1 / 26

液相層析質譜分析 LC-MS Method development and Analyte Identification

液相層析質譜分析 LC-MS Method development and Analyte Identification. 授課教師：賴滄海教授 03-12-2008. Ionization. ESI Sonic Spray I APCI APPI APLI. Ion Separation. Mass range Scan speed Mass resolution Mass accuracy. Mass Accuracy.

cana
Download Presentation

液相層析質譜分析 LC-MS Method development and Analyte Identification

An Image/Link below is provided (as is) to download presentation Download Policy: Content on the Website is provided to you AS IS for your information and personal use and may not be sold / licensed / shared on other websites without getting consent from its author. Content is provided to you AS IS for your information and personal use only. Download presentation by click this link. While downloading, if for some reason you are not able to download a presentation, the publisher may have deleted the file from their server. During download, if you can't get a presentation, the file might be deleted by the publisher.

E N D

Presentation Transcript

  1. 液相層析質譜分析LC-MS Method development and Analyte Identification 授課教師：賴滄海教授 03-12-2008

  2. Ionization • ESI • Sonic Spray I • APCI • APPI • APLI

  3. Ion Separation • Mass range • Scan speed • Mass resolution • Mass accuracy

  4. Mass Accuracy An unknown compound appears at m/z 180.094. in the positive ion mode. The mass accuracy of the spectrometer is 2-5 ppm.

  5. Assuming it contains C.H.O.N.P.S. F.Cl.Br

  6. Mass Analyzer • Quadrupole • Ion trap • Linear ion Trap • Time of flight

  7. Steps in the quantification of drugs • Sampling • Sample preparation • Separation • Detection • Data analysis

  8. General Considerations • What to measure ( drug/metabolites) • Select matrix (blood,serum,plasma,tissue) • Sample limitations (volume,sample size) • Linear range • Lower limit of quantification • Internal standard

  9. Problems with Deuterated Is [13C,D3] rofecoxib exchange with Hydrogen atoms on water molecular [J Chromatogr B 2002;767:117-129]

  10. Positive identification with GC-MS(SIM) • 3 ions • Retention time the same as standards • Ion ratio correct • S/N > 3 • Sample processed to remove interferences

  11. Aspects to be considered when setting up LC-MS procedures • Influence of the mobile phase • Influence of sodium and potassium on the formation of adducts • Influence of the curtain gas flow • Reproducibility of mass spectra • Influence of ion suppression • GC-MS data to verify LC-MS results

  12. Mass spectrometry • Ionization • Matrix effect • Full scan • MRM

  13. Figure 2.5 The influence of collision energy on the fragmentation of tacrolimus at (a)10, (b)20,(c)30,(d)40 and (e)50eV.

  14. Sample preparation • Sample dilution and protein precipitation • Liquid-liquid extraction • Solid phase extraction • Two dimensional chromatography (column switching)

More Related