CCC 2010 Book of Abstracts

124 Pages·2010·5.63 MB·English

by  Valued Customer

th
6 International Symposium on
Countercurrent Chromatography

BOOK of ABSTRACTS

Institut des Sciences et Techniques de l'Ingénieur de Lyon
July 28-30, 2010, Villeurbanne, France
6th International Conference on Countercurrent Chromatography, Lyon, July 28-30, 2010 1
6th International Conference on Countercurrent Chromatography, Lyon, July 28-30, 2010 2
Program

Wednesday, July 28, 2010

8h30 – 9h00 Registration
9h00 – 9h10 Opening A. Berthod

Session 1 - Theory and Method development chaiman: G.H. Harris
9h10 – 9h40 1-1 Plenary Lecture – Scalable Technology for the Extraction of Pharmaceutics
(STEP): the transition from academic know-how to industrial reality
I.A. Sutherland
9h40 – 10h00 1-2 Using the liquid nature of the stationary phase in CCC
A. Berthod
10h00 – 11h00 Poster session 1 with coffee break

11h00 – 11h20 1-3 Two dimensional CCC: 1st Traditional CCC, 2nd pH-zone refining CCC
Y. Pan
11h20 – 11h40 1-4 A new versatile process for purification of ionisable compounds using Centrifugal Partition
Chromatography L. Boudesocque
11h40 – 12h00 1-5 Gradient elution in CCC: a new layout for an old path
S. Ignatova
12h00 – 12h20 1-6 Building up the separation of enantiomers by CCC/CPC: the case of Whelk-O
C. Minguillon

12h20 – 13h45 Lunch break

Session 2 - Instrumentation chairman: I.A. Sutherland
13h45 – 14h30 2-1 Plenary Lecture – Origin and development of HSCCC
Y. Ito
14h30 – 14h50 2-2 Observation of two phase behavior in hydrodynamic CCC column using a small wireless CCD
camera set on the rotary frame E. Kitazume
14h50 – 15h10 2-3 Performance comparison of three types of counter-current chromatographs for the separation
of components of hydrophilic and hydrophobic color additives
A. Weisz
15h10 – 15h30 2-4 Unconventional applications of CCC and related techniques
P. Fedotov
15h30 – 15h50 2-5 Development and evaluation of a spiral tube column for CCC
X. Cao
15h50 – 16h10 2-6 Improvement of Hydrostatic-CCC performances by cocurrent elution
L. Marchal
16h10 – 16h30 2-7 Flash HSCCC
Q. Du

16h30 – 19h00 Poster session 2 with Welcome reception and Technical
Exhibition

6th International Conference on Countercurrent Chromatography, Lyon, July 28-30, 2010 3
Thursday, July 29, 2010 chairman: A. Berthod

9h00 – 9h30 3-1 Plenary lecture – CCC: Simplicity, mixing and nomenclature
W.D. Conway
9h30 – 9h50 3-2 Rapid Solvent System Scouting Utilizing "On-Demand" Preparation of HEMWat Solvent
Series Phases G. Harris

9h50 – 11h00 Poster session 3 with coffee break

Session 3 - Natural product & Biological purifications
Session A: Natural Products Session B: Biological Applications
chairman: G.G. Leitao chairman: Yoichiro ITO
11h00 – 11h20 3-3 The role of CCC to separate volatile 3-7 EECCC fractionation and biochemometric
ecological markers from Piper claussenianum evaluation of the anti-TB active principles in
M.A.C. Kaplan lipophilic hops extracts G.F. Pauli

11h20 – 11h40 3-4 Continuous elution-extrusion CCC for 3-8 CCC preparation and bioactivity studies
repeated preparation of natural cytotoxic of peptides from Mytilus coruscus
andrographolides from Andrographis Y. Lu
paniculata S. Wu
11h40 – 12h00 3-5 Isolation and identification of novel C17- 3-9 Isolation of biologicals by centrifugal
chain anacardic acids from heated cashew precipitation chromatography
nut shell oil by direct coupling prep CCC and M. Knight
ESI-MS-MS G. Jerz
12h00 – 12h20 3-6 Major saponins isolated from Platycodi 3-10 Driving purification of marine active
Radix by CCC and enzymatic transformation compounds by CPC/CCC
Y.S. Kim G. Audo

