Simultaneous Determination of Active Components and Anti-diabetic Drugs in Propolis Health Foods by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry / 分析化学

ABSTRACT

A comprehensive analytical method based on ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was developed for the simultaneous determination of active components and anti-diabetic) drugs in propolis health foods. The samples were extracted by ultrasound extraction with methanol). The insoluble residue of extract was removed by freeze-centrifuging. The analysis was performed on an ACQUITY UPLC C_(18)) column(50 mm ×1 mm, i.d., 1.7 μm) utilizing a gradient elution profile and a mobile phase of 0.3% formic acid in water and acetonitrile. The analytes were detected using an electro spray ionization tandem mass spectrometry with multiple reaction monitoring. Qualitative and quantitative analysis was based on the peak area of the parent ion and two fragment ions. The LOD and LOQ level for 14 active components ranged from 0.7 mg/kg to 42.0 mg/kg and 2.2 mg/kg to 140 mg/kg respectively, and recoveries were 77.8%-113.6%, with the intra- and inter-day precision less than 15%. The LOD and LOQ level for 9 anti-diabetics) ranged from 0.1 mg/kg to 0.9 mg/kg and 0.3 mg/kg to 2.5 mg/kg respectively, and recoveries) were 79.3%-108.5%, with the intra- and inter-day precision less than 15%. The method is simple) and sensitive, and can be used for quality control of propolis.