Itraconazole STP

YASH PHARMACEUTICALS
Khasra No. 19 M, Village: Raipur, Pargana: Bhagwanpur,Tehsil – Roorkee, Dist: -

Haridwar, Uttarakhand
STANDARD TEST PROCEDURE
Department: Quality Control Page 1 of 5
Title: Itraconazole Pellets 20.0% STP No: YPR/STP/RM/058
Revision No: Nil
Supersedes Version No.:00 Effective Date:
Reference: IHS Review Date:
1. Description: Off-White to cream Spherical pellets.

2. Identification:
A. By UV: The scan the sample and Standard solution as prepared for assay in range between
200 nm to 300nm both the solution maxima should be at about 260nm
3. Dissolution (By UV):

Not less than 75% of the label amount is dissolved in 60 minutes
Dissolution Parameters:
Medium : Simulated gastric fluid (without pepsin)

Volume : 900 ml
Apparatus : Paddle
RPM : 100 rpm
Temperature : 37ºC ± 0.5ºC
Time : 60 minutes
Dissolution medium preparation (Simulated gastric fluid without pepsin)

Weigh and transfer accurately about 2.0 gm of sodium chloride and into 1000 ml volumetric
flask. Add about 500ml of water. Shake it to dissolve. Add 7.0 ml concentrated Hydrochloric
acid and adjust the pH of the solution to 1.2 with HCl. Make up the volume up to 1000 ml with
water.
Blank Preparation: Dilute 5ml of methanol to 50 ml with Dissolution medium.
Standard Preparation: Weigh and transfer accurately equivalent to 22.2mg of itraconazole
working standard into 200ml volumetric flask. Add 80ml of methanol dissolve and dilute up to
200 ml with methanol. Mix thoroughly and dilute 5 ml of this solution to 50 ml with dissolution
medium.
Sample preparation: Separately weigh accurately about 500 mg pellets of drug (equivalent to
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Format No.: - YPR/QC/081/F02-00
Revision No: Nil
100 mg itraconazole) and transfer to separate dissolution vessel containing 900ml dissolution
medium, previously adjusted to 37 ± 0.5°C and rotate the paddle at 100 RPM for 60 minutes.
After 60 minutes filter the solution through whatman no.1 filter paper. Dilute 5ml of filter to 50
ml with dissolution medium.
Procedure: Measure the absorption of the sample and standard preparation at 255nm using blank
preparation for zero correction on a suitable spectrophotometer
Calculation: Calculate the amount of intraconazole dissolved from each sample, in % on assay
by using the formula:
At Ws 5 900 50 100 P
Dissolution % = ----------x----------x---------x-----------x---------x-------x-------x 100
As 200 50 Wt 5 20 100
Where,
At =Absorbance due to intraconazole in sample preparation.
As= Absorbance due to intraconazole in buffer standard preparation.
Ws=Weight of intraconazole working standard taken in mg.
Wt= Weight of intraconazole sample taken in mg
P= Potency of intraconazole working standard used.
4. Water:
Determined on 0.2 g of sample by karl fischer Titrator method.
Start Karl fischer Titrator apparatus, neutralize the glass bottle with karl fischer reagent,
which will be completely free from moisture.
Determination of water factor: Weigh accurately 50 mg of water & transfer it into moisture
free glass bottle, containing magnetic stirrer & start the instrument. Note the karl fischer
reagent consumed to neutralised the water which is automatically stopped the consumption of
reagent.
Calculation:
Wt. of water in mg
Factor of water = -------------------------------------
Vol. of karl fischer consumed in ml
Factor =……………

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Determination of water in sample: Weigh accurately about 5.0 g of sample, transfer it into
glass bottle containing magnetic stirrer then start the instrument. Note the Karl Fischer
reagent consumed to neutralize the substance.
Calculation:
Vol. of karl fischer reagent consumed X Factor of water X 100

Water =---------------------------------------------------------------------------
Wt. of sample in mg
Water = …………. %
5. Related Substance by HPLC: High performance liquid chromatograph equipped with variable
wavelength detector and integrator.
Column : Inertsil ODS-3 or equivalent column, 250mm x 4.6mm, 5 microns

