YASH PHARMACEUTICALS

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

Haridwar, Uttarakhand
STANDARD TEST PROCEDURE
Department: Quality Control Page 1 of 4
Title: Itraconazole Pellets 40.0% STP No: YPR/STP/RM/279
Revision No: Nil
Supersedes Version No.:00 Effective Date:

Reference: IHS Review Date:

1. Description: An off white to beige color spherical pellets.

2. Identification:
A. By UV: The scan the sample and Standard solution as prepared for assay in range between
230 nm to 400 nm 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 111.0 mg pellets 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 250 mg pellets of drug (equivalent to

Prepared by Checked by Approved by

Name
Designation
Sign. & Date
Format No.: - YPR/QC/081/F02-00
 YASH PHARMACEUTICALS
Khasra No. 19 M, Village: Raipur, Pargana: Bhagwanpur,Tehsil – Roorkee, Dist: -
Haridwar, Uttarakhand
STANDARD TEST PROCEDURE
Department: Quality Control Page 2 of 4
Title: Itraconazole Pellets 40.0% STP No: YPR/STP/RM/279
Revision No: Nil
Supersedes Version No.:00 Effective Date:

Reference: IHS Review Date:

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 40 100

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.
Limit: Not less than75% in 60 min

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 =……………
Prepared by Checked by Approved by
Name
Designation
Sign. & Date
Format No.: - YPR/QC/081/F02-00
 YASH PHARMACEUTICALS
Khasra No. 19 M, Village: Raipur, Pargana: Bhagwanpur,Tehsil – Roorkee, Dist: -
Haridwar, Uttarakhand
STANDARD TEST PROCEDURE
Department: Quality Control Page 3 of 4
Title: Itraconazole Pellets 40.0% STP No: YPR/STP/RM/279
Revision No: Nil
Supersedes Version No.:00 Effective Date:

Reference: IHS Review Date:

Determination of water in sample: Weigh accurately about 200 mg 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. 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 50mg 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.
Standard solution:
Weigh and transfer about 100 mg pellets equivalent to 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
Prepared by Checked by Approved by
Name
Designation
Sign. & Date
Format No.: - YPR/QC/081/F02-00
 YASH PHARMACEUTICALS
Khasra No. 19 M, Village: Raipur, Pargana: Bhagwanpur,Tehsil – Roorkee, Dist: -
Haridwar, Uttarakhand
STANDARD TEST PROCEDURE
Department: Quality Control Page 4 of 4
Title: Itraconazole Pellets 40.0% STP No: YPR/STP/RM/279
Revision No: Nil
Supersedes Version No.:00 Effective Date:

Reference: IHS Review Date:

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
Limit : Not less than 36.0% and not more than 44.0%

Prepared by Checked by Approved by

Name
Designation
Sign. & Date
Format No.: - YPR/QC/081/F02-00