Both UV and HPLC methods are commonly used to test Rabeprazole sodium tablets for their active ingredient content. These methods are reliable, accurate, and precise, and are widely accepted by regulatory authorities. Rabeprazole sodium Tablet Complete Testing Procedure (SOP)
PURPOSE:
To describe the procedure for analysis at in-process and finished stage of Rabeprazole sodium 20mg Tablet.
SCOPE:
This SAP gives a detailed outline for the finished product analysis of Rabeprazole sodium 20 mg Tablets and will cover In process testing activities on a physical, chemical & instrumental basis.
RESPONSIBILITY:
QC Analyst is responsible for physical / chemical testing and preparing standard analytical procedure.
It is the responsibility of QC Manager to assist and ensure Testing Procedure as per SAP and to make certain that this SAP is followed in its entirety, reviewed regularly and revised as necessary.
REFERENCE:
INNOVATORS SPECIFICATIONS
MATERIAL AND EQIUPMENT:
- UV Spectrophotometer
- Dissolution apparatus
- Friability apparatus
- Hardness apparatus
- Disintegration Tester
- Vernier Caliper
- Analytical Balance
- Moisture analyzer
- Mortar and pestle
- Spatula
- Filter Paper
- Magnetic Stirrer & Hot Plate
- Sonicator
- Vacuum Pump
- Glassware
- Tris Buffer
- Hydrochloric acid
- Sodium Hydroxide
- Distilled water
PROCEDURE:
FINAL MIX
Rabeprazole sodium Tablet Complete Testing Procedure (SOP)
Description:
A white powder.
Procedure: Take 2.0 g of the test sample in a watch glass and observe visually with black background. Check the appearance of color, nature and any visible foreign particles.
Identification: (By UV SPECTROPHOTOMETER)
The spectrum of the sample preparation corresponds to spectrum of the standard preparation as obtained in the assay.
Loss on Drying: (By Moisture Analyzer)
Procedure:
Turn on instrument 20 minute before the test. Take 2 g powder spread uniformly on Moisture Analyzer plate. Close the lid and press start button.
NMT 5.0% when determined by LOD Apparatus, Use 2.0 g of powder.
Assay: (Limit: 90%-110%)Compression Weight of Powder/Tablet…..
Procedure:
Standard Solution:
Take 40 mg of Rabeprazole sodium equivalent 40 mg of Rabeprazole sodium WS dissolved in 0.1 N sodium hydroxide and make up the volume to 100mL with 0.1 N sodium hydroxide. Shake, and sonicate for 5 minutes to facilitate dissolution
Take 2 mL from standard stock solution and make up the volume to 100 mL with 0.1 N sodium hydroxide.
Sample solution:
Take compression weight of finally grinded granules and dissolved in 0.1 N sodium hydroxide and make up the volume to 100mL with 0.1 N sodium hydroxide. Shake by mechanical mean for 10 minutes to disperse and allow any insoluble matter to settle.
Pass a portion of the sample stock solution through a suitable filter of 0.45um pore size.
Transfer the 2 mL of filtrate to a 50 mL volumetric flask make up volume with 0.1 N sodium hydroxide. Take reading at UV spectrophotometer at 293 nm using 0.1 N sodium hydroxide as blank.
Calculations:
Sample Absorbance x Standard Concentration x Ave. Weight of Tablet x Potency
Standard Absorbance x Sample Concentration x Label Claim
Disintegration Test:
Acid Stage Medium: 0.1N HCl
Test Time: One Hourat 370C ± 20C
Buffer Stage Medium: Phosphate Buffer 6.8
Test Time: 45 minutesat 370C ± 20C
Dissolution Test:
Acid Stage:
- USP Apparatus: USP Apparatus II Paddle
- Medium: 700mL 0.1N HCl
- Speed: 100 rpm
- Time: 120 Minute
- Medium Temperature: 37º ± 0.5º
- Recommended Sampling Time: Rabeprazole sodium:
- Acid Stage: 120 Minutes
- Buffer stage: 45 minutes
- Diluent: A- 0.1 N Hydrochloric acid
Standard Stock Solution: Transfer about 35.7 mg of Rabeprazole sodium WS to a 50-mL volumetric flask. Add about 30 mL of 0.1 N sodium hydroxide, and sonicate until dissolved. Add 20 mL of diluent mix, and dilute with diluent to volume.
Standard Solution: Transfer 1.0 mL of the Standard stock solution to a 25-mL volumetric flask, and dilute with Diluent to volume.
Sample solution: After 120 min, withdraw an aliquot, pass through a suitable filter of 0.45µmpore size and take absorbance using 0.1N HCl as blank
Transfer the 300mL of buffer to the vessels and set pH 8.0.