12h20 – 14h00 Buffet break with Poster session 4 and Exhibition

Session 4 - TMB, CCC & CPC and Original Applications

Session A: TMB, CCC and CPC Session B: Original Applications

chaiman: T. Maryutina chairman: Xueli Cao
14h00 – 14h20 4-1 J-type toroidal CCC for protein 4-7 Application of CCC for oil analysis:
separations retention features and kinetic aspects
R. Van den Heuvel A.V. Soin
14h20 – 14h40 4-2 Multiphase flow modeling in Centrifugal 4-8 Coupling on-line CPC with HPLC for the
Partition Chromatography fractionation of flavonoids from Hippophae
S. Adelman rhamnoides berries T. Michel

14h40 – 15h00 4-3 Effect of the key operating parameters 4-9 Preparative separation of basophiles,
on the efficiency of intermittent CC extraction major effector cells in allergy, by a density
P. Hewitson gradient method H. Shiono

4-4 Continuous liquid-liquid chromatography: 4-10 Antioxydant compounds isolated from
15h00 – 15h20
sequential centrifugal partition Athrixia phylicoides

chromatography mode of operation D. De Beer

M. Minceva

4-5 The use of renewable solvents in the 4-11 Isolation of Hops (humulus lupulus L.)
15h20 – 15h40
formulation of CC separations systems bitter acids via CCC

B.F. Freisen C. Dahlberg

4-6 Use of robotics for two-phase solvent 4-12 Intensified Extraction of Natural
15h40 – 16h00
system selection in CCC Products by Co-current Triphasic Centrifugal
I. Garrard Partition Extraction L. Marchal

16h00 – 17h00 Poster session 5
18h00 – 19h30 Evening tour of Lyon in buses
20h00 – 23h30 Gala dinner at the Chateau-Perrache Palace
6th International Conference on Countercurrent Chromatography, Lyon, July 28-30, 2010 4
Friday, July 30, 2010

Session 5 - Advances in CCC modeling chairman: W.D. Conway

9h00 – 9h20 5-1 Modeling CCC considering instrument and operational parameters
H. Guzlek
9h20 – 9h40 5-2 Modeling advanced CCC modes
J. De Folter
9h40 – 10h00 5-3 Modeling separations in non-synchronous coil planet centrifuges, the effect of critical β-values
P. Wood

10h00 – 11h00 Poster session 6 with coffee break

Sesion 6 - Symposium Closing chairman: G.F. Pauli

11h00 – 11h30 6-1 Keynote lecture: The R&D of CCC and its applications in South China
T.Y. Zhang

11h30 – 12h00 6-2 Closing lecture: Developing CCC to the needs of pharmaceutical research
N. Sumner

12h00 Closing remarks, Edward Chou and Crafty Chromatographer Award ceremony
and first announcement for CCC2012
A. Berthod

12h20 – 14h00 Buffet gathering with last Poster session 7 and Exhibition

6th International Conference on Countercurrent Chromatography, Lyon, July 28-30, 2010 5
6th International Conference on Countercurrent Chromatography, Lyon, July 28-30, 2010 6
th
6 International Symposium on
Countercurrent Chromatography

ABSTRACTS of
ORAL communications

Institut des Sciences et Techniques de l'Ingénieur de Lyon
July 28-30, 2010, Villeurbanne, France
6th International Conference on Countercurrent Chromatography, Lyon, July 28-30, 2010 7
6th International Conference on Countercurrent Chromatography, Lyon, July 28-30, 2010 8
1-1 O1
Scalable Technology for the Extraction of Pharmaceutics (STEP):
the transition from academic knowhow to industrial reality

