Table Of ContentTHE QUANTITATIVE ANALYSIS
OF DRUGS
Chapman and Hall International Edition
THE
QUANTITATIVE ANALYSIS
OF DRUGS
by
D. C. GARRATT
D.Se. (Lond.), Ph.D., Hon. lVLP.S., F.R.I.C.
Chief Analyst, Boots Pure Drug Co. Ltd.
Assisted by
L. BREALEY, B.Sc., Ph.D., F.R.I.C.
(Physical Assays)
C. A. JOH~SO~, B.Sc., B.Pharm., F.P.S., F.R.I.C.
(Chemical Assays)
K. L. S:VIITH, :\1.P.S.
(Bio-Assay<)
C; SYKES, :\I.Sc., F.R.I.C.
(c11icrobiology)
THIRD EDITION
CH:'\PlVIAN & HALL LTD
I I ~EW FETTER LANE, LONDON EC4-
TOPPA~ COMPANY, LIMITED
First Published 1937
under the title
DRUGS AND GALENICALS:
THEIR QUANTITATIVE ANALYSIS
Second edition 1955
Third edition 1964
© D. C. Garratt 1964
Catalogue number 4/526/75
Original English Language Edition published by
CHAPMA~ & Hall Ltd. London EC 4
No part of it may be duplicated or reproduced in
any manner without written permission from the
publisher.
Distribution or sale of this Edition is authorized only to
TOPPAN COMPANY, LIMITED, TOKYO,JAPAN in:
A(~hanistan, Bangladesh, Brunei, Burma, Cambodia,
Hong Kong, India, Indonesia, Japan, Korea, Laos,
Macao, Malaysia, Nepal, Pakistan, Philippines,
Singapore, Sri Lanka, Taiwan, Thailand and Vietnam.
Available in other countries only through CHAPMAN
& HALL LTD.
ISBN-13: 978-0-412-14810-1 e-ISBN-13: 978-1-4613-3380-7
DOl: 10.1007/978-1-4613-3380-7
PREFACE TO THIRD EDITION
In the present volume-as in previous editions--the intention of the
author is to survey comprehensively all medicinal drugs commonly in use
together with their pharmaceutical preparations.
The last five years has seen a very rapid advance in the field of pharma
ceutical analysis and the need for revision of the previous edition has
become evident. Further, the claims for incorporation of all methods used
in the examination of drugs-chemical, physical, microbiological and
biological-cannot be denied any longer since each type of determination
is sometimes necessary for the adequate control of medicinal preparations.
The author's practice in this book has always been to select from ex
perience those methods likely to prove most serviceable rather than pro
duce a compendium of all published methods. Because of the rapid
increase in the techniques available for pharmaceutical analysis, the need
for specialisation has grown and the author has realised the impractic
ability of keeping in touch with all the practical details which are so
valuable to the analyst. To overcome this difficulty and to enhance the
value of the book, he has obtained the collaboration of specialist colleagues
in the various fields of activity now included in the book. Each contributor
is, in the author's opinion, an authority in his sphere of work and the
author's thanks are due to Dr. L. Brealey (physical assays), Mr. C. A.
Johnson (chemical assays), :\1r. K. L. Smith (bio-assays) and Mr. G.
Sykes (microbiology) for their painstaking work; inevitably the greatest
burden fell on 1\1r. Johnson who devoted much time and energy to the
task.
About one half of the previous edition has been completely re-written,
a few monographs have been deleted and the remainder of the book has
been revised; a considerable amount of new material has been added and
many new appendices avoid repetition in the main text. A considerable
amount of explTlmental work has been necessary to adopt colorimetric
methods to the Il~t' of spectrophotometric measurements at specific
wavelengths.
The various pharmacopceias and codices have a major influence on the
control of the purity of drugs and any textbook on drug analysis must take
cognisance of the methods in current official publications. The necessarily
frequent publication of new pharmacopceias is occasioned by the new
drugs available rather than by advances in analytical chemistry; this
edition is correlated \\ith the British PharmacopCEia 1958 and the United
States Pharmacopeia XVI, but since it includes the latest trends in analyti
cal techniques its contents should cover official methods for quantitative
v
PREFACE TO THIRD EDITION
determinations in future editions of official books. However, since stand
ards may become out-of-date 'it has been decided not to include them in
this edition.
