molecule

AstraZeneca vs. Thomson Single Step Column

Patent 7,138,061, 7,381,327, 7,410,571, 8,070,957 and 8,066,875. U.K. Patent 2413972.

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Why?

  1. Annual spend is considerable $↓
  2. Make sure we are getting good value - vendors come and go
  3. Product is fit for purpose

The Study

  1. Standard compound mixture 2-Nitroaniline/4-Nitroaniline
  2. Loading: 20:1 wt ratio Silica:mixture (dry loading)
  3. Conditions: 25% EtOAcin Hexane with solvent reference (PhCH3)
  4. Flow: 40 mL/min, detection @ 254nm
  5. Determine % recovery (mass balance)
  6. Repeat run (n = 3) to minimize instrument/operator error

Conclusion

  1. Thomson SINGLE StEP (patented) simple loading & repeatable

Thomson Instrument (40g)

astrazenecacomp01.gif
 % Recovery
2-nitroaniline
% Recovery
4-nitroaniline
Thomson - 001quantitativequantitative
Thomson - 0029997
Thomson - 003quantitative98
2-Nitroaniline (4 tubes)
4-Nitroaniline (17 tubes)
No TLC needed
Loading - direct
Time 21 min

BiotageSNAP (50g)*

astrazenecacomp02.gif
 % Recovery
2-nitroaniline
% Recovery
4-nitroaniline
Biotage - 001quantitative83
Biotage - 002quantitative74
Biotage - 003NDND
2-Nitroaniline (8 tubes)
4-Nitroaniline (20+ tubes)
TLC needed
Loading - SNAP Cartridge
Time 30+ min

* The amount of aniline mixture added to the Biotagecolumn was adjusted to a total of 2.5 g to reflect the larger mass of silicai (silica:compound ratio was maintained at 20:1 for each column tested).

RediSepRf(40g)

astrazenecacomp03.gif
 % Recovery
2-nitroaniline
% Recovery
4-nitroaniline
ISCO Rf - 001quantitative92
ISCO Rf - 0029793
ISCO Rf - 003quantitative94
2-Nitroaniline (5 tubes)
4-Nitroaniline (20 tubes)
No TLC needed
Loading - sample cartridge
Time 25 min

RediSepRf(40g) Variability

astrazenecacomp04.gif astrazenecacomp05.gif astrazenecacomp06.gif astrazenecacomp07.gif astrazenecacomp08.gif astrazenecacomp09.gif astrazenecacomp10.gif

Patent 7,138,061, 7,381,327, 7,410,571, 8,070,957 and 8,066,875. U.K. Patent 2413972.