Chip High Performance Liquid Chromatography Time Of Flight Mass Spectrometry System Performance Evaluation And Small Drug Molecules

The paper set up the method of small molecule pharmaceutical analysis such as theophylline and caffeine with Nano LC-Chip/Q-TOF MS system. The system use a chip with a 500nL enrichment column instead of the traditional column. The flow rate of nanopump is 0.3μL/min, and capillarypump is 4μL/min. Compared with few thousthands plate numbers of traditional column, the chip is 14400. The system has a good stability, reproducibility and linearity. The RT RSD is less than 0.32%, PA RSD less than 6.71%. The LOD of small molecule pharmaceutical is few picograms per microlitre, which is three orders of magnitude lower than traditional HPLC.Set up the method of pfizer drugs analysis, obtained the best results under the conditions of 1μL injection volumn, 4μL injection flush volumn and chip valve model. The paper also tested the changes of detection results affected by different sample solutions. The LOD of active pharmaceutical ingredient of pfizer drugs is 0.1pg/μL, RT RSD less than 0.55%, PA RSD less than 7.27%, the dynamic range of linearity is between 10~2 and 10~3 . Detected an active pharmaceutical ingredient at about 1% level, but the API which has a similar retention time with Zipra is difficult ot detected because of the competition of ionization.Preliminary research of complex biological samples analysis with Nano LC-Chip/Q-TOF MS system, optimized the sepration conditions. Qualitative analized the target component in plasma with standard sample, MS spectrams and MS/MS spectrams.