Table Of Content-
JOURNAL OF CHROMATOGRAPHYILIBRARY volume 22A
chromatography
fundamentals and applications of
chromatographic and electrophoretic methods
part A: fundamentals and techniques
edited by
E. Heitmann
Western Regional Research Center, US. Department of Agriculture, Berkeley, CA 947 10
ELSEVIER SCIENTIFIC PUBLISHING COMPANY
Amsterdam - Oxford - New York 1983
ELSEVIER SCIENTIFIC PUBLISHING COMPANY
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P.O. Box 21 1,1000 AE Amsterdam, The Netherlands
Distributors for the United States and anad8:
ELSEVIER SCIENCE PUBLISHING COMPANY INC.
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ISBN 0-444-42043-6( Vol. 22 part A)
ISBN 0-444-41616-1( Series)
ISBN 0-444-42045-2( Set)
0 Elsevier Scientific Publishing Company, 1983
All rights reserved. No part of this publication may be reproduced, stored in a retrieval system or
transmitted in any form or by any means, electronic, mechanical, photocopying, recording or other-
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Printed in The Netherlands
TO BRIGITTE
List of authors and coauthors ( *)
Mr. Edward R. Adlard, Shell Research Ltd., Thornton Research Centre, P.O. Box 1,
Chester CH1 3SH, Great Britain (Part B)
Dr. Robert P. Bywater, Pharmacia Fine Chemicals, Box 175, 5-751 04 Uppsala,
Sweden (Part A)
Dr. Nicholas Catsimpoolas, Biochemical Research Laboratories, Department of
Biobehavioral Sciences, Boston University Medical Center, Boston, MA 021 18, USA
(Part B)
Dr. Shirley C. Churms, Department of Organic Chemistry, University of Cape
Town, Rondebosch 7700, South Africa (Part B)
Dr. Graham J. Cowling, formerly Department of Biophysics, University of London,
King’s College, School of Biologxal Sciences, London WC2B 5RL, Great Britain.
Present address: Searle Research & Development, G.D. Searle & Co., Ltd., P.O. Box
53, High Wycombe, Bucks HP12 4H1, Great Britain (Part B)
Dr. Carl A. Cramers, Laboratorium voor Instrumentele Analyse, Technische
Hogeschool, P.O. Box 513, 5600 MB Eindhoven, The Netherlands (Part A)
Dr. Rodney Croteau, Institute of Biological Chemistry, Washington State Univer-
sity, Pullman, WA 99164, USA (Part B)
Dr. David H. Dolphin, Department of Chemistry, University of British Columbia,
Vancouver, B.C., Canada V6T 1W5 (Part B)
Dr. Frans M. Everaerts, Laboratorium voor Instrumentele Analyse, Technische
Hogeschool, Postbus 513, 5600 MB Eindhoven, The Netherlands (Part A)
Dr. Lawrence Fishbein, National Center for Toxicological Research, Food & Drug
Administration, Department of Human Health Services, Jefferson, AR 72079, USA
(Part B)
Dr. Jeffrey B. Harborne, Department of Botany, Plant Science Laboratories, Univer-
sity of Reading, Reading RG6 2AS, Great Britain (Part B)
Dr. Erich Heftmann, Western Regional Research Center, U.S. Department of
Agriculture, Berkeley, CA 94710, USA. Home address: 108 Caiion Dr., P.O. Box
928, Orinda, CA 94563, USA (Parts A and B)
Dr. Csaba Horvath, Department of Chemical Engineering, Mason Laboratory, Yale
University, P.O. Box 2159, New Haven, CT 06520, USA (Part A)
Dr. Jaroslav Janak, Institute of Analytical Chemistry, 662 28 Brno, Czechoslovakia
(Part B)
Dr. Arnis Kuksis, Banting & Best Department of Medical Research, University of
Toronto, Toronto, Ont., Canada M5G 1L6 (Part B)
XI1 LIST OF AUTHORS AND COAUTHORS
Dr. Thomas Kuster, Med.-chem. Laboratorium, Kinderspital Zurich, 8032 Zurich,
Switzerland (Part B)
Dr. Michael Lederer, Institut de chimie minkrale et analytique, FacultC des Sciences,
College propkdeutique, Dorigny, CH- 1015 Lausanne, Switzerland (Part B)
Dr. Karel Macek, Institute of Physiology, Czechoslovak Academy of Sciences,
