Analysis of Crude Drugs
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the residue remaining after incineration; represents the inorganic salts naturally occurring in the drug and adhering to it, but may also include inorganic matter added for adulteration purposes

ASH CONTENT

represents the inorganic salts/substances present (residue remaining after incineration)

TOTAL ASH

the part of the total ash which is insoluble in diluted HCl or the ash treated with 3N HCl

ACID INSOLUBLE ASH

The residue after carbonized mass is treated with one ml of sulfuric acid and further incinerated after evaporating the acid under the hood

<p>SULFATED ASH</p> Signup and view all the answers

Temperature Equivalents (Heat Type)

<p>Very Dull Heat (500-550) Dull Red Heat (550-700) Bright Red Heat (800 - 1000) Yellow Red Heat (1000-1200) White Heat (1200-1600)</p> Signup and view all the answers

It is the determination of ash content by ignition to dull redness

<p>RESIDUE ON IGNITION</p> Signup and view all the answers

It is performed to control the amount of inorganic matter that may be contained in substances..

<p>RESIDUE ON IGNITION</p> Signup and view all the answers

Residue on Ignition Examples and Percentage/Wt

<p>Acetazolamide USP - NMT 0.1% Aspirin USP - 0.05% Cocaine - NMT 500mcg</p> Signup and view all the answers

It provides a means of determining the percentage of test material which is volatilized and driven off under specified conditions.

<p>LOSS ON IGNITION</p> Signup and view all the answers

It is the amount of volatile matter lost when heated

<p>LOSS ON IGNITION</p> Signup and view all the answers

Loss on Ignition Examples and Percentage/wt

<p>Lotion Calamine USP - 2.0% Magnesium Sulfate USP - 40-52% Titanium Dioxide USP - 0.5% Tribasic Calcium Phosphate - 8% Kaolin - 15% (Methoxymethyl ether) MOM - 33%</p> Signup and view all the answers

Ignition shall be continued at 800oC otherwise indicated until two consecutive weighs do not differ by more than 0.5mg/g of the substance taken, the second weighing following an additional 15-minute ignition period.

<p>IGNITE TO CONSTANT WEIGHT</p> Signup and view all the answers

Drying shall be continued until two consecutive weighings do not differ by more than 0.5mg/g of the substance taken, the second weighing following an additional hour of drying..

<p>DRY TO CONSTANT WEIGHT</p> Signup and view all the answers

Determine the amount of volatilematter of any kind that is driven off under the conditions specified

<p>LOSS ON DRYING</p> Signup and view all the answers

Many drugs that are official in the USP and NF contain varying amounts of water either as BLANK

<p>water of crystallization (hydrates) or water in the adsorbed form.</p> Signup and view all the answers

To make sure that all products fall within BLANK and to ensure product uniformity, it is necessary to specify the water content limits in BLANK

<p>PHARMACOPEIAL STANDARDS, DRUG MONOGRAPHS</p> Signup and view all the answers

METHODS IN WATER CONTENT DETERMINATION

<p>METHOD 1: TITRIMETRIC METHOD/KARL FISCHER METHOD METHOD 2: AZEOTROPIC DISTILLATION METHOD 3: GRAVIMETRIC METHOD</p> Signup and view all the answers

KARL FISCHER METHOD (3)

<p>Direct Titration Residual Titration Coulometric Titration</p> Signup and view all the answers

It is a reference method and a chemical analysis based on the oxidation of sulfur dioxide by iodine in a methanolic hydroxide solution. The original titrimetric solution (Karl Fischer Reagent) contains sulfur dioxide and iodine dissolved in pyrimidine and methanol. The analyte is to be titrated with the reagent.

<p>DIRECT TITRATION/KARL FISCHER METHOD</p> Signup and view all the answers

If sample solutions are colorless, the endpoint may be observed as a change in color from BLANK (KFM)

<p>Canary Yellow to Amber Yellow</p> Signup and view all the answers

The endpoint is more commonly determined electrometrically with an apparatus employing a simple electrical circuit. At the endpoint, a slight increase of current flow is observed. (KFM)

<p>50-150 microamperes for 30 seconds to 30 mins</p> Signup and view all the answers

For test preparations, the analyte/specimen shall contain an estimated amount of ---, unless otherwise specified in the individual monograph

<p>10 to 250 mg of water</p> Signup and view all the answers

If the specimen is an aerosol with propellant, store it in a freezer for NLT 2 hours, open the container, and test 10.0 ml of the well-mixed specimen. In a titration, determine the endpoint at a temperature of 10°C or higher.

<p>DIRECT TITRATION/KARL FISCHER METHOD</p> Signup and view all the answers

If specimen is a capsule, use a portion of the mixed contents of not fewer than 4 capsules.

<p>DIRECT TITRATION/KARL FISCHER METHOD</p> Signup and view all the answers

If specimen is a tablet, use powder from not fewer than 4 tablets ground to a fine powder

<p>DIRECT TITRATION/KARL FISCHER METHOD</p> Signup and view all the answers

If specimen is hygroscopic, dissolve the specimen in a suitable solvent (mostly methanol). Using a syringe, transfer the solution to a titration vessel. Using a 2nd portion of solvent, rinse the container where the specimen was dissolved and add the washing to the titration vessel and immediately proceed to titration.

<p>DIRECT TITRATION/KARL FISCHER METHOD</p> Signup and view all the answers

Study Notes

Ash Value

  • Represents the inorganic salts/substances present in a drug, which can be naturally occurring or added for adulteration purposes
  • Determined by the residue remaining after incineration
  • Can be further divided into soluble and insoluble parts, with the insoluble part being the residue that remains after treating the ash with diluted HCl or 3N HCl

Acid-Insoluble Ash

  • The residue that remains after treating the carbonized mass with sulfuric acid and further incineration
  • Provides a means of determining the amount of inorganic matter that may be present in a substance

Temperature Equivalents (Heat Type)

  • Involves the determination of ash content by ignition to dull redness
  • Performed to control the amount of inorganic matter that may be contained in substances

Residue on Ignition

  • Provides a means of determining the percentage of test material that is volatilized and driven off under specified conditions
  • Represents the amount of volatile matter lost when heated
  • Examples and percentage/weight can be used to determine the amount of volatile matter

Loss on Ignition

  • Determination of the amount of volatile matter that is driven off under specified conditions
  • Ignition is continued at 800°C until two consecutive weighings do not differ by more than 0.5mg/g of the substance taken
  • Drying is continued until two consecutive weighings do not differ by more than 0.5mg/g of the substance taken

Water Content Determination

  • Many drugs contain varying amounts of water, either as a bound or absorbed water
  • To ensure product uniformity, it is necessary to specify water content limits
  • Methods used for water content determination include the Karl Fischer method

Karl Fischer Method

  • A reference method and a chemical analysis based on the oxidation of sulfur dioxide by iodine in a methanolic hydroxide solution
  • The endpoint can be observed as a change in color from colorless to brown or determined electrometrically with an apparatus employing a simple electrical circuit
  • The analyte/specimen should contain an estimated amount of water, unless otherwise specified in the individual monograph

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Explore the concept of the residue left after incinerating pharmaceutical substances, which includes inorganic salts from the drug and potential adulterants. Test your knowledge on this topic with our quiz!

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