102 Protole 20mg Cap

P r o u d t o b e P a k i s t a n i
Global Pharmaceutical (Pvt.) Ltd.

ANALYTICAL CONTROL Document # Revision Effective Date Next Review On
PROCEDURE GL/SAP/P/102 No.03 30-Aug-2016 29-Aug-2019
Page #
Protole Capsules 20mg Copy # 01
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Author: Reviewed By: Approved By:
Asst. Manager Signature Dy. QC Manager Signature Quality Control Manager Signature
Naeem Qamar Shahbaz Daood Sohail Aslam
Registration No. 024750 Shelf Life: 02 Years
Reference: U.S.P. 39
Composition:
Each capsule contains:
Enteric coated pellets of
Omeprazole…….……….……20mg
(U.S.P. Specs.)
1. PRODUCT SPECIFICATIONS:
S# Parameters Final Mix Filled Capsules

Off white to pale yellow
01. Appearance NA spherical pellets filled in
empty hard gelatin capsules.
02. Cap Color NA Blue colored cap
03. Body color NA White colored body
04. Capsule size NA #2

240.0mg ± 10.0%
05. Uniformity of Mass NA
(216.0 – 264.0)
06. Uniformity of dosage Units NA Meets the requirements
Dissolution (Acid Stage) NA NMT 10 % after 2 hr.

07.
NLT 80 % after 45 min.
Dissolution (Buffer Stage) NA
(Q+5%)
08. Identification NA Must Comply
09. Assay (Omeprazole) NA 90.0% to 110.0%
A. ANALYTICAL PROCEDURE: Filled Capsules
Copyright: This Document is the exclusive property of Global Pharmaceutical. And its contents must not be Communicated to
unauthorized persons, or persons outside the company without written consent of Management.
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A1.Appearance:
Off white to pale yellow spherical pellets filled in empty hard gelatin capsules.
A2.Cap Color:
Blue colored Cap (As per Standard)
A3.Cap Color:
White colored Body (As per Standard)
A4.Capsule size:
#: 2
A5.Uniformity of Mass :( Weight variation)
Weigh 20 Capsules and calculate the average weight as:

Average weight = Weight of 20 Capsules
20
Weigh all these Capsules individually and mark among these weights maximum (W Max) & minimum (WMin) weight
Capsules. Calculate the maximum and minimum variation in percent as:
Maximum% age variation =(WMax) – (WAvg.) x 100

(WAvg.)
Minimum %age variation =(WMin) – (WAvg.) x 100
WAvg.)
Limit: ± 7.5% (Opt. Limit)
A6.Uniformity of dosage Unit :

Select not fewer than 30 capsules. Accurately weigh 10 capsules individually. Calculate the active substance,
expressed as percentage of label claim of each capsule as described in assay. Calculate the Acceptance value
(AV).
Calculation of Acceptance Value

Calculate the Acceptance Value (AV) using the formula:
AV = [M – X] + ks
in which the terms are as defined in table
Variable Definition
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X Mean of individual contents (% label claim)

