special methods of drug analysis

8/12/2019 Special Methods of Drug Analysis

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550-7000C Diluted HCl

(SILICA)

(TOTAL

INORGANIC

SALTS)


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Weigh accurately 10g of drug

Dry in an oven at 1050C for 5 hours

Cool to room temperature

Weigh until constant weight


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loss on drying% Moisture = ------------------ x 100

wt. of sample

wt. before wt. after% Moisture = ---------------------------- x 100

wt. of sample


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(wt. before wt. after) wt. of ether-soluble

extractives

% Moisture = -------------------------------------------------------- x 100

wt. of sample


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volume of water in mL% Moisture = ----------------------------- x 100

wt. of sample


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Place methanol in flask

Titrate with KF reagent until endpoint

(canary yellow)

Add weighed

Titrate with KF reagent to final endpoint


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F =

F=


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F =

F=

weight of water

% Moisture = ----------------------------- x 100wt. of sample

F x mL of KF reagent

% Moisture = ------------------------------ x 100wt. of sample in mg


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spontaneous

evaporation oven-drying


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Macerate 2gof drug in

70mL diluted

alcohol

Shake mixtureduring 8hrs at

30-minute

interval

Stand for16hrs without

shaking

Filter and wash

residue to make

100-mL filtrate

Evaporate50-mL aliquot

portion filtrate

to dryness in

water bath

Dry to

constant

weight at

1000C in oven


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Treat accurately

weighed sample in

ether

Treatment with

boiling acid

Filter through

ashless filter

paper

Weigh residue

and incinerate

using dull red heat

Dry residue

and weigh

Treatment with

boiling alkali


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Weigh accurately 5g of oil or fat

Add alc.KOH and heat under reflux condenser

Evaporate alcohol and dissolve residue

in water, then extract with ether

Dry the residue and weigh until

constant weight


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weight of residue

% Unsaponifiable = --------------------------- x 100

Matter wt. of sample


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Weigh accurately

200 mg of oil

sample

Add 20mL of CCl4,

then 25.0mL of ICl

Add 20mL KI and 100mL

recently boiled & cooled

water

Titrate liberated I2with std.

Na2S2O3 to disappearance

of blue color

Perform blank

test

Stopper, shake occasionally

and stand for 30mins

protected from light


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Weigh accurately

2g of fatty

alcohol sample

Add 2.0mL of

pyridine and 10mL

of toluene

Add 25mL distilled water,

stopper and shake

vigorously, then allow to

stand

Titrate CH3COOH formed

with std. NaOH to light pinkcolor using Pp as indicator

Perform blanktest

Add 10.0mL of CH3COCl,

then stopper flask and heat

in water bath for 20mins.


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Oil Sample(free alcohol +

alcohol as ester)

Oil Sample(alcohols in

ester form)

acetylation saponification Determine SVof acetylized

product


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Pipet oil

sample

into an EF

Run down

50.0mL of

Hydroxylamine

HCl

Stand for

10mins.,

then add

indicator

Titrate

with std.

NaOH to

endpoint

Perform

blank test


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Pipetspirit into

an EF

Add 1mL

kerosene

Add acidified

saturated CaCl2solution and

rotate bottle

vigorously

Add

sufficientCaCl2soln

to bring oil

to neck

Take the

reading


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weight of residue

% Alkaloid = --------------------------- x 100wt. of sample

* Indicator used is methyl red.


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TYPES OF ANALYSIS

1. Proximate analysis

- determination of the amount of a class of

compound present in given sample

Example: alkaloids

2. Ultimate analysis

- determination of the amount of a specific

component of the given sample

Example: morphine

special methods of drug analysis

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