17/03/2024

Overview and Outcomes

Overview of Session

Pharmaceutical  The students are oriented with the different classes of analyses.

Analysis 1 Learning Outcomes

(Week 2) At the end of the course, the student should be able to:

Methods of Analysis and Pharmacopeia

 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

1 2

Classification of Analysis I. Based on sample size

I. Based on sample size • Ultramicroanalysis < 1 mg
II. Based on the extent of determination • Microanalysis 1 mg – 10 mg
III. Based on nature of methods • Semi-microanalysis 10 mg – 100 mg
IV. Based on materials used • Macroanalysis 100 mg – 1 g

3 4

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

5 6

1
 17/03/2024

II. Based on the extent of III. Based on the nature of

determination methods
A. Classical method
B. Instrumental method
C. Miscellaneous or special method

7 8

III. Based on the nature of

methods III. Based on the nature of methods

A. Classical method B. Instrumental method

• also known as general/ chemical/ wet/ • more accurate
stoichiometric method • based on specific physical or
• example : titrimetric analysis chemical properties of the analyte
gravimetric analysis • Examples: spectrometry
polarimetry
chromatography

9 10

Types of Instrumental
III. Based on the nature of methods
Methods
• Electrochemical methods—Works by measuring the
potential (volts) and/or current (amps) in an C. Miscellaneous or special method
electrochemical cell containing the analyte
• Involves the crude drugs and other
• Optical methods—based upon the measurement of the
interaction of the molecules with electromagnetic natural products
radiation • Examples: Acid value
• Chromatography— It is defined as the process of Ash content
separation of the individual components of a mixture
Water content
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

11 12

2
 17/03/2024

IV. Based on materials used Example

An assay using 0.125 g sample, determined for
• Chemical = titrimetric method its total acid constituent using HPLC.
• Physical = instruments and special Determine the specific classification based on
size, extent, nature of methods and material
apparata used
• Biological = use of microorganism and
animals and parts thereof macroanalysis
proximate
instrumental
physical

13 14

Types of Quantitative
Example
Analysis
A 0.5g sample of glycerin was used to determine
the heavy metals content of the sample. After A. Volumetric Analysis B. Gravimetric Analysis
preparing presence of heavy metals were tested by It is an analysis involving the It is an analysis involving the
comparing the sample solution with the standard.
measurement of volume of accurate measurement of
Determine the specific classification based on size,
extent, nature of methods and material used. a solution of known weight of substance being
concentration required to determined which may be
react with the desired isolated in pure form or
macroanalysis constituent. converted to another
substance of known
proximate composition by making it
instrumental react quantitatively with
another substance usually a
physical precipitant.

15 16

Types of Quantitative 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.
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.

17 18

3
 17/03/2024

Physico-Chemical Methods Drug References

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

19 20

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)

21 22

BP (British Pharmacopeia)
 JP was first published in 25 June,
 1864 – Medical Act of 1858 published the 1886
first combined Pharmacopeia
(London, Edinburgh and Dublin)
 In 2007 – BP edition included monographs of materials used for
 IP was published in the year 1951 by
Traditional Chinese medicines WHO in cooperation with United Nations

 2008 Edition and thereafter - revision is annual and is made

official every 1st of January each year
 EP was published in 1969

23 24

4
 17/03/2024

First US Pharmacopeia USP/NF

 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.
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 NF as establishing
legal standards for medical and pharmaceutic substances.

27

25 26

USP/NF Parts of USP

 1975– USP acquires NF and Drug standards
Laboratory from APhA 1. General Notices Section
 1980 – First combined USP-NF was published • The section which presents the basic
assumptions, definitions, and default
 2002 – USP revised and published annually, made conditions for the interpretation and
official every 1st of May each year. application of the United States
--------------------- Pharmacopeia (USP) and the National
May of 2020 – USP / NF Formulary (NF).

30

27 28

General Notices: Topics Parts of USP

1. Monographs and General chapters 2. General Chapters - < >
2. Monograph components 1 to 999 – Physical tests and determinations,
3. Testing practices and procedures microbiological tests, Chemical tests and assays,
4. Test results Biological tests and assays
 ENFORCEABLE
5. Terms and definitions
 1000 to 1999 – General Information (no
6. Prescribing and dispensing mandatory requirement)
7. Preservation, packaging, storage and  Above 2000 apply to articles classified as
labeling Dietary ingredient or supplements

31 32

29 30

5
 17/03/2024

Examples Parts of USP

<41> WEIGHTS AND BALANCES
<611> ALCOHOL DETERMINATION 3. Monograph
<741> MELTING RANGE OR TEMPERATURE  APIand FPP
---
 providesa specification by way of a
 <1160> Pharmaceutical Calculations in Prescription
name, definition, description, tests,
Compounding procedures, and acceptance criteria and
 <1176> Prescription Balances and Volumetric sometimes packaging and labeling
Apparatus Used in Compounding requirements.
---  Sample Raw Material (RM) monograph
file://localhost/Users/tinasabroso/Desktop/Screen Shot 2018-11-13 at 2.07.09 PM.png
<2232> Elemental Contaminants in Dietary Supplements
<2750> Manufacturing Practices for Dietary Supplements

31 32

Official Compendia (USP)

The USP–NF is a combination of two official
compendia: the United States Pharmacopeia The complete monograph of a raw material or a
(USP) and the National Formulary (NF). finished dosage form includes the following
information:
 Monographs for drug substances and 1. chemical structure
preparations are featured in the USP. 2. chemical name
 Excipient monographs are found in the NF 3. purity rubric
 Monographs for dietary supplements and 4. packaging and storage
ingredients appear in a separate section of the 5. reference standard
USP.

35

33 34

Official Compendia Pharmacopeia

• The complete monograph of a raw material or a finished
dosage form includes the following information: …focus mainly on assurance of
6. Identification tests
7.Corresponding tests for chemical and physical constants quality of products by
various tools of analytical
such as melting range, rotatory power, refractive index
etc.
8. Water content
9. Assay procedure
sciences (WHO)
Sample monograph..\..\Acetaminophen Monograph A.docx

35 36

6
 17/03/2024

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.

37