The document provides information about a pharmaceutical analysis course for week 2. It includes the names of several Philippine cities where the college of pharmacy is located. It lists the instructor and course facilitator, and covers pharmaceutical analysis 1. The overview describes classifying analytical methods and listing official references. The learning outcomes are to describe analytical methods, list references, and describe pharmacopeial monographs. It then covers classification of analysis based on sample size, extent of determination, nature of methods, and materials used. It also discusses quantitative analysis methods, drug references, and parts of monographs in references like the USP.

1. COLLEGE OF PHARMACY
Valenzuela. Quezon City. Antipolo. Pampanga. Cabanatuan. Laguna
Name of Instructor
C o l l e g e o f P h a r m a c y
C O U R S E FAC I L I TATO R
Pharmaceutical
Analysis 1
WEEK 2
DATE:

2. References
TEXTBOOK: Knevel, A.M. and Digangi, F.E., Jenkin’s Quantitative Pharmaceutical
Chemistry.USA: Mc Graw Hill. 1977.
REFERENCES:
• Watson, David G. Pharmaceuticals analysis: a textbook for pharmacy students and
pharmaceutical chemists, 4th ed. Singapore: Elsevier. 2017.
• Remington’s Pharmaceutical Sciences, (2013) Philadelphia: Lippincott William
and Wilkin
• WHO Expert Committee on Specifications for Pharmaceutical Preparations .
Geneva: World Health
• British Pharmacopeia . 2017.
• The United States Pharmacopeia(USP 40) : NF 35: The National Formulary
.Rockville, Md.: United States Pharmacopeial Convention. 2017.
• Handbook of Modern Pharmaceutical Analysis (2011) Amsterdam; Boston:
Academic Press/Elsevier
• Harris, D.C., Quantitative Chemical Analysis, 9th ed. New York :
W.H. Freeman. 2015

3. Pharmaceutical
Analysis 1
(Week 2)
Methods of Analysis and Pharmacopeia

4. Overview of Session
 The students are oriented with the different classes of analyses.
Learning Outcomes
At the end of the course, the student should be able to:
 Describe the different analytical methods
 List down official references used during pharmaceutical analysis
 Enumerate the different sections in USP and parts of a monograph
 Describe how to use a pharmacopeial monograph
Overview and Outcomes

5. Classification of Analysis
I. Based on sample size
II. Based on the extent of determination
III. Based on nature of methods
IV. Based on materials used

6. I. Based on sample size
• Ultramicroanalysis
• Microanalysis
• Semi-microanalysis
• Macroanalysis
< 1 mg
1 mg – 10 mg
10 mg – 100 mg
100 mg – 1 g

7. II. Based on the extent of
determination
• Proximate analysis
Total amount of a class or a group of
active plant principles in a given
sample.
• Ultimate analysis
Amount of a specific constituent or a
single chemical species present in the
sample

9. II. Based on the extent of
determination

10. III. Based on the nature of
methods
A. Classical method
B. Instrumental method
C. Miscellaneous or special method

11. III. Based on the nature of
methods
A. Classical method
• also known as general/ chemical/ wet/
stoichiometric method
• example : titrimetric analysis
gravimetric analysis

12. III. Based on the nature of methods
B. Instrumental method
• more accurate
• based on specific physical or
chemical properties of the analyte
• Examples: spectrometry
polarimetry
chromatography

13. Types of Instrumental
Methods
• Electrochemical methods—Works by measuring the
potential (volts) and/or current (amps) in an
electrochemical cell containing the analyte
• Optical methods—based upon the measurement of the
interaction of the molecules with electromagnetic
radiation
• Chromatography— It is defined as the process of
separation of the individual components of a mixture
based on their relative affinities towards stationary and
mobile phases.
• Thermal method—Refers to group of techniques in which a
physical property of a substance is measured as a function
of temperature while the substance is subjected to a
controlled temperature program

14. III. Based on the nature of methods
C. Miscellaneous or special method
• Involves the crude drugs and other
natural products
• Examples: Acid value
Ash content
Water content

15. IV. Based on materials used
• Chemical = titrimetric method
• Physical = instruments and special
apparata
• Biological = use of microorganism and
animals and parts thereof

16. Example
An assay using 0.125 g sample, determined for
its total acid constituent using HPLC.
Determine the specific classification based on
size, extent, nature of methods and material
used
macroanalysis
proximate
instrumental
physical

17. Example
A 0.5g sample of glycerin was used to determine
the heavy metals content of the sample. After
preparing presence of heavy metals were tested by
comparing the sample solution with the standard.
Determine the specific classification based on size,
extent, nature of methods and material used.
macroanalysis
proximate
instrumental
physical

18. Types of Quantitative
Analysis
A. Volumetric Analysis
It is an analysis involving the
measurement of volume of
a solution of known
concentration required to
react with the desired
constituent.
B. Gravimetric Analysis
It is an analysis involving the
accurate measurement of
weight of substance being
determined which may be
isolated in pure form or
converted to another
substance of known
composition by making it
react quantitatively with
another substance usually a
precipitant.

19. Types of Quantitative
Analysis
C. Special Methods
analysis which require a distinct type of
technique such as analysis of crude drugs,
assay of fats and fixed oils, assay of
volatile oils and assay of alkaloids.

20. Types of Quantitative
Analysis
D. Physico-Chemical Methods
Analysis based on some specific physical
or chemical property or properties of the
substance being analyzed with the use of
instruments such as: spectrophotometer,
chromatograph units, polarographer,
polarimeter, flourometer.