Instrumental Conditions
- Mode: UV
- Analytical wavelength: UV 329 nm
- Blank: Medium
Calculations:
Sample Absorbance x Standard Concentration x Potency
Standard Absorbance x Sample Concentration
Tolerances: NMT 10% of the labeled amount of Rabeprazole sodium is dissolved.
Buffer Stage:
- USP Apparatus: USP Apparatus II Peddle
- Medium: 1000mL Buffer pH 8.0(700mL 0.1 N hydrochloric acid after 2 hr add 300mL Tris Buffer and adjust pH 8.0)
- Speed: 100 rpm
- Time: 45 Minute
- Medium Temperature: 37º ± 0.5º
- Recommended Sampling Time: Rabeprazole sodium:
- Buffer stage: 45 minutes
Tris Buffer Preparations: Dissolve 144.4444 g of tris buffer in water and make up volume to 2000mL with water
Dissolution Medium: 700 mL 0.1N HCl. After 2 h, continue with a pH 8.0tris buffer as follows. To the vessel, add 300 mL of tris buffer, and adjust with 2 N hydrochloric acid or 2 N sodium hydroxide, if necessary, to a pH of 8.0 ± 0.10.
Analysis: After 45 min, withdraw an aliquot, pass through a suitable filter of 0.45µ pore size.
Determine the amount of Rabeprazole sodium dissolved in the Buffer stage.
Diluent: Dissolution Medium
Standard Stock Solution: Transfer about 50 mg of Rabeprazole sodium WS to a 100mL volumetric flask. Add about 10 mL of 0.1 N sodium hydroxide, and sonicate until dissolved. Add 30 mL of diluent mix, and dilute with diluent to volume.
Standard Solution: Transfer 2.0 mL of the Standard stock solution to a 50 mL volumetric flask, and dilute with Diluent to volume.
Sample solution: After 45 min, withdraw an aliquot, pass through a suitable filter of 0.45µmpore size and take absorbance using diluent as blank
Instrumental Conditions
- Mode: UV
- Analytical wavelength: UV 286 nm
- Blank: Medium
Calculations:
Sample Absorbance x Standard Concentration x Potency
Standard Absorbance x Sample Concentration
Tolerance: NLT 80% of the labeled amount of Rabeprazole sodium is dissolved.
Uniformity of Dosage Units: (By Weight Variation)
Weigh 20 tablets individually and calculate the average weight as:
Average weight = (Weight Of 20 Tablets)/20
Weigh all these tablets individually and mark among these weights maximum (WMax) & minimum (WMin) weight tablets. Calculate the maximum and minimum variation in percent as:
Maximum% age variation =((WMax) – (WAvg.))/WAvg×100
Minimum % age variation ((WMin) – (WAvg.))/WAvg×100
Hardness Test & Dimensions:
Perform the hardness test on 10 tablets and take the average. Power on the instrument and regulate zero adjustment and preset the ‘’HARDNESS’’ and “Thickness” mode. Place the tablet on the test plate, begin testing and read the hardness thickness and diameter. Clean the shattered tablet and print out test results, perform the test on 10 tablets and take the average.
Friability Test:
For tablets with a unit mass equal to or less than 650 mg, take a sample of whole tablets corresponding to 6.5 g. For tablets with a unit mass of more than 650 mg, take a sample of 10 whole tablets. The tablets should be carefully dedusted prior to testing. Accurately weigh the tablet sample, and place the tablets in the drum. Rotate the drum 100 times, and remove the tablets. Remove any loose dust from the tablets as before, and accurately weigh. Generally, the test is run once. If obviously cracked, cleaved, or broken tablets are present in the tablet sample after tumbling, the sample fails the test. If the results are doubtful or if the weight loss is greater than the targeted value, the test should be repeated twice and the mean of the three tests determined. A maximum mean weight loss from the three samples of not more than 1.0% is considered acceptable for most products.
% FRIABILITY= W1-W2/W1 x 100
Leak Test:
Take 06 blisters of tablet 03 filled and 03 empty. Dip these blisters in the bowl of leak test apparatus containing colored water. Create vacuum 250 mmHg and hold for one minute. Release vacuum and check the penetration of water inside the blisters. All blisters should be free of water.
CONTENT UNIFORMITY TEST: By Weight variation
Calculation of Acceptance Value (AV):
Limits:
L1= ≤ 15 (For 10 Unit)
L2= ≤ 25 (For 30 Unit)
General Formula = M-x̄ ±ks
Acceptability Constant = (k)
Standard Deviation (SD) = s
Number of Units = (n)
Reference Value = M
Mean of Individual Content = x̄