142 20 Prague, Czechoslovakia (Part A)
* Dr. Harold M. McNair, Department of Chemistry, Virginia Polytechnic Institute
and State University, Blacksburg, VA 24061, USA (Part A)
* Dr. Nigel V.B. Marsden, Institutionen for Fysiologi och Medicinsk Fysik, Up-
psala Universitets Biomedicinska Centrum, Box 572, S-751 23 Uppsala, Sweden
(Part A)
* Dr. Wayne R. Melander, Department of Chemical Engineering, Mason Labora-
tory, Yale University, P.O. Box 2159, New Haven, CT 06520, USA (Part A)
* Dr. F.E.P. Mikkers, Laboratorium voor Instrumentele Analyse, Technische
Hogeschool, Postbus 513, 5600 MB Eindhoven, The Netherlands (Part A)
* Dr. Alois Niederwieser, Med.-chem. Laboratorium, Kinderspital Zurich, 8032
Zurich, Switzerland (Part B)
* Dr. Robert C. Ronald, Institute of Biological Chemistry, Washington State
University, Pullman, WA 99164, USA (Part B)
Dr. Raymond P.W. Scott, Instrument Division, Perkin-Elmer Corporation, Norwalk,
CT 06856, USA (Part A)
* Dr. J. Vacik, Department of Physical Chemistry, Charles University, 501 65
Hradec KralovC, Czechoslovakia (Part A)
* Dr. Th.P.E.M. Verheggen, Laboratorium voor Instrumentele Analyse, Technische
Hogeschool, Postbus 513, 5600 MB Eindhoven, The Netherlands (Part A)
Dr. Gerald H. Wagman, Microbiological Strain Laboratory, Schering-Plough Corpo-
ration, Kenilworth, NJ 07033, USA (Part B)
Dr. Harold F. Walton, Department of Chemistry, University of Colorado, Campus
Box 215, Boulder, CO 80309, USA (Part A)
* Dr. Marvin J. Weinstein, formerly Microbiological Strain Laboratory, Schering-
Plough Corporation, Kenilworth, NJ 07033, USA (Part B)
List of abbreviations
A ampere (Amp)
A Angstrom = lop8c m
AC alternating current
AE aminoethyl
AFID alkali flame-ionization detector
AGR anhydroglucose residue
ANB 2-amino-5-nitrobenzophenone
ASTM American Society for Tesbing and Materials
atm atmosphere = 760 Torr
BD-
cellulose benzoylated DEAE-cellulose
t-BDMS t-butyl dimethylsilyl
BHT (2,6)-di-t-butyl-p-cresol (butylated hydroxytoluene)
b.p. boiling point
b.r. boiling range
BSA N ,0-bis( trimethylsily1)acetamide
BSTFA bis( trimethylsily1)trifluoroacetamide
BTT 3-benzyl- 1- p-tolyltriazine
C centigrade, Celsius
CA cycloamyloses
CAM cellulose acetate membrane (electrophoresis)
cc cubic centimeter (cm3)
cc column chromatography
CCD countercurrent distribution
CDD chlorinated dibenzo-p-dioxins
CECD Coulson electrolytic conductivity detector
Chap. chapter
CI chemical ionization
CLU crosslinked unit structure
CM carboxymethyl
cm centimeter
conc. concentrated
CPm counts per minute
C.V. coefficient of variation
CZE continuous zone electrophoresis
DBM diazobenzyloxymethyl
DC direct current
DCC droplet countercurrent chromatography
DEAE diethylaminoethyl
DMSO dimethylsulfoxide
DP degree of polymerization
DTT di thiothrei to1
XIV LIST OF ABBREVIATIONS
DP degree of polymerization
D?T di thiothreit o1
DVS divinylsulf one
ECD electron-capture detector
ECL effective chain length
ECTEOLA epichlorohydrint riethanolamine
ED electrochemical detector
EDTA ethylenediaminetetraacetica cid
EHV effective hydrodynamic volume
El electron impact
ELS electrophoretic light scattering
EMIT enzyme multiplied immunoassay technique
eqn. equation
eV electron-volt
FD field desorption
FFF field-flow fractionation
f g femtogram = 10-l~g
FIA fluorescent indicator analysis
FID flame-ionization detector
fmole femtomole = 10- Is mole
ft feet
FTIR Fourier transform infrared
8 gram
GC gas chromatography
GC glass capillary gas chromatography
GLC gas-liquid chromatography
GPC gel-permeation chromatography
GSC gas-solid chromatography
h hour
HETP height equivalent to a theoretical plate
HFB heptafluorobutyryl
HI hydrophobic interaction
