摘要： With the multiple biological activities and health benefit effects, polysaccharide in medicine and food dual purpose plants (MFDPPP) has been extensively applied in many fields, such as medical treatment, stock farming, and cosmetic industry. However, up to date, quality issues of MFDPPP and analytical technologies of polysaccharide post challenges to chemists. Reported herein is a rapid and high-throughput quality control method for analyzing MFDPPP, based on the matrix assisted laser desorption/ionization mass spectrometry (MALDI-MS). For the analysis of illegal addition and doping, ferroferric oxide nanoparticles was screened out as MALDI matrix to avoid the small molecule interference. Qualitatively, high sensitivity was obtained for both illegal drugs and glucose. Quantitatively, the best linear response (R2 > 0.99) was attained at the concentration range from 0.005 to 1 mg·mL-1 for glucose as an example. For the analysis of polysaccharides, 2,5-dihydroxybenzoic acid/N-methylaniline was employed as MALDI matrix to increase the detection sensitivity and mass range coverage. Furthermore, the established method was successfully applied to the analysis of supplements from Astragalus polysaccharides and Lentinan real samples, respectively, thus showing its potential in quality control for MFDPPP.