Artificial sweeteners in beverages by ultra performance liquid chromatography with photodiode array and liquid chromatography tandem mass spectrometry

- UPLC-PDA and LC-MS/MS were validated to determine artificial sweeteners.
- Minimal sample preparation is required.
- Successful application to analyse sugar-free beverages consumed in Spain.
- Methodologies are suitable in quality control and food safety.

Two fast, accurate and sensitive liquid chromatography methods have been developed and optimized for a better control of the content of artificial sweeteners in industrial beverages. Ultra performance liquid chromatography coupled with photodiode array (UPLC-PDA) and liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) methods were implemented for the monitoring of aspartame, neohesperidine dihydrochalcone, neotame, potassium acesulfame, saccharin, sodium cyclamate and sucralose in beverages marketed as “sugar-free” or “diet,” including soft and powdered drinks. Minimal sample preparation procedure consisting on a simple dilution and filtration is required before analysis. The methods showed excellent linearity (R2 < 0.9990) for target compounds. Limits of quantification (LOQs) were far below the legal requirements for all considered compounds (0.01-0.1 μg mL−1 and 0.05-5 ng mL−1 for UPLC-PDA and LC-MS/MS, respectively). Precision and recovery studies in real samples showed excellent results. The recoveries at two concentration levels ranged between 90.0 and 114.6%, with relative standard deviations lower than 9.4 RSD%. Finally, the proposed methodology was successfully applied to the analysis of artificial sweeteners in 66 beverage products commonly consumed in Spain. Different sample categories were evaluated, including energy drinks, soft drinks, juices, teas, soy beverages, dairy-based drinks, beers, and spirit alcoholic drink, and proved its suitability for quick and reliable application in quality control laboratories.