x1, x2,...,xi Individual estimated contents of the units tested. Where x1 = w 1 x A/W, here A is
contents of drug substance (5age of label claim), determined as described in
Assay and W is mean of individual weights of units used in the Assay.
W1, w2, ………wn Individual weights of the units tested for weight variations
n Sample size (number of units in a sample)
k Acceptability constant if n = 10, then k = 2.4 if n = 30, then k = 2.0
s Sample standard deviation
T Target test sample amount at time of manufacturer (T = 100.0% unless otherwise
specified in the individual monograph)
M Reference value; M (case 1), T < 101.5% or M (case 2), T > 101.5%
Case 1
If 98.5% < X < 101.5, then M = X , If X < 98.5%, then M = 98.5% If X > 101.5, then
M = 101.5%
Case 2
If 98.5% < X < T then M = X, If X < 98.5% then M = 98.5%, If X > T, then M = T%
AV Acceptance value; AV = | M-X |+ks
L1 Maximum allowed acceptance value (L1 = 15.0 unless otherwise specified in the
individual monograph)
L2 Maximum allowed range for deviation of each dosage unit tested from the
calculated value of M (L2 = 25.0 unless otherwise specified in the individual
monograph)
CRITERIA
Apply the following criteria, unless otherwise specified.
The requirements for dosage uniformity are met if the acceptance value of the first 10 dosage units is less than or
equal to L1. If the acceptance value is greater than L1, test the next 20 dosage units and calculate the
acceptance value. The requirements are met if the final acceptance value of the 30 dosage units is less than or
equal to L1 and no individual content of the dosage unit is less than (1 - L2 × 0.01) M nor more than (1 + L2 ×
0.01) M in calculation of acceptance value under content uniformity or under mass variation. Unless otherwise
specified, L1 is 15.0 and L2 is 25.0
A7. Dissolution:
Acid resistance Stage:
Medium : 0.1N Hydrochloric acid, 900ml
Apparatus1 :100rpm,
Time :02 hours.
Sample Solution: After 2 h, take about 50ml of sample and filter through a nylon filter of 0.2-µm pore size.
Standard Solution: Take omeprazole working standard equivalent to 22.2mg of omeprazole in 100ml volumetric
flask and make up volume with 0.1M NaOH. Sonicate to dissolve and dilute 5ml to 50ml with 0.1M HCl. Filter
through a nylon filter of 0.2-µm pore size.
Analysis: Note the absorbance of sample and standard solution on UV spectrophotometer at 305nm using
0.1MHCl as blank.
Calculations = (Rs/Ru)x(Cu/Cs)x100
Cs= Concentration sample solution.
Cu= Concentration standard solution
Rs= Absorbance of sample from the sample solution
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Ru= Absorbance of standard from the standard solution.
Tolerance: the average of the 6 units is NMT 10 % of omeprazole dissolved.
Buffer Stage:
Medium : 0.05M pH6.8 phosphate buffer, 900ml
Apparatus1 :100rpm,
Time :45 min.
Analysis : Proceed as directed for acid resistance stage with a new set of capsules from the same
batch. After 2 hrs, replace the acid medium with buffer medium, and continue the test for 45min. determine the
amount of omeprazole dissolved from UV Absorbance at the wavelength of maximum absorbance at about
305nm on portion of solutions under test passed through a nylon filter of 0.2-µm pore size, in comparison with
standard solution having same concentration as that of sample of Omeprazole in same medium.
Tolerance: NLT 80% (Q+5%) is dissolved.
A8.Identification (Omeprazole):
By HPLC
The principal peak in the chromatogram obtained with the test solution is similar in retention time and size to the
principal peak in the chromatogram obtained with reference solution.
A9.Assay(HPLC) :
Chromatographic system:
Column :4.0-mm × 15-cm, 5 µm, based-deactivated packing L7.
Lambda max. : 305nm
Flow Rate :1.2ml/min.
Temp. :Ambient
Injection :10µL
Procedure:
Solution A:
Dissolve 6.0g of glyceine in 1500ml of water, adjust with 50% sodium hydroxide solution to a pH: 9.0 and dilute
with water to 2000ml.
Solution B:
Acetonitrile and Methanol (85:15)
Diluent:
Dissolve 7.6g of sodium borate decahydrate in about 800ml of water. Add 1.0g of edentate disodium, and adjust
with 50% sodium hydroxide solution to a pH: 11.0± 0.1. Transfer the solution to a 2000ml volumetric flask, and
400ml of dehydrated alcohol and dilute with water to volume.
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Mobile phase:
See Table
Time (min.) Solution A (%) Solution B (%)
0 88 12
20 40 60
21 88 12
25 88 12
Standard Solution:
0.2mg /ml of Omeprazole (Standard) in diluent, using sonication if necessary.
Sample Solution:
Weigh and mix the contents of NLT 20 capsules. Transfer an accurately weighted portion of the capsule content,
equivalent to 20mg of Omeprazole, to a 100ml volumetric flask, and add about 50ml of diluent and sonicate for 15
min. cool and dilute with diluent to volume, mix and pass through a membrane filter 0.45µm or fine pore size.
Procedure: Separately inject equal volumes (about 10 µL) of the Standard solution, the sample solution into the
chromatograph, record the chromatograms, and measure the responses for the major peaks.
Calculations:
%age Assay: = Area of Sample X Concentration of Reference X Potency of Standard
Area of Reference X Concentration of Sample
(Limit: 90.0%- 110.0 %)
A10. Assay: (By UV spectrophotometer Alternate method)
Sample Preparation:
Transfer crushed pellets equivalent to 20 mg of Omeprazole to a 100 ml volumetric flask. Dissolve it in 60ml of
0.1N NaOH. Make volume up to mark with the same solvent. Sonicate for 15 minutes. Filter through 0.2 micron
nylon filter and dilute 5 ml of solution to 100 ml with 0.1NaOH.
Standard Preparation:
Accurately weigh working standard equivalent to 100 mg of Omeprazole and transfer it to 100 ml volumetric flask.
Dissolve it in 60ml of 0.1N NaOH and make volume up to mark. Sonicate for 15 minutes. Filter through 0.2 micron
nylon filter. Dilute 1 ml of solution to 100 ml with 0.1N NaOH.
Measure the absorbance of both sample and standard solution at U.V Visible spectrophotometer at 305 nm.
Calculations:
Assay %age = (AU/ AS) x (CS/CU) x 100
AU = Absorbance of the Sample preparation

AS = Absorbance of the Standard preparation
CS = Concentration of Omeprazole in the Standard preparation (mg/mL)
CU = Concentration of Omeprazole in the Sample preparation (mg/mL)
(Limit: 90.0%- 110.0 %)
2.0 AMENDMENT HISTORY
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Initiated Page
Rev.# Date Nature of Amendment Done By
by #
03 30.08.2016 D.Q.C.M. All Reviewed according to USP 39 M.R.

102 Protole 20mg Cap

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102 Protole 20mg Cap

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Copyright:

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P r o u d t o b e P a k i s t a n i

Global Pharmaceutical (Pvt.) Ltd.

Author: Reviewed By: Approved By:

Registration No. 024750 Shelf Life: 02 Years

Each capsule contains:

Enteric coated pellets of

S# Parameters Final Mix Filled Capsules

03. Body color NA White colored body

04. Capsule size NA #2

Dissolution (Acid Stage) NA NMT 10 % after 2 hr.

09. Assay (Omeprazole) NA 90.0% to 110.0%

A. ANALYTICAL PROCEDURE: Filled Capsules

A5.Uniformity of Mass :( Weight variation)

Weigh 20 Capsules and calculate the average weight as:

Maximum% age variation =(WMax) – (WAvg.) x 100

Limit: ± 7.5% (Opt. Limit)

A6.Uniformity of dosage Unit :

Calculation of Acceptance Value

in which the terms are as defined in table

X Mean of individual contents (% label claim)

Column :4.0-mm × 15-cm, 5 µm, based-deactivated packing L7.

Lambda max. : 305nm

Flow Rate :1.2ml/min.

with water to 2000ml.

Acetonitrile and Methanol (85:15)

Assay %age = (AU/ AS) x (CS/CU) x 100

AU = Absorbance of the Sample preparation

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