The author again desires to thank the General Medical Council for
permission to include material from the British Pharmacopreia and the
Pharmaceutical Society of Great Britain for permission to include material
from the British Pharmaceutical Codex. The Association of Official Agri
cultural Chemists has also granted permission to utilise information from
their Official Methods of Analysis.
The author wishes to thank numerous journals, particularly The
Analyst and The Journal of Pharmacy and Pharmacology for permission to
publish information. The Society for Analytical Chemistry has also been
generous in permitting access to its Analytical Methods Committee reports
when in the press.
During revision the author has had the benefit of assistance of col
leagues other than those already mentioned. He wishes to thank Mr. W. L.
Sheppard, B.Sc., F.R.I.e., for the revised monographs on Vitamin A and
Vitamin D, Mr. P. G. Marshall, M.A., for the appendix on Infra-red
Spectroscopy, Mr. G. Brewer, A.I.L., for checking the references, Mr.
K. Hazzledine for line drawings and numerous associates for personal
contributions; these include Messrs. P. Atherton, A.R.I.C., D. A. Elvidge,
B.Sc., F.R.I.e., W. H. Harper, and Miss N. F. Mullholland, B.Sc.
Others are acknowledged in the text.
Finally, the author's grateful thanks are given to Miss C. King, B.Sc.,
for preparation of the index, for very patient proof-reading and assistance
in preserving uniformity of style and also to Miss I. Ladden, B.Pharm.,
for compilation of manuscripts and proofs for the printers; their en
thusiastic heIp was invaluable.
D. C. GARRATT
VI
CONTENTS
PAGE
PREFACE TO THIRD EDITION V
ABBREVIATIONS lX
GENERAL MONOGRAPHS, ALPHABETICALLY ARRANGED AND CONSISTING
OF METHODS FOR QUANTITATIVE DETERMINATION OF THE SUBSTANCE,
ITS SA~TS, AND PREPARATIONS OF WHICH IT IS A PRINCIPAL CON-
STITUENT 1
SYNTHETIC ORGANIC COMPOUNDS. METHODS FOR DETERMINATION OF
SUBSTANCES NOT INCLUDED IN THE GENERAL MONOGRAPHS 700
ESSENTIAL OILS 716
OILS, FATS AND WAXES 750
ApPENDICES
I. Determination of Alcohol Content 778
II. Complexometric Titrations 786
III. Kon-aqueous Titrations 792
IV. The Oxygen-Flask Combustion Technique 796·
~Dm~~~~Wmr ~
VI. Extraneous Matter in Food and Drugs 809
VII. Microbiological Assays 813
VIII. Tests for Sterility 827
IX. Pyrogen Testing 833
X. Interpretation of Analytical Results 836
XI. Destruction of Organic Matter 851
XII. Extraction of Organic Chemicals from Viscera, etc. 859
XIII. Electrometric Titrations 864
XIV. Flame Photometry 870
XV. Gas Chromatography 876
XVI. Infra-Red Spectroscopy 881
XVII. The Elimination of Emulsions 887
XVIII. Lam: and Eynon Sugar Titration Tables 888
XIX. Hinton and '\Tacara Chloramine Sucrose Corrections 889
XX. Specific Gravity of Aqueous Glycerol 890
XXI. International Atomic Weights, 1961 891
XXII. Weights and '\leasures, Conversion Tables 893
GENERAL INDEX 895
Vll
The use of portions of the text of the
United States Pharmacopeia, XVI Revision,
official October 1, 1960, is by permission
received from the Board of Trustees of the
United States Pharmacopeial Convention.
The said Board is not responsible for any
inaccuracies of the text thus used.
Permission to use portions of the text of
the National Formulary, Eleventh Edition,
official October 1, 1960, has been granted
by the American Pharmaceutical Associa
ti~n. The American Pharmaceutical
Association is not responsible for any
inaccuracy of quotation, or for false im
plications that may arise by reason of the
separation of excerpts from the original
context.
