Pharmaceutical and Medical Applications of Near-Infrared Spectroscopy

190 Pages·2002·3.116 MB·English

by  Emil W. Ciurczak, James K. Drennen III

Pharmaceutical and
Medical Applications
of Near-lnf rared
Spectroscopy
Emil W. Ciurczak
Applied Chemometrics
Sharon, Massachusetts
James K. Drennen Ill
Duquesne University
Pittsburgh, Pennsylvania
m
MARCEL
-
MARCEDL EKKEIRN,C . NEWY ORK BASEL
DEKKER
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To mom and dad, my sweetie, my kids, my grandson,
and, yes, to my furry companion—
theiractualnamesareAlbinaandEmil;Alissa;Alex,Adam,andAlyssa;
Charlie; and the ever-popular Button (the wonder dog)
EWC
To my family,
with gratitude for their understanding, love, and support
JKD
Copyright 2002 by Marcel Dekker, Inc. All Rights Reserved
Preface
Thenear-infrared(NIR)regionofthespectrumwasdiscoveredin1800
by Sir William Herschel, the noted British astronomer. Considering
that it took 150 years to capitalize on the region, it cannot be called
an overnight success. Large bodies of work exist for the agricultural,
food, textile, polymer, petroleum, and fine chemical industries. It is
onlyinthelast15yearsthatseriouspapershavebeenpublishedinthe
fields of pharmaceutical and medical research. During that time, the
numberofpaperspublishedeachyearhasseemedtoincreasegeometri-
cally, leading to an explosion of references for the novice to peruse.
With this rapid growthof near-infrared spectroscopic research in
the health sciences, it is time for a text such as this. The authors have
combined more than 35 years of industrial and university research ex-
perience in this volume. The pharmaceutical presentation is arranged
inalogicalprogression:theory,instrumentation,physicalmanipulation
Copyright 2002 by Marcel Dekker, Inc. All Rights Reserved
(blending,drying,andcoating),analysis(bothqualitativeandquantita-
tive), and, finally, validation of the method. The varied mathematics
usedinNIR,calledchemometrics,areonlybrieflymentioned.Detailed
explanations and applications are covered in texts or chapters devoted
to the subject (1–4).
In the text, we attempt to showcase the diversity of applications,
not give specific ‘‘cookbook’’ instructions for duplication of prior
work. Numerous references are given, identifying workers in the field
and providing further information about their latest contributions. The
applications are varied, and although the book does not include every
possible citation, a representative cross section of applications and re-
searchers in the field is presented.
All steps in the process of producing a product are assisted by
NIRmethods.ThelevelofcompliancewithFoodandDrugAdministra-
tion(FDA)guidelinesandtherigorousnessofvalidationincreaseasthe
raw materials and active pharmaceutical ingredients (API) are mixed,
granulated,andturnedintoamarketableproduct.Theworkinthepapers
cited runs the gamut from brief feasibility studies to fully validated
methodsreadyforsubmissiontotheFDA.Theamountoftestingvaries;
however, the chemistry and principles are essentially the same for all.
Themedicalchapterisself-containedbydesign.Thetheoryisno
differentfrom‘‘normal’’ chemistryand theinstrumentsare oftenone-
of-a-kind, designed by the researchers. Thus, the importance of the
chapter is to give an overview of the types of applications of NIR in
medicine.Majortopicsinclude:(1)diagnosis(analysis)ofthechemis-
try of the bodily fluids, (2) chemistry of the organs, (3) imaging of
major organs, and (4) chemistry of the skin. The chapter distinguishes
between pediatric (pre- or postnatal) and adult applications, but only
becausetheformerdealwith‘‘wellness,’’whilethelatterapplyto‘‘ill-
ness.’’
Determinationsthoughttobeintherealmofsciencefictionamere
decadeagoarenowalmostroutine:brain–bloodoxygen,fetalmaturity
