COLLEGE OF PHARMACY
Valenzuela. Quezon City. Antipolo. Pampanga. Cabanatuan. Laguna
Pharmaceutical
Analysis 1
UNIT 14
Name of Instructor
College of Pharmacy
COURSE FACILITATOR DATE:
EXTRACTIVE AND
CRUDE FIBER
CONTENT
Objectives
❖ Explain the principles and methods of the
different special methods of analysis
❖ Applying special methods in the analysis of
natural product
❖ Assessing product conformance to standards and
specifications
OUTLINE
1. Extractive and Crude Fiber Content
-Preparation of Extract
- Alcohol / Water- Soluble Extractives
2. Crude Fiber Content
3. Extraction of Alkaloids
4. Practice Problems
Extractive and Crude
Fiber Content
Extractives
❖ Product of extraction procedure
❖ The amount of extractives, which a drug yields to
a given solvent, is a measure of the amount of
certain constituents or group of related
constituents, which the drug contains.
Extractives
❖ It is important that the solvent used will not
dissolve appreciable quantities of substances
other than those sought in the extraction.
❖ In some cases, the amount of drug soluble in
a given solvent is an index of its purity, e.g. acacia
must yield not more than 1% water
insoluble residue to meet the official
requirement.
❖ % extract (solvent-soluble residue)
❖ % insoluble residue
Properties of good
solvent
❖ Low toxicity
❖ Ease of evaporation
❖ Rapid physiologic absorption of the extract
❖ Preservative action
❖ Inert – inability to cause complex
Preparation of Extract
❖ EXTRACTION METHODS
❖ MACERATION
❖ PERCOLATION
❖ DIGESTION
❖ INFUSION
❖ DECOCTION
❖ ENFLEURAGE
❖ CONTINUOUS EXTRACTION
Extraction Procedure
❖ The Soxhlet apparatus is generally used for
extraction with volatile solvents where small
quantities of a drug are extracted.
Soxhlet apparatus
❖ The percentage of extractives in the drug is
calculated from the weight of the residue.
% extractive = wt of residue x 100
wt of sx
% insoluble residue=wt of sx in the thimble after
drying x 100
wt of sx
Alcohol Soluble
Extractives
❖ Solvent used for resinous matter is alcohol
❖ Determination of the alcohol-soluble extractive is
frequently employed to determine approximately
the amount of resin in those drugs in which
resinous matter is the important constituent.
❖ Extraction is done using Soxhlet apparatus and
the insoluble residue is collected dried and
weighed
❖ Alc. Sol Extract = wt of moisture-free drug
- wt of insoluble residue
Water-Soluble
Extractives
❖ The determination of water-soluble extractives is
applied to drugs containing one or more
important constituents which are soluble in
water e.g. aloe.
❖ The determination is performed in the same way
as in the determination of diluted alcohol
extractives.
❖ Extraction is performed by maceration and
residue after drying to constant weight is
determined
❖ Water sol. Extract = wt of residue after
Other Solvents
Hexane – for fats and fixed oils, extraction is by
continuous extraction
Ether – for resins, fixed oils, coloring matter and
crude fiber, extraction is by continuous extraction
Crude Fiber Content
❖ 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.
❖ Frequently, this material is the outer cellulose
layer or protective coating which contains a
larger proportion of lignified tissues.
❖ The determination of the crude fiber content of
food and animal feed is mandatory worldwide,
this determines the presence of adulterants
which are also the crude fiber or the plant wastes
Determination of the
Crude Fiber Content
❖ Solvent exhausted sample (THIMBLE)
❖ Add 200 mL of 1.25% boiling sulfuric acid
solution, boil for 30 minutes.
❖ Filter and wash the residue
❖ Rinse the residue back into the flask with 200 mL
of boiling sodium hydroxide solution adjusted to
exactly 1.25%. Again heat the mixture to boiling
and continue the boiling for exactly 30 minutes
Determination of the
Crude Fiber Content
❖ Then filter through a linen or hardened-paper filter
and wash the residue on the filter with boiling water
until no longer acid.
❖ Rinse the residue back into the flask with 200 mL of
boiling sodium hydroxide solution adjusted to exactly
1.25%. Again heat the mixture to boiling and continue
the boiling for exactly 30 minutes.
❖ Under the reflux condenser wash the residue with
boiling water until the last washing is neutral, dry it at
110°C until of constant weight and note the weight.
❖ Incinerate the dried residue and weigh the ash.
Notes:
❖ The sample is exhausted with ether to remove fats and waxes which
tend to prevent the penetration of the acid and alkali solution into the
drug particles.
❖ To prepare 1.25% sulfuric acid, dilute exactly 51 mL of 1-N H2SO4 to 200
mL.
❖ To prepare 1.25% sodium hydroxide, dilute 70 mL of 1-N NaOH to
exactly 200 mL.
❖ The dried residue after boiling with acid and alkali solution consists
chiefly of cellulose and small amounts of hemicellulose, pentoses,
inorganic matter, etc.
❖ The weight of the ash subtracted from the weight of the residue gives
the weight of crude fiber.
❖ The crude fiber limit for cocoa is 7% of ether-insoluble residue.