Ylll
ABBREVIATIONS
Publications
A.B.C.M. The Association of British Chemical
:Vlanufacturers
A.G.A.C. :\lethods of Analysis of the Associatiol of
Official Agricultural Chemists 9th edn.,
( 1960)
Acta Chem. Scand. Acta Chemica Scandinavica
Acta Pharm. Sinica Acta Pharmaceutica Sinica: also known as
Yao Hsueh Hsueh Pao
Acta Pharmacol. Toxicol. Acta Pharmacologica et Toxicologica.
Kobenhavn
Amer. J. Pharm. American Journal of Pharmacy
Amer. ]. Sci. American Journal of Science
Amer. Soc. Testing Materials, American Society for Testing Materials,
Spec. Tech. Publ. Special Technical Publication
Anal. Chern. Analytical Chemistry
Anal. Chim. Acta Analytica Chimica Acta
Analyst Analvst
Ann. Appl. Bioi. Ann,;ls of Applied Biology
Ann. Chim. Anal. et Annales de Chimie Analytique et de
Chim. Appl. Chimie Appliquee
Ann. Chim. Appl. (Roma) Annali di Chimica Applicata (Rom2)
Annalen Annalen der Chemie, Justus Liebigs
Antibiotics & Chemotherapy Antibiotics & Chemotherapy
Arch. Biochem. Biophy.l. Archives of Biochemistry and BiophysIcs
Arch. Pharm. Archiv der Pharmazie
Aui ConKr. ;Vaz. Chim. Pum Atti del Congresso Nazionale di Chimica
ed Appl. Pura ed Applicata
B.M.J. British :VTedical Journal
B.N.F. British]\; ational Formulary (1960)
B.P. British Pharmacopcria (11,58)
B.P.C. British Pharmaceutical Codex (1959)
B.S. British Standard
B. Vet. C. British Veterinary Codex (1953)
Ber. Berichte der Deutschen Chemischen
( ;ese llschaft
.r.
Biochem . Biochemical J Durnal
Biometrika Biometrika
Boll. Chim.-Farm. Bollettino Chimico-Farmaceutico. Milano
Brit. J. Anasthesia British Journal of Amesthesia
Brit. ]. Ind. Med. British Journal of Industrial Medicine
Brit. ]. Nutrition British Journal of Nutrition
Bul. Soc. Sti. RII(ure~ti Bulctinul Societatii de Stiinte din
Bucure~ti
Bull. Narcotics Bulletin on Narcotics, United Nations,
I )epartment of Social Affairs
IX
ABBREVIATIONS
Bull. Sci. Pharmacol. Bulletin des Sciences Pharmacologiques.
Paris
Bull. Soc. Chim. France Bulletin de la Societe Chimique de France
C&D Chemist and Druggist
Geskosl. Farm. Ceskoslovenska Farmacie
Chem. Anal. (Warsaw) Chemia Analityczna (\Varszawa)
Chern. & Ind. Chemistry and Industry
Chern. Eng. Mining Rev. Chemical Engineering and Mining Review.
Melbourne
Chem. Listy Chemickc Listy
Chern. Weekblad Chemische Weekblad
Chern. Zvesti Chemicke Zvesti
Chemiker-Ztg. Chemiker-Zeitung
Chim. et Ind. (Paris) Chimie et Industrie (Paris)
Chimia (Switz.) Chimia (Switzerland)
Compt. Rend. Comptes Rendus Hebdomadaires des
Sceances de I'A cademie des Sciences
D.A.B. Deutsches Arzneibuch, 6 Ausgabe
German Pharmacopreia, 6th Edition
Dansk. Tidsskr. Farm. Dansk Tidsskrift for Farmaci
Determination of Trace The Society for Analytical Chemistry.
