DOSY 3.1 News and Additions in the Diffusion Software

Transcription

1 DOSY 3.1 News and Additions in the Diffusion Software Agilent Roadshow Paris, 08. June 2011 Péter Sándor Agilent Technologies GmbH, Germany

2 DOSY 3.1 New Features and Functionalities New functionalities: non-uniform gradient (NUG) calibration monoexponential fitting with NUG correction multiexponential fitting, with and without NUG correction (uses a modified SPLMOD)* fitting of distributions of diffusion coefficients with CONTIN* Performance enhancements: improved support for 3D DOSY (including N- and P-type absolute value processing) user-friendly phase-sensitive 3D acquisition and processing display of residuals optional point-by-point instead of peak-segmented 2D DOSY fitting and display removal of peak number limitations in 2D DOSY full panel support for every experiment in the package full ChemPack compatibility (* only for 2D DOSY data sets)

3 Experiment Selection Menu Fully integrated into ChemPack-style Menus

4 DOSY What to do with overlapping peaks? F1 (D) multicomponent fit D DOSY (DOSYHMQC) F2 (ppm) 13 C 1 H F1 (D) D (m 2 /s*10-10 ) Diffusion 6 quinine 8 10 geraniol camphene mixture F2 (ppm)

5 2D DOSY of a Resin Mixture Excellent Chromatographic Resolution of Overlapping Peaks) F1 (10-10 m 2 /s) 1.0 EPIKOTE 1007 "solid resin n~7 2.0 no overlap D.E.R. 331, "liquid resin n= F2 ( 1 H, ppm) 5 June 8, 2011

6 DOSY Phase-sensitive 3D DOSY-HMQC Comparatime mobility study of two polypeptide components (chimeric SH3-domain) F1 ( 15 N, ppm) (0.06) (0.06) F1 ( 15 N, ppm) Averge of 4 peaks: Minor: 1.80+/-0.07 Major: 1.66+/ (0.05) (0.07) (0.04) 1.86(0.08) F2 (1H, ppm) F2 ( 1 H,ppm) 1.65(0.03) 1.76(0.07) F2 ( 1 H, ppm) MGPREVTMKKGDILTLLNSTNKDWWKVEVNDRQGFVPAAYVKKLDSGTGKELVLALYDYQESGDNAPSYSPPPPP

7 + Spatial inhomogeneity of gradient coils B 0 _ B Hz

8 Diffusion range The effect of non-uniform gradients (NUG) Length of the RF coil (16-18 mm)

9 Pulse Sequence for NUG Calibration

10 The Doneshot_nugmap Experiment ~400 Hz G/cm

11 NUG Calibration 0 Semilog plot of comparison between calculated and fitted signal decay #1 # natural log of signal vs (nominal gradient in G/cm) squared

12 2D Default and Pulse Sequence Panels

13 2D Processing and Fiddle Panels

14 Structures and 1 H spectrum of the QGC mixture (in CD 3 OD) CH3 H2C H CH3 H N camphene CH2 H OH CH3 CH3 O CH3 H3C OH N geraniol quinine ppm ppm

15 2D DOSY (Doneshot) of the QGC mixture F1 (D) dosyproc= discrete ncomp=1 nugflag= n F2 (ppm)

16 2D DOSY (Doneshot) of the QGC mixture dosyproc= discrete ncomp=1 nugflag= n

17 2D DOSY (Doneshot) of the QGC mixture dosyproc= discrete ncomp=1 nugflag= n

18 2D DOSY (Doneshot) of the QGC mixture dosyproc= discrete ncomp=1 nugflag= y

19 2D DOSY (Doneshot) of the QGC mixture dosyproc= discrete ncomp=1 nugflag= y

20 2D DOSY (Doneshot) of the QGC mixture dosyproc= discrete ncomp=2 nugflag= n

21 2D DOSY (Doneshot) of the QGC mixture F1 (D) dosyproc= discrete ncomp=2 nugflag= y F2 (ppm)

22 2D DOSY (Doneshot) of the QGC mixture dosyproc= discrete ncomp=2 nugflag= y

23 2D DOSY (Doneshot) of the QGC mixture dosyproc= discrete ncomp=2 nugflag= y

24 3D Default and Pulse Sequence Panels

25 Peak Selection in 3D DOSY Spectra

26 The 3D DOSY Display Panel H O H O O H O O H H O O O H sucrose O H O O H

27 The DOSY Package in VNMRJ_3.1 The DOSY processing software was developed by: Prof. Gareth A. Morris and his group members Mathias Nilsson and lots of others Manchester University, Department of Chemistry Incorporated into VNMRJ_3.x by Dan Iverson, Paul Bowyer, Bert Heise, Péter Sándor

28 Thank you! Questions? 28 June 8, 2011