Ian Sutherland1,*, Svetlana Ignatova1, Peter Hewitson1,
Lee Janaway2, Philip Wood2, Neil Edwards2, Hacer Guzlek2, David Keay2,
Keith Freebairn3, David Johns3, Nathalie Langdale3, Chris Thickitt3, Elsa Vilminot3,
Ben Mathews4
1,* Brunel Institute for Bioengineering, Brunel University, Uxbridge, UB8 3PH, UK,
Tel: [phone], Fax:[phone], [email protected]
2 Dynamic Extractions Ltd, 890 Plymouth Road, Slough, UK
3 GlaxoSmithKline, Stevenage, UK
4 Pfizer, Sandwich, UK

Keywords: Pharmaceutical, Extraction, Scale-up, Counter-current Chromatography, High Value
Manufacturing, Solvent Systems

The manufacture of high value pharmaceutical products, whether from natural products,
fermentation processes or chemical/biochemical synthesis, involves multiple, down stream
processing steps (often using generic equipment common to various pharmaceutical indutries)
before a pure product is obtained. The plant involved is highly capital intensive and major change
comes at a high cost, even if efficiency is vastly improved. Waste and its disposal are economically
and environmentally challenging issues. In this research and development programme we plan to
develop small footprint, versatile, continuous manufacturing technology and methodologies which
can be inserted into existing process plant and systems and, as a scalable continuous process.

The product is always maintained in an easily managed liquid stream which is able to cope with
crude extracts and particles without any pre-conditioning, thus reducing the number of processing
steps and leading to highly efficient, and environmentally friendly production processes with no
expensive solid support materials easily recycled liquids. The basic science, developed with
industry and supported by the Research Councils, has already been successfully demonstrated;
scale up is feasible in batch and continuous process mode at the laboratory and pilot scale and the
technology is now at readiness level 3. This development programme is driven by the needs of the
pharmaceutical industry and integrates technology providers and the scientific development team,
addresses major production challenges and aims to provide a flexible, low capital change to
production processes.

This £1.5m user driven research programme [1] part funded by industry and part funded by the UK
government started in September 2009 and is proceeding well with a number of user driven
applications in its portfolio with 100% success rate so far. It has also identified a few hurdles that
could delay the uptake of the technology if not addressed urgently by the scientific and industrial
community involved in the development of the technology. While there will be limitations from a
commercial confidentiality point of view on what can be exposed, the research challenges will be
presented along with summary results.
6th International Conference on Countercurrent Chromatography, Lyon, July 28-30, 2010 9
1-2 O2
Using the liquid nature of the stationary phase in CCC
Alain Berthod*, Yi Feng Li and Nazim Mekaoui
*Laboratoire des Sciences Analytiques, Université de Lyon, CNRS, Batiment CPE, 69622 Villeurbanne,
France, e-mail: [email protected]; fax [phone]

Keywords: liquid properties, countercurrent chromatography, elution-extrusion, dual mode, back extrusion

The liquid state of the stationary phase in countercurrent chromatography (CCC) is the characteristic feature
of the technique. It was shown the this feature has tremendous advantages that justify the great effort
needed to obtain a stable and liquid stationary phase in chromatography.

The main advantage of the liquid stationary phase is loadibilty. The solutes to be separated have access to
the volume of the stationary phase rather than just its surface as it is with any solid stationary phase. CCC is
mainly a preparative technique.

The next huge advantage is sample recovery. Irreversible adsorption in the stationary phase does not
belong to CCC. If part of the injected sample is too strongly retained by the liquid stationary phase, it will be
easy to recover that part of the sample by emptying the column.

The dual-mode method was introduced long time ago. It allows for full recovery of the injected sample by
changing both the phase flow direction (haid(cid:1)tail becomes tail(cid:1)head or vice versa) and the phase nature
(the mobile lower phase is switched for the stationary upper phase, or vice versa).

The elution-extrusion method was more recently introduced, consisting in extruding the column content after
a selected time of classical elution. The CCC column is cleaned by the stationary phase being ready to start
over after the separation. The back-extrusion method was also described as the last logical step in the use
of all possible elution modes using the liquid nature of the stationary phase in CCC.

The four possible modes are compared in term of separation, resolution, experiment duration and ease of
procedure using a hypothetical mixture and computing the data.

6th International Conference on Countercurrent Chromatography, Lyon, July 28-30, 2010 10