in utero, viability of tissue upon transplantation, and liver function.
Whoknowswhatwonderswillexistinthenextdecade?Thenextyear?
Emil W. Ciurczak
James K. Drennen III
Copyright 2002 by Marcel Dekker, Inc. All Rights Reserved
REFERENCES
1. H. Mark, Principles and Practice of Spectroscopic Calibration,
John Wiley & Sons, New York, 1991.
2. H. Mark and J. Workman, Jr., Statistics in Spectroscopy, Aca-
demic Press, New York, 1991.
3. H.Mark,‘‘DataAnalysis:MultilinearRegressionandPrincipal
Component Analysis,’’ in Handbook of Near-Infrared Analysis
(D. Burns and E. Ciurczak, eds.), Marcel Dekker, New York,
1992.
4. H.-R. Bjorsvik and H. Martens, ‘‘Data Analysis: Calibration of
NIR Instruments by PLS Regression,’’ in Handbook of Near-
InfraredAnalysis(D.BurnsandE.Ciurczak,eds.),MarcelDek-
ker, New York, 1992.
Copyright 2002 by Marcel Dekker, Inc. All Rights Reserved
Contents
Preface
1. Basic Principles and Theory
2. Instrumentation
3. Blend Uniformity Analysis
4. Granulation, Drying, and Coating
5. Pharmaceutical Assays
6. Validation Issues
7. Medical Applications
Copyright 2002 by Marcel Dekker, Inc. All Rights Reserved
1
Basic Principles and Theory
I. HISTORY
To fully appreciate the basics of near-infrared, a short intro-
duction to its origins and theory are helpful. Understanding
the origin of NIR spectra may assist the practitioner with its
applications.
In 1800, the English astronomer William Hershel was
working on a seemingly trivial astronomical question: Which
color in the visible spectrum delivered heat from the sun? He
used a glass prism to produce a spectrum, while a thermome-
ter,itsbulbwrappedinblackpaper,wasusedtomeasurethe
temperature change within each color. Slight increases were
noted throughout the spectrum, but they were nothing when
Copyright 2002 by Marcel Dekker, Inc. All Rights Reserved
comparedwith thatof ‘‘pure’’sunlight,i.e., allthecolors com-
bined. Going out for a meal, he left the thermometer on the
table just outside the spectrum . . . next to the red band.
When he returned, the temperature had risen dramati-
cally. He postulated an invisible band of light beyond (Latin,
infra) red. Since his prism was glass and glass absorbs mid-
range infrared (IR) radiation, the band was truly near-infra-
red (short wavelength IR). This work was duly reported [1]
and essentially forgotten.
Some work was done in the NIR region of the spectrum
inthelaterportionofthe19thcentury,namely,byAbneyand
Festing [2] in 1881. They measured the NIR spectrum photo-
graphically from 700 to 1200 nm. Some workers made NIR
photographs throughout the early part of this century; how-
ever,fewpracticaluseswerefoundforthetechnique.In1881,
Alexander G. Bell [3] used the NIR to heat a sample inside
of an evacuated cell. Along with the sample was a sensitive
microphone that he used to detect heating/expansion of the
sample as it was exposed to various wavelengths of (NIR)
light. This was the earliest beginnings of photoacoustic spec-
troscopy.
Around 1900, W. W. Coblentz used a salt prism to build
aprimitiveinfraredspectrometer[4,5].Itconsistedofagalva-
nometerattachedtoathermocoupletodetecttheIRradiation
atanyparticularwavelength.Coblentzwouldmovetheprism
a small increment, leave the room (allowing it to re-equili-
brate), and read the galvanometer with a small telescope.
Readings would be taken for the blank and the sample. The
spectrumwouldtakeanentiredaytoproduceand,asaconse-
quence, little work was done in the field for some time.
II. EARLY INSTRUMENTATION
World War II produced the seeds for mid-range infrared in-
struments.Syntheticrubberproducedtoreplacesupplieslost
due to the German naval presence needed to be analyzed. In-
Copyright 2002 by Marcel Dekker, Inc. All Rights Reserved