Фармацевтика Аналитика Акта

Абстрактный

Simultaneous Determination of Paracetamol, Propyphenazone, Aspirin and Caffeine in White Wine Samples by Liquid Chromatography-Triple Quadrupole Tandem Mass Spectrometry

Dan Han, Yongliang Ding, Kun Peng, Bobing Tang, Cunxian Xi, Anping Deng

A highly sensitive Liquid Chromatography-Triple Quadrupole Tandem Mass Spectrometry (LC-MS/MS) for simultaneous determination of analgesic-antipyretics drugs, e.g. Paracetamol (PC), Propyphenazone (PZ), Aspirin (AS) and Caffeine (CF), in white wine samples was presented. The chromatographic separation was carried out on a narrow C18 column by a gradient elution using Acetonitrile (A) and 10 mM ammonium acetate with 0.1% formic acid (B) as the solvents at a flow rate of 0.3 ml/min. Qualitative and quantitative analysis of PC, PZ and CF were achieved by Multiple Reaction Monitoring (MRM) in positive mode, while the analysis of AS was completed by MRM in negative mode. Under optimal conditions, good linearity with high correlation coefficient (>0.9981) were obtained between 0.05-50 ng mL^-1 for PC, 0.005-20 g mL^-1 for PZ, 0.3-200 g mL^-1 for AS, and 1.0-50 g mL^-1 for CF. The Limit Of Detection (LOD) values of the method for PC, PZ, AS and CF were found to be 0.015, 0.0015, 0.08 and 0.25 g mL^-1, respectively. Spiking experiments revealed good recoveries in range of 87.6~111.0% with Relative Standard Deviations (RSD) of 2.1~9.4%. Total 1006 white wine samples were collected and analysed by the proposed method. PC was found in three inferior white wines samples, and the residual levels of PC, PZ, AS and CF in other samples were undetectable. It was demonstrated that the proposed LC–MS/MS is a powerful analytical tool for sensitive determination of PC, PZ, AS and CF in white wine samples.