ACT NO. 12: Analysis Of Crude Drugs Flashcards
Reagents in Expt. 12
• Tsaang-gubat
• 10% Acetic acid in Ethanol
• Concentrated Ammonium Hydroxide Solution
• 20% Ammonium Hydroxide Solution
What is a crude drug?
The products from plant and animal origin found in a raw form.
USP in Crude Drugs
USP <56>
Part 2 of Philippine Pharmacopeia lists the following test performed on crude plant drugs. These are:
a. Microscopic examination
b. TLC
c. Foreign matter
d. Loss on drying
e. Extractives
f. Total ash
g. Acid-insoluble ash
h. Volatile oil determination
i. Pesticide residues
Allows more detailed examination of a drug and it can be used to identify the organised drugs by their known histological characters.
Microscropic Examination
Mostly used for qualitative evaluation of organised crude drugs in entire and powdered forms.
Microscopic Examination
Stains in Microscopic Examination can be used to distinguish ________________.
cellular structure
This is phloroglucinol and concentrated hydrochloric acid give RED stain.
Lignin
This stained pink with RHUTHENIUM RED.
Mucilage
TLC principle
ADsorption
TLC meaning
Thin Layer Chromatography
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 organic matters.
Foreign Matter
Amount of volatile matter of any kind that is driven off at _______ DEGREES CELSIUS.
110-120
Loss on Drying
Presence of moisture in a crude drug can lead to its deterioration due to either activation of certain enzymes or growth of microbes.
Moisture Content
Moisture Content can be determined by heating the drug at _______ in an oven to a constant weight and calculating the loss of weight.
150°C
- Gravimetric method (w,v)
- Gravimetric method (e)
- Azeotropic method or toluene distillation
- Titrimetric method or karl fischer method
- Dew point method
- Electrolytic hygrometric
Methods for the determination of moisture content
Water Content Determination Official Methods
Method 1. Titrimetric Method / Karl-Fischer Method
Method 2. Azeotropic Method / Toluene Distillation Method
Method 3. Gravimetric Method / Drying / Thermal Method
1 mL of the reagent is equivalent to approximately 5 milligrams of water
1 mL of Reagent = 5 mg of H2O
Method 1. Titrimetric Method / Karl-Fischer Method
Primary standard KARL FISHER REAGENT
Na Tartrate
This react with water to SO3
Sulfur dioxide
Prevent reversibility of rxn
Pyridine
Prevent pyridine-S complex
Anhydrous methanol
rx with HI (Hydrogen iodide)
Iodine
SOLVENT in Method 2. Azeotropic Method / Toluene Distillation Method
Toluene and xylene
Method of choice for chemical samples (1-2 grams), biologics
Method 3. Gravimetric Method / Drying / Thermal Method
The extracts obtained by exhausting crude drugs with different solvents are approximate measures of their chemical constituents.
Extractives
Types of Extractives
A. Water soluble extractive
B. Alcohol-soluble extractive
C. Ether-soluble extractives
• glycosides, tannins, mucilage
Water soluble extractive
• tannins, glycosides, resins
Alcohol-soluble extractive
• volatile constituents and fats
Ether-soluble extractives
It is the residue left after incineration.
Total Ash
Total Ash may also include inorganic matter added for the purpose of _______________.
ADULTERATION
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.
Residue on Ignition
Igniting the sample to _____ redness and RESIDUE SHOULD NOT EXCEED _________
DULL redness
500 ug
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
Acid-insoluble ash is part of the total ash that is insoluble with diluted ___________________.
hydrochloric acid
500 to 550° C
Very Dull Red Heat
550 to 700°C
Dull Red Heat
800 to 1000°C
Bright Red Heat
1000 to 1200°C
Yellow Red Heat
1200 to 1600°C
White Heat
Calcium carbonate- calcium oxalate
825°C
Calcium phosphate - calcium pyrophosphate
1550 C
Lithium carbonate - lithium oxide
600 C
Potassium chloride - sublimes at
1500 C
Efficiency of several drugs is due to their odorous principle.
Volatile Oil Determination
The process of removing extraneous matter, such as other parts of the plant, dirt, and added adulterants → prior to use or packaging.
Garbling
Loss on drying employs temperature of __________.
105 +/- 2 C
