基于液相色谱-高分辨质谱的天然香原料非靶向分析OA

To develop a non-targeted analytical method based on liquid chromatography-high resolution mass spectrometry(LC-HRMS)for natural flavors,the effects of sample pretreatment method and chromatography-MS conditions on the detection were systematically investigated,and the detection results of the non-targeted analytical method was further evaluated.The results showed that:1)A ternary solvent combination of Vmethanol∶Vacetonitrile∶Vwater=35∶35∶30 combined with 20 min ultrasound treatment could achieve better extraction results,and the operation was convenient.2)The single-stage gradient elution was performed on the complementary C18 and Amide chromatographic columns,in which 0.1%(volume fraction)formic acid was added to the mobile phase of the C18 column,and 0.1%formic acid and 5 mmol/L ammonium acetate were added to the mobile phase of the Amide column.The effects of injection volume and column temperature were not obvious,which were set at 2 µL and 30℃,respectively.3)The optimized MS conditions were separate scans for positive and negative ion modes,full MS scans in the range of m/z 70-1 050 with a resolution of 60 000,and the normalized collision energies of 20%,40%and 60%,respectively.4)All the total ion chromatograms obtained from the multi-needle injection under the"dual-column dual-mode"detection conditions showed good overlap,and the complementary combination of the reversed-phase and hydrophilic interaction modes of the two columns as well as the synergistic positive and negative ion detection modes could effectively improve the coverage of compound identification.The developed non-targeted analysis method based on the"dual-column dual-mode"for natural flavors showed high detection throughput and good stability,and is suitable for quality control and compositional analysis of complex natural flavors.