DRUG ANALYSIS

 Quantitative analysis of crude drugs and of the products derived from them is made to establish the purity, or to
determine the amount of therapeutically active constituents present for the purpose of standardization.
 The special methods employed in the analysis of this type may be classified as follows:
(1) Chemical Methods such as those employed in the determination of ash, moisture, crude fiber, and extractive
obtained with different solvents, estimation of alkaloidal content, assay of fats, fixed oils, waxes, balsams,
and resins, assay of volatile oils, etc.
(2) Physicochemical and Instrumental Methods such as Spectrometry, Chromatography, Potentiometry,
Polarography, Radioactivity, etc.
(3) Biological Methods in which the effects of drugs upon microbes, animals, as animal tissues are measured.
This method requires special apparatus for their performance and a technique that is not chemical in nature.

Determination of Ash

 The ash content of a crude drug is the residue left after incineration.
 It usually represents the inorganic salts naturally occurring in the drug adhering to it. But it 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 and gives information relative to its
adulteration with inorganic matter.
 Ash standards set a maximum limit on total ash which is part of the total ash that is insoluble in dilute
hydrochloric acid.
 Total ash usually contains carbonates, phosphates, sulfates, chlorides, oxides, etc. of calcium, magnesium,
potassium, sodium, aluminum, iron and other metallic elements. Other inorganic constituents of drugs like
ammonium salts, some alkali iodides and nitrates are volatilized and may no longer be included in the total ash.
 The acid-insoluble ash consists almost entirely of silica derived from the soil adhering to the drug.
 The control temperature is the most important analytical; factor in making ash determination.
(1) Very dull-red heat = 500 to 550 C
(2) dull red heat = 550C to 700C.
(3) bright red heat = 800C to 1000C will convert carbonates to oxides and alkali chlorides if present may lose
some chlorides by volatilization.
(4) Yellow red-red heat = 1000 to 1200C
(5) White heat = 1200 to 1600C

Example 1 - Determination of the Total and Acid-Insoluble Ash Content of Acacia

Accurately weigh two (2) to four (4) grams of the air-dried material in a tared crucible and incinerate at a low
temperature not to exceed very dull red heat (500C to 550C) until free from carbon and determine the weight of
the total ash.

Boil the ash obtained with 25 mL of diluted hydrochloric acid for five (5) minutes, collect the insoluble matter in a
tared filter or ashless filter, wash with hot water, ignite and weigh.

Determine the percent of total ash and acid-insoluble ash in the sample and find out if it conforms with USP ash
limits.

 USP ash limits – Total Ash – 4%; Acid-Insoluble Ash – 0.5%