ESI-MSElectrospray Ionisation-Mass Spectrometry
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Nano-LC ESI-MS of a representative plasma fraction from a single patient TIP-enriched with mAb 42-46 after limited exoglycosidase treatment and trypsin digestion.
At the heart of the MEA--Multinozzle Emitter Array is a disk-shaped, silicon-based microfluidic chip that can sequentially spray up to 96 nanoscale analyte samples into the ion cone, or intake port, of an ESI-MS detector.
ABS has developed an ESI-MS interface that addresses the pharmaceutical industry's requirements for specificity, sensitivity and accuracy in the development of new therapeutic compounds.
Compound 1 and compound 2 were characterized as lucenin-2 and vicenin-2 based on UV and ESI-MS spectra, that showed deprotonated molecule at m/z 609 and m/z 593, respectively, as well as the MS/MS fragmentation pattern, identical to those previously described by Abranko et al.
for [C.sub.56][H.sub.42][N.sub.4][O.sub.3]Zr: C 73.90, H 4.65, N 6.16; found: C 73.65, H 4.88, N 5.42; ESI-MS (C[H.sub.3]OH): m/z calcd.
[.sup.1]H-NMR (DMSO-[d.sub.6]): [delta] ppm: 2.44 (s, [.sup.3]H, -C[H.sub.3]), 7.19 (s, [.sup.1]H, =CH), 7.32-7.36 (t, [.sup.1]H), 7.44-7.49 (m, [.sup.3]H), 8.04-8.06 (d, [.sup.2]H, J=8 Hz), 8.87-8.93 (q, [.sup.1]H); ESI-MS m/z: 346.81 (M+47); Anal.
White powder (21 mg); TLC: Rf = 0.39 (CH3OH/CHCl3, 1:9); 1H NMR (DMSO-d6): d 8.32 (1H, s, H-8), 8.11 (1H, s, H-2), 7.23 (2H, s, 6-NH2), 5.79 (1H, d, J = 2.4 Hz, H-1'), 5.61 (1H, d, J = 4.0 Hz, 2'-OH), 4.54 (1H, m, H-2'), 4.31 (1H, m, H-4'), 3.61/3.43 (2H, m, 5'-CH2), 2.21/1.89 (2H, m, 3'-CH2); 13C NMR (DMSO-d6): d 156.3 (C-4), 152.4 (C-2), 148.9 (C-6), 139.1 (C-8), 119.2 (C-5), 90.6 (C-1'), 80.4 (C-4'), 74.3 (C-2'), 62.7 (C-5'), 34.2 (C-3'); (+) ESI-MS: m/z 252 [M+H]+ and 274 [M+Na]+; (+) HRESI-MS m/z 252.10912 [M+H]+.
The methods used in this study include UV and NMR spectroscopy, electrospray ionization-mass spectrometry (ESI-MS), phase-solubility, and molecular modeling.
Contract notice: Supply and commissioning of two hplc and 1 ESI-MS system for metabolic tracer studies.
The ESI-MS spectra of 1 showed the molecular ion [[M-H].sup.-] at m/z 863, which indicates an A-type interflavanoid linkage procyanidin trimer.