trends in analytical chemistry, vol. 8, no.
9,1989
.
concepts have been included in the
keyword file. The authors have se-
lected short passages from a number
of files in the GC-MS module and
have ranked them according to their
significance to the concept under
consideration. When the user selects
a concept from the menu of the key-
word file, he or she receives informa-
tion on the concept selected by the
module authors, ranked in order of
importance. This mode thus provides
a degree of artificial intelligence,
linking the user with persons experi-
enced in GC-MS .
Everything you wanted to know about HPLC
method development
Practical HPLC Method Develop-
ment, by L. R. Snyder, J. L. Glajch
and J. J. Kirkland, Wiley, 1988,
f 28.75 (xvii + 260 pages) ISBN O-
471-62782-g
It is difficult to critically review any
HPLC book by two acknowledged
leading figures in modern HPLC,
and one of their younger protoges
and colleagues (JLG). Fortunately,
there is little to be critical about. This
book has been overdue for quite
some time, and it differs from classic
books on HPLC in that it attempts to
teach the reader how to practically
develop a new HPLC method for al-
most any mixture of compounds.
Though it discusses most of the basics
of HPLC, it does this from the per-
spective of how to vary parameters in
order to optimize a final separa-
tion/resolution. Its goal, as summa-
rized in the last chapter, is to enable
the reader to develop a useful, prac-
tical, and working method of separa-
tion for a given sample, without (at
times) even knowing its composition.
The book is very readable. The
reader is led through the basic prin-
ciples of separation development,
basics of mobile phase effects on sep-
aration (resolution vs. solvent
strength, mobile phase make-up,
pH, ionic strength, column type,
temperature selectivity, plate num-
ber, etc). It very nicely summarizes
The GC-MS subject is covered
with a wide array of topics ranging
from basic principles to practical il-
lustrations of GC-MS applications in
medicine, pharmacy, environmental
science and forensic science. Each
section is accompanied by a list of
relevant books and articles.
The subjects covered are diverse
in their scope, but concise in struc-
ture and content. As such, the mod-
ule cannot be used as a textbook in its
own right, but must be supplemented
with outside readings. On the other
hand, the module does provide a way
the manipulation of mobile phases to
improve separations/resolutions,
and how to develop a logical ap-
proach to solvent selection, solvent
compositions, binary/ternary/qua-
ternary compositions, etc. It covers
modern packings, silica and poly-
meric, advantages and disadvan-
tages, bonding chemistry onto silica,
stability and instability of silica
packings/coverings, bonded phase
concentration/coverage, and the ba-
sic causes of band tailing, shortened
column lifetimes, peak asymmetry,
and low plate number.
Throughout the book there are
tables of steps for ensuring success in
each of the components leading to a
final, successful and reproducible
separation. For instance, there are
tables of steps for ensuring good col-
umn lifetimes and performance, for a
systematic approach to obtaining an
HPLC separation, for preferred
HPLC methods and columns for dif-
ferent samples, for additional sepa-
ration variables to change band spac-
ing in HPLC, for controlling band
spacing in reversed-phase HPLC,
etc. The tables and figures are clearly
conceived and produced, and are de-
signed to aid the reader in using all
the various parts of an HPLC system
to develop a suitable and practical
separation method.
The central four chapters (4-7),
dealing with approaches to systemat-
ic method development, difficult
349
for a user with limited GC-MS expe-
rience to obtain a rapid review of
GC-MS principles. As GC-MS in-
struments proliferate in use, this
module will undoubtedly find a niche
in many laboratories as a valuable
training aid.
RICHARD SAFERSTEIN
Dr. Richard Saferstein is Chief Forensic
Scientistat the New Jersey StatePolice Fo-
rensic Science Bureau, West Trenton, NJ
08625, U.S. A.
separations and the use of other sep-
aration variables and procedures,
gradient elution, and special samples
and techniques (inorganic ions and
ion-exchange, size exclusion, enan-
tiomeric separations, and trace anal-
ysis) form the heart of the book.
They contain most of the practical
hints and steps for method develop-
ment, and deal with virtually all the
major components available to the
chromatographer using HPLC.
Chapter eight deals with comput-
er-assisted method development,
and describes many of the more im-
portant and popular software pro-
grams available today for system
(HPLC) optimization, resolution op-
timization, gradient development,
peak capacity maximization, data
analysis, instrument control, and so
forth. This chapter is clear, lucid,
concise and describes how the soft-
ware works, how it can be optimized,
how it can be routinely employed,
and what it cannot yet do. The
authors have emphasized their own
DRYLAB software, which is com-
mercially available, and though
there are clear efforts not to be pre-
judiced, some bias was probably un-
avoidable. Other software programs
are described, but they seem to me to
get less emphasis. Simplex is dis-
cussed, but not more advanced forms
of system optimization, such as mul-
tiplex or optiplex.
The last chapter (nine) alone is
worth the price of the book. It sum-
marizes method development proce-
dures in almost cookbook or road-
map fashion: start here, do this, do
350
that, if this happens, take this route,
if that happens, take the other road.
