Determination of Illegally Added Sodium Picosulfate in Internet-famous Weight-loss Foods by Salting-out Assisted and Pass-through Cleanup SPE-UHPLC-MS/MS
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Abstract:
An ultra high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS) method was developed for the determination of illegally added sodium picosulfate in the internet-famous weight-loss foods. The samples were extracted by a salting-out assisted methanol-water solution system, and purified by an Oasis PRiME HLB solid phase extraction column with a pass-through cleanup strategy. The separation was carried out on a C18 column using acetonitrile ammonium acetate as the mobile phase in a gradient elution mode. Eletrospray ionization source with positive ion (ESI+) ionization mode, multiple reaction monitoring (MRM) scanning and external standard quantification method were used. In this study, the extraction system was optimized to achieve good dispersion of different matrix samples and good anti interference effect. The established method showed a linear relationship in the picosulfate concentration range of 0.50~250.00 ng/mL, with the correlation coefficients higher than 0.998, and the limit of detection (LOD) and the limit of quantitation (LOQ) being 10.00 μg/kg and 25.00 μg/kg, respectively. At low (25.00 μg/kg), medium (50.00 μg/kg) and high (250.00 μg/kg) concentrations, the average recoveries ranged from 81.51% to 104.53%, with the relative standard deviation (RSD) ranging from 1.14% to 5.64%. This method is somple, efficient and accurate with strong anti-interference, thus is suitable for the qualitative and quantitative analyses of sodium picosulfate illegally added to weight-loss foods.
