR: The proposed method has been successfully applied to the determination of the nine high-intensity sweeteners in drinks, yoghurts and fish products and is suitable for routine quality control analysis of foodstuffs.
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.
TL;DR: The results indicate that the synthetic sweetening agents, saccharin, sodium cyclohexyl sulfamate, dulcin, and P-4000 may be divided into a toxic group and a relatively nontoxic group.
Abstract: Data are given on the chronic oral toxicities of the synthetic sweetening agents, saccharin, sodium cyclohexyl sulfamate, dulcin, and P-4000. The results indicate that these four substances may be divided into a toxic group and a relatively nontoxic group. Dulcin and p-4000 were toxic to rats at dosage levels of 0.1 per cent and above, whereas saccharin and sodium cyclohexyl sulfamate had only slight effects at a dosage level of 5 per cent.
TL;DR: In pigs, the gustatory preferences in pigs towards 33 compounds known to be sweet in humans were evaluated through a specific two-choice preference method as discussed by the authors, and all the 14 carbohydrates tested are preferred over water, sucrose being the most effective.
TL;DR: The levels of artificial sweeteners, preservatives and caffeine were in good agreement with those determined by the high-performance liquid chromatographic (HPLC) procedure currently used in the Laboratory.