INTRO TO SPECIAL METHODS AND ASH CONTENT Flashcards
natural substances
Vegetable or animal drugs
made to establish the purity, or to determine the
amount of therapeutically active constituents
present
Analysis of Crude Drugs
Analysis of Crude Drugs made to establish the purity, or to determine the
amount of therapeutically active constituents
present for the purpose of ________
standardization
Scope of Drug Evaluation
identity, purity and quality
identification of biological source
of the drug.
Identity
the quantity of the active
constituents present.
Quality
the extent of foreign organic
material present in a crude drug.
Purity
Methods of Drug Evaluation:
(1) Organoleptic
(2) Microscopic
(3) Physical
(4) Chemical
(5) Biological
It includes the visual examination of drug
Organoleptic
Gives the gross, morphological structure of
the sample
Organoleptic
Organoleptic Plant parts:
Barks, Underground
structures, Leaves, Flowers, Fruits,
Seeds
Color, odor, taste, texture, shape or
size
Organoleptic
Gives a more detailed examination of a
drug
Microscopic or Anatomical
Evaluation:
Microscopic or Anatomical
Evaluation:
Gives a more detailed examination of a
drug, even _______ (cells and
tissues) useful for plants DNA barcoding
histological stuctures
Physical contents or physical properties innate
or characteristic of specific compound in the
sample or the sample as a whole
Physical Evaluation
Physical Evaluation includes
✔ Moisture Content
✔ Viscosity
✔ Melting point
✔ Ash Content
✔ Extractive values
✔ Volatile oil Content
- Optical Rotation
- Refractive Index
Chemical constants or analytical constants,
determination of chemical constituents -
ash, moisture, crude fiber, and extractive
Tests to determine different and specific
chemical constituents
Chemical Evaluation
Tests to determine different and specific
chemical constituents -
estimation of
alkaloidal content, acid value, ester value
or phytoconstituents
They make use of various instruments for
evaluation like spectrophotometry,
chromatography, etc.
Physicochemical and
Instrumental
Determination of the effects of drugs upon
microbes, animals, as animal tissues
Biological Evaluation
This method requires special apparatus for their
performance and a technique that is not chemical
in nature.
Biological Evaluation
Digitalis
Pigeon
Insulin injection
HPLC (rabbit)
Glucagon Injection
Cat
Oxytocin injection
Chicken
Vasopressin injection
Male rat
Rat, same (but of either sex)
Corticotropin injection
Male rat
Vasopressin injection
HPLC (rabbit)
Tubocurarine injection
Metocurine injection
Insulin injection
Female rat (20-23days old)
Human Chorionic Gonadotropin
Sheep blood plasma
Heparin
Protamine sulfate
Spectrophotometer (rachitic rat)
Cod liver oil
Microbiological testing
Niacin
Lactobacillus plantarum
Microbiological testing
Panthothenic acid
Lactobacillus plantarum
Microbiological testing
Cyanocobalamin
Lactobacillus
lechmannii
is the residue left after
incineration.
Ash Content
Ash Content usually represents the ______
naturally occurring in the drug adhering to it.
inorganic salts
Ash Content may also include inorganic matter added for the
purpose of ______
adulteration.
High ash content =
adulteration, substitution,
contamination or carelessness in handling
This may serve as basis for judging the identity
and cleanliness of a drug
Determination of Ash
set a maximum limit on total ash
or acid insoluble ash
Ash standards
Total ash usually contains
carbonates, phosphates, sulfates,
chlorides, oxides, etc. of calcium, magnesium, potassium,
sodium, aluminum, iron and other metallic elements
is the residue after incineration
using the residue after acid treatment and it
represents
Acid insoluble ash
silica
Very dull-red heat
500 to 550 °C
550°C to 700°C.
Dull red heat
Bright red heat
800°C to 1000°C
will convert carbonates to
oxides and alkali chlorides
if present may lose some
chlorides by volatilization
Bright red heat = 800°C to 1000°C
1000 to 1200°C
Yellow red-red heat
White heat
1200 to 1600°C
°C Ca carbonates -> oxides
825 °C
°C – Ca phosphates -> pyrophosphates
1550 °C
°C – Li carbonates -> oxides
600°C
°C – KCl -> sublimes
1500°C
represents silica AND SAND
Acid insoluble ash
Use ASHLESS filter
paper
less than 0.007%
ash content
Acid insoluble ash formula
% acid insoluble ash = wt
of acid insoluble ash x
100/wt of sample
Water soluble ash
= represents
soluble chlorides,
alkali and
ammonium salts
Water soluble ash formula
% WSA = wt of total ash – wt of
residue (upon treating with
water) /wt of sample x 100
For determining ash content of expensive
chemicals.
Residue on Ignition
Residue on Ignition
❖ For determining ash content of expensive
chemicals. Igniting the sample to ______
and residue should not exceed ______
dull redness
500micrograms
volatilized and driven off under the
temperature range of 800 +/- 25 degrees
Celsius
Loss on Ignition
Loss on Ignition
❖ volatilized and driven off under the
temperature range of
800 +/- 25 degrees
Celsius
volatile matter of any kind that is driven off
at 110-120 degrees Celsius
Loss on Drying
Loss on Drying
❖ volatile matter of any kind that is driven off
at
110-120 degrees Celsius
When 2 consecutive weighings do not
differ by more than 0.5 mg
Constant Weight
Constant Weight
When 2 consecutive weighings do not
differ by more than
0.5 mg
use of the five senses especially the eyes
Organoleptic
used in Botany
Microscopic/Anatomical
identification of phytochemical constituents
Phytochemical screening
includes the primary use of numbers or values
Chemical evaluation
alternative for sheep blood plasma
chicken
what vitamin is niacin
B3
what vitamin is Panthothenic acid
B5
what vitamin is cyanocobalamin
B12
incinerator
muffle furnace