UNIT 2.

METHODS IN NATURAL PRODUCTS

CHEMISTRY
 Identification of plant material and
its active compound

Extraction

(eg: cold extraction,

Soxhlet extraction)
Isolation and purification

(eg: partitioning, ion-exchange

chromatography)
Structural elucidation

(eg: Mass spectrometry, NMR

spectroscopy)
IDENTIFICATION OF BIOLOGICALLY ACTIVE
MATERIALS
Identity can be achieved by macro- and
microscopical examinations. Voucher
specimens are reliable reference sources.
Outbreaks of diseases among plants may
result in changes to the physical
appearance of the plant and lead to
incorrect identification. At times an
incorrect botanical quality with respect to
 Drug may be collected from:
1 - Wild plants. 2-
Cultivated plants.
Wild plant Cultivated plant
Disadvantage Advantage
Scattered in large or Present in limited
unlimited area area
Difficult to reach Easy to reach
The collector must be The collector must not
highly skilled be skillful person
botanists
Deficiency may occur Continuous supply
due to continuous
collection
 The following precautions should be
considered during stage of collection:
1.The proper time of the day, time of the year and
maturity stage of collection is particularly important
because the nature and quantity of constituents may
vary greatly in some species according to the season
and time of collection
2.The collected plant should be free from any
contamination.
3.Collecting plants which are free from diseases (i.e.
which are not affected by viral, bacterial, fungal
infection).
Authentication of plant material :

This may be confirmed by:

1. Establishing the identity by a taxonomy experts.

2.Collection of a common species in their expected

habitat by a field botanist.

3. By comparing the collecting plant with a voucher

specimen ( herbarium sheet).
Drying of plant materials
Aim of drying:
1. Ease of transport.

2. Ease of grinding

3. Inhibit the growth of microorganisms.

4. Preservative of active constituents.

Drying is done in:

Shade and in sunlight (Natural drying).

Hot air drying or by freeze-drying (Artificial drying).

EXTRACTION
Extraction and fractionation of constituents :

There is no general (universal) method for the

extraction of plant materials.

The precise mode of extraction depends on:

1- The texture of the plant material.

2- The water content of the plant material.

3- The type of substances to be extracted or nature

of active constituents.
EXTRACTION DEFINITION:
The separation of medicinally active portion of
plants through the use of selective solvent
and suitable methods extraction.
The principal methods of extraction are:
1 - Macration
2 - Percolation
3 - Infusion
4 - Dcoction
5 - Digestion
6 - Continuous hot extraction (Soxhlet
extraction procss).
7 - Liquid-liquid extraction
8 - Solvent-solvent ppt.
9 - Distillation
Definition

An extract is a substance made by

extracting a part of a raw material,
often by using a solvent such as
ethanol or water
Method: 1. Percolation

This method uses percolator

The powdered material is packed in the percolator
Enough solvent is than poured to soak the powder
Then more solvent is poured and allowed to percolate
through the material
The extract is collected in a receiver
The process is continued until extraction is complete
 Method: 2. Soxhlet extraction

This is a continuous process of extraction with

a hot solvent
This extractor is provided with a siphoning
system the powdered plant material is packed
in a thimble
The solvent is boiled in a flask
 The evaporated solvent passes through
the side tube of the extractor and
condensed in the condenser, pitted at
the top of the extractor
The condensed hot solvent runs into the
thimble and soaks the material and
extracts the constituents
When the chamber holding the thimble
becomes full the solvent siphons down
to the flask and the process is
continuously repeated until complete
MACERATION :
1. In maceration powdered drug is soaked
in organic solvent and kept for about 24
hrs , sometimes 3-4 days also, depending
upon the part of the plant to be
extracted.

2. The solvent is decanted, filtered and

concentrated.
DECOCTION :
In case of decoction , the powdered plant
material is boiled with the solvents .It is
collected and filtered. Filtered solvent is
concentrated.

Eg. Preparation of tea.

Successive solvent extraction example :

Petroleum ether (60-80)

Benzene

Chloroform

Acetone

Ethanol (95%)

Chloroform water
ISOLATION AND PURIFICATION
STRUCTURAL ELUCIDATION

The process of determining the

chemical structure of molecules.
The following are common methods
determining the chemical structure
(structure elucidation)
1. X-ray diffraction crystals are available
2. Proton NMR
3. Carbon-13 NMR
 WHAT IS STRUCTURAL
ELUCIDATION?
Structure
elucidation is the process of determining
the chemical structure of a compound.
Fororganic compounds, it will often involve the
use of nuclear magnetic resonance spectroscopy
(NMR spectroscopy).
Other characterization techniques include mass
spectrometry, infrared spectroscopy and X-ray
crystallography.
NUCLEAR MAGNETIC RESONANCE
(NMR)
Nuclear Magnetic Resonance (NMR)
spectroscopy is an analytical chemistry
technique used in quality control and
research determining the content and
purity of a sample for as well as its
molecular structure.
INFRARED SPECTROSCOPY

Infrared Spectroscopy is the analysis of infrared light interacting with a

molecule.
This can be analyzed in three ways by measuring absorption, emission
and reflection.
The main use of this technique is in organic and inorganic chemistry.
Used by chemists to determine functional groups in molecules.
X-ray Crystallography

X-ray crystallography is a tool used for identifying the

atomic and molecular structure of a crystal. In which the
crystalline atoms cause a beam of incident X-rays to diffract
into many specific directions.
Mass Spectrometry

A mass spectrometer can rapidly and

accurately measure the molecular weight
and quantities of many substances.
This technique alone cannot distinguish
between two or more substances with the
same molecular weight.
LEARNING CHECK

1- Name the instruments used is isolation and

purification
2- State the instruments used in structural
elucidation.
3- State the properties of alkaloid.
4- State the difference between primary and
secondary metabolites.
THANK YOU