WEEK 11&12 Flashcards
Assay of Hydrogen Peroxide TITRANT
KMnO4
Assay of Hydrogen Peroxide ANALYTE
H2O2 HYDROGEN PEROXIDE
Assay of Hydrogen Peroxide INDICATOR
KMnO4
Assay of Hydrogen Peroxide ENDPOINT
pink color
Assay of Hydrogen Peroxide CHEMICAL REACTION
KMnO4 + H2O2 + H2SO4 — > MnSO4 + K2SO4 + O2 + H2O
Assay of Hydrogen Peroxide AMOUNT OF ANALYTE
2mL
MW OF H2O2
34
mEq OF H2O2
0.017
USP REQT FOR H2O2
2.5-3.5%
%H2O2 =
Vol. of KMnO4 x N x (H2O2/2000)/
Vol. of H2O2 used
H2O2 USP requirement per 100 ml is
nlt 2.5g and nmt 3.5 g
Oxidizing agent, wound cleanser
H2O2
DIRECT PERMANGANATE METHOD
H2O2
KBr
INDIRECT PERMANGANATE METHOD
MALIC ACID IN CHERRY JUICE
TiO2
MnO2
generally applies to the
products from plant and animal origin found in a raw
form.
crude drug
outlines the different methods of analysis that
include physical and chemical tests. The
objective is to establish the identity and
conformity to set standards.
Pharmaceutical Analysis I Laboratory
USP <56> Articles of Botanical Origin
allows more detailed examination of a drug and it
can be used to identify the organised drugs by their
known histological characters
Microscopic examination
mostly used for qualitative evaluation of organised
crude drugs in entire and powdered forms.
Microscopic examination
can be used to distinguish cellular structure
stains
Lignin- phloroglucinol and concentrated hydrochloric
acid give
red stain
Mucilage - stained
pink with rhuthenium red
TLC
* Principle :
Adsorption
useful to analyse Alkaloids, Glycosides like all bio-
constituents
TLC
The parts of the organ or organs other than those
parts of drugs mentioned in the definition and
description of the drug are known as
Foreign matter
Amount of volatile matter of any kind that is driven
off at 110-120 DEGREES CELSIUS.
Loss on Drying
Sodium Chloride
* USP Requirement:
NMT 0.25 % loss of weight
Loss of weight of sample =
weight of sample – weight of dried sample
%Loss on drying =
loss of weight of sample x 100/
Weight of sample
can be determined by heating the drug at 150⁰C in
an oven to a constant weight and calculating the
loss of weight
Moisture content
Methods for the determination of
moisture content
- Gravimetric method (w,v)
- Gravimetric method (e)
- Azeotropic method or toluene distillation
- Titrimetric method or karl fischer method
- Dew point method
- Electrolytic hygrometric
1 mL of the reagent is equivalent to approximately _
milligrams of water
5
Primary standard KARL FISHER REAGENT:
Na Tartrate
react with water to SO3
Sulfur dioxide
prevent reversibility of rxn
Pyridine
prevent pyridine-S complex
Anhydrous methanol
rx with HI
Iodine
Azeotropic Method/ Toluene
Distillation Method
Solvent:
Toluene and xylene
Method of choice for chemical samples (1-2
grams),
✓biologics
Gravimetric Method/
Drying/Thermal Method
the extracts obtained by exhausting crude drugs
with different solvents are approximate measures
of their chemical constituents
Extractives
Water soluble extractive
glycosides, tannins, mucilage
Alcohol- soluble extractive
tannins, glycosides, resins
ether-soluble extractives
volatile constituents and fats
is the residue left after incineration
Total Ash
It may also include inorganic matter added for the
purpose of ADULTERATION.
TOTAL ASH
This may serve as basis for judging the IDENTITY
AND CLEANLINESS of a drug
Total Ash
useful for detecting low grade products, exhausted
drugs, and excess of sandy or earthy matter
Total Ash
_______
*For determining ash content
of expensive chemicals.
Igniting the sample to dull
redness and RESIDUE SHOULD
NOT EXCEED _____
RESIDUE ON IGNITION
500 ug
USP requirement:
* Total ash : NMT _
* Acid insoluble ash : NMT _
5 %
1%
%Total Ash =
weight of ash x 100/
wt. of sample
consists almost entirely of silica derived from the soil
adhering to the drug.
Acid-insoluble ash
Used for the determination of earthy matter present on
roots, rhizomes, and also on the leaves, Crude drugs contain
calcium oxalate crystals the amount may varies depending
on the environmental conditions.
Acid-insoluble ash
Part of the total ash that is insoluble with diluted
hydrochloric acid
Acid-insoluble ash
% Acid-insoluble ash =
wt of the acid-insoluble ash x 100/
wt of the sample
Calcium carbonate- calcium oxalate
825 C
Calcium phosphate – calcium pyrophosphate
1550 C
Lithium carbonate – lithium oxide
600 C
Potassium chloride – sublimes
1500 C
is the process of removing extraneous
matter, such as other parts of the plant, dirt, and added
adulterants
Garbling