❖ A cocoa sample with weight of 10.265g was place in a tared
thimble and extracted with ether for 5 hours using
continuous extraction method. The ff. are the data
collected:
Wt of insoluble
Wt of tared thimble 0.9285 g residue
Wt of sample and thimble
After extraction 5.0092 g
Wt of empty dish 38.9966 g Wt of extract
Wt of dried residue and
dish after drying over H2SO4 41.9875 g
Wt of residue after treatment
with acid and alkali 2.1872 g %CF = wt CF
wt of insol residue
Wt of residue after incineration 1.9016 g
%CF = 7%
If cocoa should contain 40-55% extractives and nmt 7% crude
fiber content, does the sample meet the specifications?
Extraction of Alkaloids
❖ Alkaloids may be defined as chemical substances
which (1) are obtained from plant, animal or
synthetic sources (2) contain organic nitrogen(s)
within their chemical structures and (3) usually
possess physiological activity.
Physical Property
(Solubility)
❖ Alkaloids (R3N) are sparingly soluble in water but
readily soluble in most organic solvents
immiscible in water such as ether, chloroform
(CHCl3) and carbon tetrachloride (CCl4).
❖ Alkaloidal salts (R3+NHCl-) are readily soluble in
water and sparingly soluble in immiscible
solvents.
Chemical Properties
❖ Alkaloids combine directly with acids to form salts that are usually
soluble in water but insoluble in certain organic solvents.
R3N + HCl R3+NHCl- (water soluble)
❖ Alkaloids are liberated from aqueous solutions of their salts by
alkalies.
R3+NHCl- + NaOH R3N + NaCl + H2O
(soluble in organic solvents)
❖ Alkaloids form highly insoluble precipitates with a considerable
number of reagents especially with the salts of some heavy metals
such as mercury, gold and platinum.
Alkaloidal Test
❖
Solutions
Mercuric Iodide TS – commonly known as Valser’s Reagent
is prepared by slowly adding 10% solution of potassium
iodide to red mercuric iodide until almost all the red
mercuric iodide is dissolved. The excess mercuric iodide is
then removed by filtration. This reagent forms a white
precipitate.
❖ Iodine TS – commonly known as Wagner’s Reagent is a
solution containing iodine and potassium iodide dissolved
in distilled water. A 0.1-N Iodine solution may be employed.
Wagner’s Reagent yields a reddish or red-brown
precipitate.
❖ Mercuric Potassium Iodide – Mayer’s Reagent, is a solution
of 1.358g of mercuric chloride in 60 ml of water with 5 g of
KI in 10 ml of water and the mixture diluted to 100 ml. This
reagents gives white or slightly yellow precipitates with
dilute solution of alkaloids
Extraction of Alkaloids
Practice problems
1. Determine % w/w of alkaloids in belladonna leaf if
15.00ml of 0.0210N sulfuric acid was added to the
extracted alkaloids and 7.30 ml of 0.0198N NaOH
for the residual titration. The weight of the
powder of belladonna leaf was 1.021g. Each ml of
0.02 N sulfuric acid is equivalent to 5.788 mg of
hyoscyamine.
2. Calculate the %w/w aminophylline if 0.3120 g
sample , assayed following the procedure given,
required 12.10ml of 0.1100N NH4SCN to bring
about the endpoint in the residual titration of
silver nitrate. Exactly 20ml of 0.1200N AgNO3 was
taken initially.
The titer value for 1 ml of 0.1N AgNO3 is 21.02 mg
aminophylline.
Practice Problems
3. 20 tablets of codeine sulfate (3/4 grain)
weighing 1.66 gram. An aliquot portion
weighing 0.5589 g was extracted with
chloroform and the extract was evaporated
and dried at 100°C for 2 hours leaving a
residue which weighed 0.305 g. Compute for
the percent labeled amount.
Ave wt of tab = 1.66g/20
labeled amount = ¾ gr
% purity = % assay = wt of residue/wt of
sample x 100
4. The weight of 25 tablets of morphine
sulfate (150 mg) is 3.075 g. If 0.3075 g
was used in the assay and it required
10.3 ml of 0.023N NaOH to back titrate
25 ml of 0.021N H2SO4. Calculate the
percent labeled amount of morphine
sulfate. Each ml of 1N H2SO4 is
equivalent to 758.83 mg of morphone sulfate.
5. What would be the volume of 0.02N
H2SO4 needed to titrate 100 ml of
paregoric if the sample contains 0.035
g of morphine. Each ml of 0.02N
H2SO4 is equivalent to 28.53 mg of
morphine.
Related Links
Determination of Crude Fiber Content
❖ https://www.youtube.com/watch?v=p1a3kctJuIs
References
TEXTBOOK: Knevel, A.M. and Digangi, F.E., Jenkin’s Quantitative Pharmaceutical
Chemistry.USA: Mc Graw Hill. 1977.
REFERENCES:
• Watson, David G. Pharmaceuticals analysis: a textbook for pharmacy students and
pharmaceutical chemists, 4th ed. Singapore: Elsevier. 2017.
• Remington’s Pharmaceutical Sciences, (2013) Philadelphia: Lippincott William
and Wilkin
• WHO Expert Committee on Specifications for Pharmaceutical Preparations .
Geneva: World Health
• British Pharmacopeia . 2017.
• The United States Pharmacopeia(USP 40) : NF 35: The National Formulary
.Rockville, Md.: United States Pharmacopeial Convention. 2017.
• Handbook of Modern Pharmaceutical Analysis (2011) Amsterdam; Boston:
Academic Press/Elsevier
• Harris, D.C., Quantitative Chemical Analysis, 9th ed. New York :
W.H. Freeman. 2015
ANY
QUESTIONS?
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OLFUValenzuelaPharmacy/ (8)-661-3023 loc. 106
