Practicum of Pharmaceutical

Analytical Chemistry
 Early information
• 2 CREDITS
• Practicum
• Examination: OSCE (practicum) and Final Exam
 Introduction

• Analysis of the active compound

Definition: Analytical
Chemistry
The application of:

Microbiological
Sciences Active compound
with biological
Activity
 Why?
• Quality
• Safety
• Efficacy
 Analysis processes involve:

1. Characteristic determination and

measurement

2. An assessment of a standard requirements

to assess the quality.
 Analysis will answer
two basic questions:
• about the material that is what exists in the
material (qualitative)
• and how much of the material (quantitative).
 ? ?? ?
Qualitative

Quantitative

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 Qualitative Quantitative
Identification Content/amount

Answering “what” Answering ‘How much”

What chemicals are How much of one or more

present constituent is present
SEMI-
QUANTITATIVE?
 Analyte and Matrices

Part of the sample (material to be analyzed).

Other materials contained in the sample

WHICH ONE?????
 Pure compound (raw material)

• Analysis directly
• Convert samples into a solution suitable to the
measurement technique or method
 Dosage form/Mixture
• Often susceptible to interference (from what?)
• Results will not / less accurate and precise

WHAT IS THE DIFFERENCE BETWEEN ACCURACY

AND PRECISION???
 Quantitative Analysis
A. Analytical Chemistry
R to A in solution

Stoichiometric
VOLUMETRI
aA + bR ↔ AaRb

GRAVIMETRI
Aa Rb = solid 14
B. Physicochemical Method

- Physical characteristic
- Derivatisation
- Instrumental Method

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 Differences?

Chemical Physicochemical
Analysis Analysis

Sample number

Component

Direct/indirect

Standard

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Titration
 INDICATOR

Titrant
Aliquot

Terminologi
Titration
Equivalent point ?
End point
?
 Requirement of Titration
1. Known stoichiometric
2. Route of reaction
3. Fast Equilibrium
4. No side effect
5. Deviation as small as possible
 General of Titration reaction
• aA + b R pP + qQ

• Keq = [P]p [Q]q

[A]a [R]b
 Curve of Titration

-log A E

TS
TS

ml titrant ml titrant
 Type of Titration
Reaction Titration titrant
a) Netralisation (proton
transfer)
- Acidimetry Acid
Aqueous HCl, H2SO4
NAT HClO4 (CH3COOH)
-Alkalimetry
Aqueous NaOH
NAT CH3ONa/CH3OLi
 Titration media
• In aqueous

• If not?
 Reason:
.......................

?
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Reaksi Titration titrant

b) Redox
- Cerimetry Ce4+
- Permanganometry MNO4-
- Cromometry Cr2O72-
- Bromometry Br2 (BrO3-/Br-)
- Iodimetry I2
- Iodometry S2O32-
- Iodatometry IO3-
- Nitritometry NaNO2
Reaksi Titration titrant
c) Precipitation
- Argentometry Ag+
- Mercurimetry Hg+
d) Complexometry EDTA
 Steps in Analysis
Problem Determination Analysis

Selection Method

Sampling

Preparation of samples for analysis

Treatment separation analysis

Measurement

Calculation

Reporting
 Literature
1. 5th Indonesia Pharmocopoeia
2. United State Pharmacopoeia (USP)
3. British Pharmacopoeia (BP)
4. Christian G.D. Analytical Chemistry, 6th ed. John
Willey & Sons, Inc. 2004
5. Mitra S. Sample Preparation Techniques in
Analytical Chemistry, John Willey & Sons, Inc., 2003
(E-book, November 2005).
Etc...