Wave length : 260nm
Flow rate : 1.5ml/min
Injection volume : 20µl
Temperature : Ambient
Run time: 30 minutes
Mobile Phase: Mix acetonitrile and water in ratio of 70: 30 and degas it with ultrasonic bath.
Placebo Preparation: Crush the 5.0g dummy placebo in to fine powder and weigh accurately pellets
equivalent to half x average net content and transfer it into 100ml volumetric flask, add 70ml of
methanol, shake it mechanically for 10 minutes, sonicate it for 20minutes and mark up the volume with
methanol to 100ml. filter the above solution through 0.45µ filter.
Sample Preparation: Crush the pellets into the powder and weigh accurately about 250mg pellets
(equivalent to about 50mg of Itraconazole) and transfer it into 100ml volumetric flask add 70ml of
methanol, shake it mechanically for 10 minutes, sonicate it for 20 minutes and make up the volume with
methanol to 100ml. filter the above solution through 0.45µ filter.
Procedure for Injection: Separately inject about 20µl of methanol, placebo preparation and five
replicate injections of sample preparation and calculate the system suitability parameter and inject

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duplicate smaple preparation into the equilibrated HPLC system and record the response of the major
peaks.
System suitability: Relative standard deviation for Itraconazole area of sample solution should be not
more than 2.0%. Resolution coefficient between active ingredient (Itraconazole) and nearest impurity
should be not less than 1.2. The tailing factor for Itraconazole peak should not be more than 2.0.
Calculation:
1. Disregard any peak obtained in sample solution due to the mobile phase, methanol and placebo
preparation.
2. In the chromatogram obtained with the sample solution, the area of any individual peak, apart from
the principal peak should not be more than 0.2%.
3. Sum of area of all peaks apart from the principal peak should not be more than 1.0%.
Maximum individual impurity area

Maximum individual impurity in % = ------------------------------------------------- x 100
Total area
Total impurities area

Total impurities in % =-------------------------------- x 100
Total area
6. Assay: By UV: (For itraconazole pellets equivelent to Itraconazole)
0.1M Methanolic Hydrochloride Acid
Dilute 8.5 ml of Hydrochloric acid to 1000 ml with methanol.
Test Solution:
Weigh accurately about 100 mg pellets (equivalent to about 20mg of Itraconazole) and transfer into a
100 ml volumetric flask. Add 70ml of 0.1 M Methanolic hydrochloric acid sonicate for 20 minutes,
dilute up to 100 ml with 0.1 M methanolic hydrochloric acid. Mix thoroughly and filter, Discard first 20
ml of the filtrates, dilute 2 ml of the filtrates to 50 ml with 0.1 M methanolic hydrochloric acid and mix.

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Standard solution:
Weigh and transfer about 20mg Itraconazole working standard in 100 ml volumetric flask. Dissolve in
70 ml of 0.1 M Methanolic hydrochloric acid, dilute up to 100 ml with 0.1 M methanolic hydrochloric
acid and mix. Further dilute 2ml of this solution to 50ml with 0.1 M methanolic hydrochloric acid and
mix.
Procedure:
Measure the absorbance of test and standard at the maximum at about 260nm using
methanol to set blank on a suitable spectrophotometer. Calculate the assay using
formula.
Calculation:
Calculate the amount of Itraconazole present in pellets, in % using the following
formula:
At Ws 2 100 50
----- x ---------x----------x----------x------------x Potancy
As 100 50 Wt 2
Where,
At = Absorbance due to Itraconazole in sample preparation
As = Absorbance due to Itraconazole standard preparation
Ws = Weight of Itraconazole working standard taken in mg
Wt = Weight of Itraconazole sample taken in mg
P = Potency of Itraconazole working standard used

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Itraconazole STP

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YASH PHARMACEUTICALS

Khasra No. 19 M, Village: Raipur, Pargana: Bhagwanpur,Tehsil – Roorkee, Dist: -

Reference: IHS Review Date:

1. Description: Off-White to cream Spherical pellets.

3. Dissolution (By UV):

Medium : Simulated gastric fluid (without pepsin)

Dissolution medium preparation (Simulated gastric fluid without pepsin)

Prepared by Checked by Approved by

Reference: IHS Review Date:

Prepared by Checked by Approved by

Reference: IHS Review Date:

Vol. of karl fischer reagent consumed X Factor of water X 100

Column : Inertsil ODS-3 or equivalent column, 250mm x 4.6mm, 5 microns

Prepared by Checked by Approved by

Reference: IHS Review Date:

Maximum individual impurity area

Total impurities area

6. Assay: By UV: (For itraconazole pellets equivelent to Itraconazole)

0.1M Methanolic Hydrochloride Acid

Dilute 8.5 ml of Hydrochloric acid to 1000 ml with methanol.

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Reference: IHS Review Date:

Prepared by Checked by Approved by

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