Phase solubility analysisssss
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Transcript of Phase solubility analysisssss
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PHASE SOLUBILITY ANALYSIS
Presented byB.N.S.SAILAKSHMIM.Pharmacy(pharmaceutics)
SRI PADMAVATHI MAHILA VISWAVIDYALAYAM TIRUPATHI
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STANDARD METHOD
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GRAPHICAL REPRESENTATION
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Solvent charecterstics:
Sufficient volatility
Boiling point b/w 60 – 150 c⁰
Not react with test substance
Not form solvates or salts
Pure in nature
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APPARATUS CONSTANT
TEMPERATURE BATH– Contain horizontal
shaft(25rpm)– Temp with in +/- 0.1 c⁰– Vibrator(100-120/sec)
AMPULE
- 15 ml ampules SOLUBILITY FLASK
15ml
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Increased amount of sample
5ml solvent
Cool in dry acetone Double jet air gas burner
Weigh all ampoules
PROCEDURESYSTEM COMPOSITION
15 ml 15 ml15 ml 15 ml
15 ml 15 ml 15 ml15 ml
weigh
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Calculate the system composition,in mg per g,for each ampule by the formula:-
1000(W 2 –W 1) / (W 3-W 2)
in which W 2 = wt.of ampule plus test substance,
W 1 =wt.of empty ampule,
W 3 =wt.of ampule plus test substance,solvent.
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EQUILIBRATION
Varies with Substance Method of mixing Temperature
DETERMINATION OF EQUILIBRATION:
∆ 40⁰ c
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SOLUTION COMPOSITION
Content settles
Ampoule(F1)Water bath
Transfer 2ml Solution
Solubility flask(weight F2)
Dry residue(F3)
Open ampule
Evaporate vacuumcool
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CALCULATIONS
System composition in mg/gm for each ampoule =1000(w2-w1)/(w3-w2)
Solution composition in mg/gm for each ampoule = 1000(F3-F1)/(F2-F3)
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Along DE- saturated with
main compound
Point E- Saturated in both
compound and impurity
The rise of the curve along
the segment DE- Wt of the
impurity per unit wt of the
sample.
%Purity by weight = (1-
Slope of segment DE) * 100%
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Point C- Sum of the solubilities
of the substance and the
impurity
Ponit b- solubility of the pure
substance
Solubility of the substance= b/
Solvent Volume
Solubility of the impurity= c-b/
Solvent Volume
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Additional
impurities-
Additional
breaks or as
deviation of the
initial slope
from 1.0Insoluble or
volatile
impurity-
Initial slope will
become less
than 1
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PURIFICATION TECHNIQUE
Test specimen Non reactive solvent 10% material dissolved seal & shake room temperature,24hr
Mother liquor Residue , Rince,dry
Impurity residue Pure reference
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CONCLUSIONSolubility is an important factor in pharmaceutical
process.Phase solubility analysis is an important process for
Detection of impuritiesPreparation of reference substanceSeparation of optical isomers.
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