MODULE 6

ASH AND WATER CONTENT

EXTRACTIVE AND CRUDE FIBER

CONTENT DETERMINATION
 Ash content determination
⮚ residue remaining after incineration by
burning the ash content of the drug
⮚ represents inorganic salts of carbonates,
phosphates, silicates of sodium, potassium,
calcium and magnesium.
⮚ Ash value is a criterion to judge the identity
or purity of crude drug
⮚ Different types of ash values are used in
detection of crude drugs
▪ Total ash
▪ Acid-insoluble ash
▪ Water-soluble ash & Sulphated ash
 Ash Value
⮚A high ash value is indicative of :
▪ Contamination
▪ Substitution
▪ Adulteration
▪ Carelessness in preparing the
crude drug for marketing and
manufacturing
 Ash content determination
a. Total ash = the residue remaining after
incineration
= represents inorganic salts

% Total Ash = Weight of Ash x 100

Weight of sample

▪If weight of ash is 0.7 gram

▪Weight of sample 5 grams
▪% Total ash = 0.7/5 x 100
▪=14% total ash value
 Ash content determination
b. Acid-insoluble ash (AIA) = part of the
total ash which is insoluble in diluted HCl
% AIA = wt of AIA x 100
wt sample
▪ if the weight od ash is 0.2 gram
▪ weight of sample 5 grams
▪ % AIA = 0.2/5 x 100

= 4% Acid insoluble ash value

 Ash content determination
c. Water-soluble ash = represents soluble chlorides, alkali and NH4
salts.
▪ Water soluble ash is the difference in weight between total ash
and residue after treatment of total ash with water
▪ Weight of water soluble = weight of total ash – weight of
water insoluble ash
▪ % water soluble ash = Weight of water soluble ash x100
Weight of sample

▪ Weight of total ash = 0.7 gram

▪ Weight of water insoluble ash = 0.3 gram
▪ Weight of water soluble ash = 0.7 g – 0.3 g = 0.4 g
▪ % water soluble ash = 0.4 / 5 x 100 = 8%

d. Sulfated ash = treated with H2SO4

 Substances with Ash Limits
Substance Total Ash, % Acid-insoluble Ash,
%
Acacia 4.0 0.5

Agar 6.5 0.6

Aloe 4.0

Cocoa 8.0 0.4

Glycyrrhiza ----- 2.5

Caraway ------ 1.5

Digitalis 5.0 -------

Rauwolfia serpentina ------ 2.0

Senna ------ 3.0

Approximate temperature
equivalents

Very dull red heat

500 – 550 degrees Celsius

Dull red heat

550 - 700 degrees Celsius
Approximate temperature
equivalents
Bright red heat
800 - 1000 degrees Celsius

Yellow red heat

1000-1200 degrees Celsius

White heat
1200 - 1600 degrees Celsius
Terms to define
Loss on Ignition
• Percentage of test material that is
driven off under the temperature range
of 800 + 25 degrees Celsius
Loss on Drying
• Amount of volatile matter of any kind
that is driven off at 110-120 degrees
Celsius
Terms to define
Ignite to Constant Weight
“Ignition shall be continued at 800 +
25 degrees Celsius unless otherwise
indicated until 2 consecutive weighing
do not differ by more than 0.5 mg/g of
the substance taken; the second
weighing following an additional 15-
minute ignition period.”
Terms to define
Drying to constant weight
“Drying shall be continued at 110-120
degrees Celsius unless otherwise
indicated until 2 consecutive weighing
do not differ by more than 0.5 mg/g of
the substance taken; the second
weighing following an additional hour
of drying.”
Water content determination
•Method I: Titrimetric
•Method II: Azeotropic
•Method III: Gravimetric
Water content determination
METHOD I. Titrimetric Method/
Karl-Fischer Method
• “1 mL of the reagent is equivalent to
approximately 5 milligrams of
water”

Formula:
% water = mL KFR x EF x 100
wt sample (mg)
Karl Fischer Titrator
Contents of KFR
Prevents the
Anhydrous pyridine-sulfur
methanol complex

HYDROIODIC ACID
Iodine
React with water
Sulfur dioxide
SULFUR TRIOXIDE

Prevents reverse
Pyridine reaction
Practice Problem
Calculate the water content of Streptomycin
powder using 3.50 g Sample. The water
equivalence factor, F, of the KF reagent was 4.6
and the volume consumed was 9.2 mL.
Formula:
% water = mL KFR x EF x 100
wt sample (mg)
= 9.2 mL x 4.6 x 100
3,500 mg

answer: 1.21%
Water content determination

METHOD II. Azeotropic Method / Distillation

Method
Solvent: xylene, toluene

% water: mL reading x 100

wt sample
Water content determination

METHOD III. Gravimetric Method/

Drying/Thermal Method
• Method of choice for chemical samples
(1-2 grams), vegetable drugs and
biologics
*The moisture content of a drug may be
- water of hydration
- water in absorbed form
EXTRACTIVE AND CRUDE FIBER
CONTENT
 Extractive and Crude Fiber Content
• Volatile and Nonvolatile Ether-soluble Extractive
- The determination of total ether-soluble constituents is applied to
drugs which contain volatile oils, while the determination of
nonvolatile ether-soluble constituents is applied to drugs having
active constituents associated with volatile matter.

• Alcohol-soluble Extractive
- Alcohol is a good solvent for resinous matter.
- For determination of the amount of resin in drugs in which
resinous matter is the important constituent.
• Solvent Hexane-soluble Extractive
- Solvent hexane is a good solvent for fats and fatty
oils.

- The hexane extractive is an index to the amount of

fat present and serves as a check on the amount of
seeds contained in colocynth pulps, the seeds
contain a large amount of fatty matter.

• Crude Fiber
- The crude fiber content of a drug is the residue,
consisting chiefly of cellulose that remains
undissolved after successive treatment with boiling
acid and alkali.
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