21. Physico-Chemical Methods

22. Drug References
It comprises LIST
of pharmaceutical
substances,
formula along with
their description
and standards
Official Compendia : Approved sources of
guidelines for drug quality required by certain
practitioners or agencies.
Pharmacopoeia: the word derives from the
ancient Greek φ
α
ρ
μ
α
κ
ο
π
ο
ι
ΐ
α
(pharmakopoiia), from φ
α
ρ
μ
α
κ
ο
-
(pharmako-)
′′drug′′, followed by the verb-stem πο
ι
- (poi-)
′′make′′and finally the abstract noun ending - ι
α
(-ia). These three elements together can be
rendered as ′′drug-mak-ing′′or ′′to make a d
r
u
g
′′.

24. Philippine Pharmacopeia
1996– Creation to signing of the first Philippine Pharmacopeia in
cooperation with the Japanese Government through the initiatives of Dr.
Conrado S Dayrit and Prof Akira Hamada.
May 26, 1999 – Creation Pharmacopeia Organization for the preparation
and publication of the Phil Pharmacopeia thru Department Order no. 216-
F
Exec. Order 302 – Declaring and adopting the Phil Pharmacopeia as
the Official book of Standards and Reference for Pharmaceutical Products
and Crude plant drugs in the Philippines (Mar 29, 2004)

25. BP (British Pharmacopeia)
1864 – MedicalAct of 1858 published the
first combined Pharmacopeia
(London, Edinburgh and Dublin)
 In 2007 – BP edition included monographs of materials used for
Traditional Chinese medicines
 2008 Edition and thereafter - revision is annual and is made
official every 1st of January each year

26.  JP was first published in 25 June,
1886
 IP was published in the year 1951 by
WHO in cooperation with United Nations
 EP was published in 1969

27. First US Pharmacopeia
 1778 - The first American formulary compiled by Gen
William Brown was so called “Lititz
Pharmacopeia,” published at Lititz, Pensylvania,
for use by the Military Hospital of the United States
Army.
27

28. USP/NF
1820 – The first US Pharmacopeia through the efforts of :Dr.
Lyman Spalding, Dr. Samuel Mitchill and Dr. Jacob Bigelow
(Founders of US Pharmacopeial Convention)
1888 – First National Formulary was published by
American PharmacistsAssociation (APhA)
1906 - President Theodore Roosevelt signed into law the first
Federal Pure Food and Drug Act and changed the title to National
Formulary, designating both USP and NFas establishing
legal standards for medical and pharmaceutic substances.

29.  1975 – USP acquires NF and Drug standards
Laboratory from APhA
 1980 – First combined USP-NF was published
 2002 – USP revised and published annually, made
official every 1st of May each year.
---------------------
May of 2020 – USP / NF
USP/NF

30. Parts of USP
1. General Notices Section
• The section which presents the basic
assumptions, definitions, and default
conditions for the interpretation and
application of the United States
Pharmacopeia (USP) and the National
Formulary (NF).
30

31. General Notices: Topics
1. Monographs and General chapters
2. Monograph components
3. Testing practices and procedures
4. Test results
5. Terms and definitions
6. Prescribing and dispensing
7. Preservation, packaging, storage and
labeling
31

32. Parts of USP
2. General Chapters - < >
 1 to 999 – Physical tests and determinations,
microbiological tests, Chemical tests and assays,
Biological tests and assays
 ENFORCEABLE
 1000 to 1999 – General Information (no
mandatory requirement)
 Above 2000 apply to articles classified as
Dietary ingredient or supplements
32

33. Examples
<41> WEIGHTS AND BALANCES
<611> ALCOHOL DETERMINATION
<741> MELTING RANGE OR TEMPERATURE
---
 <1160> Pharmaceutical Calculations in Prescription
Compounding
 <1176> Prescription Balances and Volumetric
Apparatus Used in Compounding
---
<2232> Elemental Contaminants in Dietary Supplements
<2750> Manufacturing Practices for Dietary Supplements

34. Parts of USP
3. Monograph
 API and FPP
 provides a specification by way of a
name, definition, description, tests,
procedures, and acceptance criteria and
sometimes packaging and labeling
requirements.
 Sample Raw Material (RM) monograph
file://localhost/Users/tinasabroso/Desktop/Screen Shot 2018-11-13 at 2.07.09 PM.png

35. The USP–NF is a combination of two official
compendia: the United States Pharmacopeia
(USP) and the National Formulary (NF).
 Monographs for drug substances and
preparations are featured in the USP.
 Excipient monographs are found in the NF
 Monographs for dietary supplements and
ingredients appear in a separate section of the
USP.
35

36. Official Compendia (USP)
The complete monograph of a raw material or a
finished dosage form includes the following
information:
1. chemical structure
2. chemical name
3. purity rubric
4. packaging and storage
5. reference standard

37. Official Compendia
• The complete monograph of a raw material or a finished
dosage form includes the following information:
6. Identification tests
7.Corresponding tests for chemical and physical constants
such as melting range, rotatory power, refractive index
etc.
8. Water content
9. Assay procedure
Sample monograph....Acetaminophen MonographA.docx

38. Pharmacopeia
…focus mainly on assurance of
quality of products by
various tools of analytical
sciences (WHO)

39. Assignment no. 2
Assignment:
1. Submit a copy of Pharmacopeial Monograph
(RM and FPP) from BP and USP
.
2. Given a USP or BP monograph, identify the
Qualitative tests by enclosing in a box and
Quantitative tests by placing double
underline.

40. ANY
QUESTIONS?
You can find me at:
@fatima.edu.ph
facebook.com/
OLFUValenzuelaPharmacy/ (8)-661-3023 loc. 106