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Qualitative-Quantitative Chemistry

● also known as Analytical Chemistry or Pharmaceutical

Pharmaceutical ●
Chemistry.
is a branch of chemistry which provides information
Analysis 1 relative to the composition of matter

Prepared by:
Samantha Leigh L. Ocampo, RPh

Divisions of Analytical Chemistry Classification of Analysis

1. Qualitative – involves the nature of the constituents of a given material. 1. Based on a sample size
- Composition determination (elements, compounds, AI)
a. Ultra micro : <1 mg
- Ascertainment of impurities present in a given sample
b. Micro: 1mg – 10mg
- Answers the question, WHAT IS PRESENT in a given sample?
c. Semi-micro: 10mg – 100mg
2. Quantitative – determination of the proportion of components in a given
sample. d. Macro: 100mg – 1g

- Answers the question, HOW MUCH is present in a given sample?

Classification of Analysis Classification of Analysis

2. Based on the extent of determination 3. Based on nature of methods

a. Proximate – total amount of class or group of active plant
a. Classical – aka General / Chemical Reaction
principles in a given sample
Ex: Det. of total alkaloids, – Ex: Titrimetric analysis, Gravimetric analysis
a. Ultimate – amount of specific compartment / single b. Instrumentation – based on specific physical or chemical
chemical species present in the sample properties of analyte; more accurate analysis

Ex: Assay of atropine in Belladonna –Ex: Spectrophotometry, Polarimetry,

Chromatography

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Classification of Analysis Classification of Analysis

3. Based on nature of methods 3. Based on nature of methods

c. Miscellaneous / Specific Methods – involves crude drugs c. Miscellaneous / Specific Methods – involves crude drugs
and natural products derived from them. and natural products derived from them.
–Ex: Water content determination, Ash content, Acid Value –Ex: Water content determination, Ash content, Acid Value

Classification of Analysis Data Assessment: Errors

4. Based on Material used ● Absolute Error

Actual - Theoritical
a. Chemical – used of chemical reagents

b. Physical – instruments and special apparatus ● Relative Error

Actual – Theoritical
c. Biological – use of microorganism, animals
Theoritical

Two types of Errors: Two types of Errors:

1. Indeterminate errors 1. Indeterminate errors

■ Uncontrollable causes ■ are intangible & their elimination by the analyst is

impossible.
■ aka “random errors”
■ causes:
■ manifest themselves by slight variations in a series of
observations made by the same observer under identical ● Difficulty to detect
conditions.
● eg. a differences in the judgment & skill of the analyst

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Two types of Errors: Two types of Errors:

2. Determinate errors 2. Determinate errors

■ Identifiable causes ■ causes:

■ aka “systematic errors’ or “bias” a. Personal errors made by the individual analyst

b. Errors of method caused by faulty procedure (Methodic)

c. Apparatus errors due to poor construction or calibration

(Instrumental)

Data Assessment: Accuracy and Precision Repeatability

● Accuracy - Expresses the precision obtained under the same

○ Precision
operating conditions over a short interval of time.
○ closeness to true value/
● closeness of actual values - It can also be termed intra-assay precision
literature value.
● indicates how clos
○ indicates how well a
measurement agrees w/
the accepted or true
value

Intermediate Precision Data Assessment: Statistical consideration

- Expresses within laboratory variation of precision. a. Confidence Interval

- When a the analysis is done by different analyst and range of value around an actual result w/ which true value
different equipment. is expected to lie w/ a define level of probability.

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Data Assessment: Statistical consideration
b. Significance Test
compare individual values or set of values for significant
differences.
○ Null hypothesis (HO) - there is no significant differences
○ Alternate hypothesis (HA)
Definition of Other Terms
● Analytical blank
○ This consist of all the reagents or solvents in an analysis
without any of the analyte being present.
● Calibration
○ Involves comparison of the value or values if a particular
parameter measured by the system under strictly defined
conditions with pre-set standard values.
Definition of Other Terms
● Linearity
○ Most analytical methods are based on processes where the
method produces a response that is linear and which
increases or decreases linearly with analyte concentration.
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Data Assessment: Statistical consideration
Alternate hypothesis (HA)
■ One-tailed - there is a significant difference & indicates
what is the dissimilarities or variations, (greater than…. less
than….).
■ Two-tailed - there is a significant difference but doesn’t
indicate the dissimilarities or any variations.
Definition of Other Terms
● Limit of detection
○ This is the smallest amount of an analyte which can be
detected by a particular method.
x – Xb = 3SB
X = signal from the sample
XB = signal from the analytical blank
SB = is the SD of the reading for the analytical blank
Definition of Other Terms
● Robustness
○ Refers to how resistant the precision and accuracy of an assay
is to small variations in the method.
■ Example: Changes in instrumentation, slight variations in
extraction process, sensitivity to minor impurities in reagents
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Definition of Other Terms Definition of Other Terms

● Selectivity ● Sensitivity
○ Is a measure of how capable it is of measuring the analyte ○ Indicates how responsive it is to a small change in the
alone in the presence of other compounds contained in the concentration of an analyte.
sample.

○ The most selective analytical method involve a

chromatographic separation.

Definition of Other Terms

● Weighing by difference
○ Used to minimize weighing errors in an analytical procedure.

○ The sample is weighed in a suitable vessel; The weighing

vessel is then reweighed and the difference between the
weights before and after transfer gives the weight of the
sample.