HIC hydrophobic interaction chromatography
HIE hydrogen isotope exchange
HPLC high-performance liquid chromatography (high-pressure liquid chro-
matography)
HPTLC high-performance thin-layer chromatography
hRF R,X 100
HVE high-voltage electrophoresis
IC Ion Chromatography
ID inside diameter
IF isoelectric focusing
in. inches
IP Institute of Petroleum
IR infrared
xv
LIST OF ABBREVIATIONS
ITLC Instant Thin-Layer Chromatography
ITP isotachophoresis
v
kV kilovolt = 103
1 liter
LC liquid chromatography
LCC liquid column chromatography
LC-EC liquid chromatography electrochemical detector
LFER linear free energy relations
LLC liquid-liquid chromatography
LSC liquid-solid chromatography
M molar
m meter
mA milliampere = A
PA microampere = lop6 A
MBE moving-boundary electrophoresis
m.d.q. minimum detectable quantity
ME mercaptoethanol
meq milliequivdents = lop3e quivalents
Peq microequivdents = equivalents
MF mass fragmentography
mg milligram = 10-~g
Pg microgram = g
MID multiple-ion detection
min minutes
ml milliliter = lop31
Pl microliter = 1
mM millimolar = lop3M
mm millimeter = m
Ccm micrometer = lop6 m
mmole millimole= lop3m ole
1-1m ole micromole = lop6 mole
MO methyl oxime
mol. molecular
mP melting point
MS mass spectrometry
MSA N-methyl-N-trimethylsilylacetamide
msec milliseconds = sec
MSTFA N-methyl-N-trimethylsilyltrifluoroacetamide
MTH methylthiohydantoin
MTX methotrexate
MU methylene unit
v
mV millivolt = 10-~
MW molecular weight
MZE multiphasic zone electrophoresis
N normal
XVI LIST OF ABBREVIATIONS
ng nanogram = 10-~g
nm nanometer = lop9m
nmole nanomole = 10-~m ole
NMR nuclear magnetic resonance
NPD nitrogen-phosphorus detector
OD outside diameter
ODS octadecylsilane or octadecylsilyl
OPA o-phthalaldehyde
PAGE polyacrylamide gel electrophoresis
PC paper chromatography
PCA polycyclic aromatic hydrocarbons
PCB polychlorinated biphenyls
P-cellulose phosphate cellulose
PCN pol ychloronaphthalene
PCP pentachlorophenol
PDM programed multiple development
PE paper electrophoresis
PEG polyethylene glycol
PEI pol ye thyleneimine
PEO polyethylene oxides
PFB pentafluorobenzyl
Pg picogram = lo-’’ g
PGE pore-limit gel electrophoresis
PI isoelectric point
PLC preparative layer chromatography
PLOT porous-layer open tubular (columns)
pmole picomole = lo-’’ mole
PPb parts per billion = parts
PPm parts per million = parts
PPt parts per trillion = 10- I’ parts
psi pounds/sq.in. = 5 1.77 torr
PTFE polytetrafluoroethylene (Teflon)
PTH phenylt hioh y dan toin
RI refractive index
R.I. Retention Index
RIA radioimmunoassay
RRT relative retention time
RT retention time
SBF separation by flow
SCOT support-coated open tubular (columns)
S.D. standard deviation
SDS sodium dodecyl sulfate
SEC size- (or steric) exclusion chromatography
sec seconds
SFC supercritical-fluid chromatography
LIST OF ABBREVIATIONS XVII
SIM selected-ion monitoring
SM sul f omet hy 1
SP sulfopropyl
sq. square
sss
steady state stacking
t tertiary
TAS thermomicro-transfer-application-separatio(nt echnique)
TCA trichloroacetic acid
TCD thermal conductivity detector
TCDD tetrachlorodibenzodioxins
TCP tetrachlorophenol
TD thermionic detector
TEA thermal energy analyzer
TEAB triethylammonium bicarbonate
TEAE tetraethylaminoethyl
temp. temperature
TFA trifluoroacetyl
TFG t hermof rac tography
THF tetrahydrofuran
TLC thin-layer chromatography
TLE thin-layer electrophoresis
TLG thin-layer gel chromatography
TMAH trimethylanilinium hydroxide
TMCS trimethylchlorosilane
TMS trimethylsilyl
TMSDE trimethylsilyldiethylamine
Tris tris( hydroxymethy1)aminomethane
uv
ultraviolet
V volt
vol. volume
vol .p ol.
v/v
WCOT wall-coated open tubular (columns)
wt. weight
w/w wt./wt.