These flow-charts are really practi-
cal, and together with the descrip-
tions, are easy to follow to develop
an optimized method in reversed-
phase, normal-phase, or ion-pair
HPLC. This chapter teaches the
reader how to develop a particular
separation, without even knowing
the sample constituents.
One problem I had with the book
is that it does not really assume that
the analyst knows his sample make-
up or for which analyte(s) he is devel-
oping a method. It is assumed that
the analyst just wishes to resolve all
components in his particular sample,
which may or may not be the case. If
we have a complex sample, but only
need to analyze for one component,
we obviously do not need to resolve
all constituents to baseline. We are
developing methods for unknown
peaks, rather than asking ‘I have a
particular component in a complex
sample matrix, how do I now develop
a separation so that I can qualitative-
ly and quantitatively identify this one
component, or perhaps two compo-
nents?’
There are some other minor crit-
icisms as well. For one, the authors,
perhaps expectedly, have referenced
much of their own work. Indeed, in
any given reference list for a specific
chapter, usually half of the items are
from one or more of the authors.
Granted that they have published a
great deal in all areas of HPLC, espe-
cially in optimization, methods selec-
tion and development, packings, and
so forth, but it would have been nice
to see other work mentioned more
often. The references are very up-to-
date, with very few before 1980.
There is no discussion of method val-
idation, nor how to determine when
optimum separation has been
reached, what criteria should be used
and how reproducibility, accuracy,
precision, and validation can be dem-
onstrated. Is it only baseline resolu-
tion of all components in the shortest
time possible, minimum peak asym-
metry numbers, maximum peak ca-
pacity, shortest gradient times, what
else? Usually, we develop an overall
method of identification and quanti-
tation for an analyte in the sample,
not just its best possible separation.
An HPLC separation is but a part of
the final method, and ultimately it
will be used along with analyte iden-
tification methods, quantitation,
sample preparation and work-up, an-
alyte extraction and pre-concentra-
tion, data acquisition and manipula-
tion, etc. How do we then validate
that method, if at all? How do we val-
idate the final, presumably opti-
mized HPLC separation? Few of us
develop separations alone, whereas
this book really discusses HPLC sep-
arations development, not final ana-
lytical methods involving HPLC sep-
arations.
Finally, the book assumes that vir-
tually any mixture of compounds can
be separated via normal-phase, re-
versed-phase, or ion-pairing tech-
niques, columns, and mobile phases.
It seldom addresses the question of
sample mixtures that contain mixed
analytes, perhaps both charged and
uncharged solutes, or those of widely
differing molecular weights, or those
with both anions and cations, etc. It
treats sample mixtures as simple
components of 16 polycyclic aromat-
ic hydrocarbons, or 4 basic amine
drugs, or 20-odd synthetic organic
compounds, or 8 peptides, or x-sub-
stituted aromatics (unspecified struc-
tures), etc. Reality is more complex.
Don’t we need to know something
about structures before we select
methods, columns, mobile phases,
and so forth? Don’t we have to know
SFC-87
Modern Supercritical-Fluid Chroma-
tography, by C. M. White (Editor),
Hiithig, 1988, DM 98.00, (xii + 239
pages) ISBN3-7785-1569-l
This book consists of a selection of
papers presented at what is described
in the introduction as ‘the first meet-
ing ever held that was devoted exclu-
sively to the topic of supercritical-
fluid chromatography’ (SFC). This
meeting, SFC-87, was held in Pitts-
burgh, PA, U.S.A., l-2 October
1987, and attracted more than 200
trends in analyticalchemistry, vol. 8, no. 9, 1989
c
what it is that we wish to determine in
that sample? What do we really have
to know about the sample compo-
nents if we wish to separate all of
them from one another? What about
multimodal chromatography, the
ability of certain columns to function
as both HIC and RP as a function of
mobile phase conditions, or HIC and
IEC, again mobile phase dependent?
Multidimensional chromatography is
mentioned, all too briefly, given
what it can do for very complex sam-
ples.
This book is to be recommended to
all those who use or will use HPLC
for methods development. It com-
plements other books of recent vin-
tage on the fundamentals of HPLC.
It is a tutorial rather than a reference
text. As such, it should be bought
and used by all those involved in
HPLC. It is not really a text for col-
leges or university courses, nor a
stand-alone analytical separations
book. It is a text to be used as we de-
velop our own research program(s).
It is useful, practical, problem-solv-
ing, and should be put onto a smart
system, software program for even-
tual employment in the HPLC labo-
ratory.
I. S. KRULL
Professor Krull is at the Department of
Chemistry, The Barnett Institute, North-
eastern University, 360 Huntington Ave-
nue, Boston, MA 02115, U.S.A.
registered participants.
At first sight, the book is beautiful-
ly produced. It is type-set with a clear
lay-out and good quality figures and
photographs. Each chapter has both
a summary and a ‘concentrate’. I
guess the concentrates were meant
for those readers not even willing to
read the summaries. However, the
concentrate can be as long as the
summary (Chapter 6) or completely
missing (Chapter 4). While reading
the book, I did find a number of edi-
torial mistakes (some of them rather
unpleasant) and some omissions
(there is a Fig. 8a in Chapter 9, but
Fig. 8b is missing). Worst for the
reader is the incomplete information