Objective

To perform a MALDI MS analysis of the Ugi product 62E.

Procedure


Instrumentation: All spectra were collected on a Bruker Reflex III MALDI TOFMS operating in reflectron mode. All spectra were collected using the same set of instrument parameters.

Materials:
PEG 400 calibration standard: 7.36mg/ml in MeOH
CHCA matrix: 0.1M stock solution in MeOH
Dithranol matrix: 0.1M stock solution in THF
LiTFA cationization reagent: 0.0024M stock solution in MeOH
Analyte (Ugi product): 1.15mg/ml = 0.023M stock concentration in MeOH

Methods: The MALDI sample was prepared by adding 10ul of the analyte solution to 100ul of the matrix solution in a small glass sample vial; the solution was mixed by vortexing briefly. When a cationization reagent (salt) was required, 10ul of the cationization reagent solution was added to the same matrix/analyte mixture. 0.5uL of the sample solution was spotted on the standard Scout-26 stainless steel sample plate and allowed to air-dry (i.e., this is the dried-droplet sample preparation).

Results


MALDI of Ugi62E product in CHCA matrix
MALDI of Ugi62E product in dithranol matrix
MALDI of PEG400 in CHCA matrix
MALDI of PEG400 in dithranol matrix
MALDI of CHCA background
MALDI of dithranol background

Discussion


Conclusion


Tags

62EInChI=1/C25H33N3O7/c1-24(2,3)27-22(30)21(16-9-10-18-19(12-16)34-15-33-18)28(14-17-8-7-11-32-17)20(29)13-26-23(31)35-25(4,5)6/h7-12,21H,13-15H2,1-6H3,(H,26,31)(H,27,30)
CHCA InChI=1/C10H7NO3/c11-6-8(10(13)14)5-7-1-3-9(12)4-2-7/h1-5,12H,(H,13,14)/b8-5+
Dithranol InChI=1/C14H10O3/c15-10-5-1-3-8-7-9-4-2-6-11(16)13(9)14(17)12(8)10/h1-6,15-16H,7H2
LiTFA InChI=1/C2HF3O2.Li/c3-2(4,5)1(6)7;/h(H,6,7);/q;+1/p-1