Elements, S.A.C. Analytical :vIethods Committee. Trace
Elements in Fertilisers and Feeding
Stuffs Sub-Committee. Determination
of Trace Elements, with Special
Reference to Fertilisers and Feeding
Stuffs (Cambridge), W. Hefler and
Sons Ltd., 1963
Drug Standards Drug Standards
Drugg. Circ. Druggists' Circular, New York
Dtsch. Apoth.-Ztg. Deutsche Apotheker-Zeitung
Endocrinology Endocrinology
FAO Plant Protection Food and Agriculture Organisation of the
Bulletin United Nations, FAO Plant Protection
Bulletin
F.D.A. United States Food and Drug
Administration
Federation Proc. Federation Proceedings
Giorn. Farm. Chim. Giornale di Farmacia, di Chimica e di
Scienze affini
Helv. Chim. Acta Helvetica Chimica Acta
Ind. Eng. Chem. Industrial and Engineering Chemistry
Ind. Eng. Chern., Anal. Edn. Industrial and Engineering Chemistry,
Analytical Edition
Int. Sugar ]. International Sugar Journal
].A.O.A.C. Journal of the Association of Official
Agricultural Chemists
]. Agric. Food Chern. Journal of Agricultural and Food Chemistry
]. Amer. Chern. Soc. Journal of the American Chemical Society
]. Amer. Oil Chernists' Soc. Journal of the American Oil Chemists'
Society
]. Amer. Pharm. Ass. Journal of the American Pharmaceutical
Association
x
ABBREVIATIONS
]. Amer. Pharm. Ass., Journal of the American Pharmaceutical
Sci. Edn. Association, Scientific Edition
]. Appl. Chem. Journal of Applied Chemistry
]. BioI. Chem. Journal of Biological Chemistry
]. Chem. Educn. Journal of Chemical Education
]. Chem. Soc. Journal of the Chemical Society
]. Chroma tog. Journal of Chromatography
]. Endocrinology Journal of Endocrinology
]. Fed. Insts. Brewing Journal of the Federated Institutes of
Brewing, London
]. Ind. Eng. Chem. Journal of Industrial and Engineering
Chemistry
]. Inst. Petrol. Journal of the Institute of Petroleum
]. Org. Chem. Journal of Organic Chemistry
]. Pharm. Chim. Journal de Pharmacie et de Chimie
]. Pharm. Pharmacal. Journal of Pharmacy and Pharmacology
]. Pharm. Sci. Journal of Pharmaceutical Sciences
]. Pharmacal. Journal of Pharmacology and Experimental
Therapeutics
]. Roy. Soc., N .•S .W. Journal of the Royal Society of New South
\Vales
]. Roy. Statist. Soc., Suppl. Journal of the Royal Statistical Society,
Supplement
]. Sci. Food Agric. Journal of the Science of Food and
Agriculture
]. Soc. Chem. Ind. Journal of the Society of Chemical
Industrv
]. Soc. Chem. Ind., japan Journal o(the Society of Chemical Industry,
Japan
Lez. Chim. Org. Lezioni di Chimica Organica
Microchem. j. IVlicrochemical Journal
Mikrochemie l\ Iikrochemie vereinigt mit Mikrochimica
Acta
Mikrochemie. Pregl-Festschr. Mikrochemie. Pregl-Festschrift
Mikrochim. Acta l\1ikrochimica Acta
Mitt. Dtsch. Pharm. Ges. :\litteilungen der Deutschen Pharmazeut
(pub!. in Arch. Pharm.) ischen Gesellschaft und der Pharma
zeutischen Gesellschaft der DDR. In
cluded in Archiv der Pharmazie
N.F. :\ational Formulary XI (1960)
Nature :\"ature
N aturwissenschaften l\'" aturwissenschaften
P.E.O.R. Perfumery and Essential Oil Record
Ph. I. Pharmacopcea Internationalis
(I nternational Pharmacopceia)
First Edition
Pharm. Acta Helv. Pharmaceutica Acta Helvetia:
Pharm . .f. Pharmaceutical Journal
Pharm. Soc. The Pharmaceutical Society of Great
Britain
Pharm. Weekblad Pharmaceutische Weekblad
Pharm. Zentralhalle Pharmazeutische Zentralhalle
Pharm. Ztg. Pharmazeutische Zeitung
Xl
