It seems like you are referring to the testing of Clopidogrel 75mg Tablet Testing by Ultraviolet (UV) Spectroscopy UV spectroscopy is a common technique used in pharmaceutical analysis to determine the concentration of a substance in a sample based on its absorption of ultraviolet light. However, the specific details about the testing of Clopidogrel 75mg Tablet using UV spectroscopy, such as the methods, results, or any ongoing studies, would require access to recent research papers or publications in the field of pharmaceutical analysis.
PURPOSE :
To describes the procedure for analysis at in-process and finished stage of clopidogrel 75mg Tablet.
SCOPE:
This SAP gives detailed outline for the finished product analysis of clopidogrel 75mg Tablet and will cover In process testing activities on 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:
USP 44 NF 39 SPECIFICATIONS
MATERIAL AND EQIUPMENT:
- HPLC
- Dissolution apparatus
- Friability apparatus
- Hardness apparatus
- Disintegration Tester
- Vernier Caliper
- Analytical Balance
- pH meter
- Moisture analyzer
- Mortar and pestle
- Spatula
- Filter Paper
- Magnetic Stirrer & Hot Plate
- Sonicator
- Vacuum Pump
- Glassware
- Methanol HPLC Grade
- Hydrochloric acid
- Distilled water
FINAL MIX PROCEDURE:
Description:
A white to off 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 HPLC)
The retention time of major peak of the sample preparation corresponds to that 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 By UV Spectrophotometer:
(Limit: 90%-110%)Compression Weight of Powder/Tablet: …….mg /tablet
Procedure:
Standard Solution:
Take 97.5 mg of clopidogrel hydrogen sulfate WS equivalent to 75 mg of clopidogrel dissolved in 0.1 normal hydrochloric acid and make up the volume to 100mL with 0.1 normal hydrochloric acid. 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 normal hydrochloric acid.
Sample solution:
Take weight of finally grinded granules equivalent to 75mg of clopidogrel and dissolved in 0.1 normal hydrochloric acid and make up the volume to 100mL with 0.1 normal hydrochloric acid. 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 100mL volumetric flask make up volume with 0.1normal hydrochloric acid. Take reading at UV spectrophotometer at 241 nm using 0.1 normal hydrochloric acid as blank.
Calculations:
Average Sample AUC x Standard Concentration x Ave. Weight of Tablet x Potency
Average Standard AUC x Sample Concentration x Label Claim x Factor
(Limit Clopidogrel: 90%-110%of the labeled amount)
CORE TABLET
Description:
Compression weight/Tablet:…….
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
Standard Limit: ± 5.00%
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.
Hardness Standard Limit: Not more than 10.00 Kg
Thickness Standard Limit:…..
Width Standard Limit:……
Length/Diameter Standard Limit:…….
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 x 100/W1
Disintegration Test:
Place the beaker filled with water into the beaker stand inside the bath and. Switch on the instrument, set the temperature at 37ºC± 2º C and wait till the temperature of the beaker reaches to the 37ºC± 2º C. Engage the basket on basket hook put the tablets in 6 tubes individually and place the discs then start the oscillations and timer. Note the disintegration time of all the six tablets.
Note the Disintegration time of 1st tablet to the last tablet.
Disintegration Time: NMT 15 minutes at 37C ± 2C
Acceptance criteria of disintegration for tablets:
If 1 or 2 tablet fail to disintegrate completely repeat the test on 12 additional tablets, not less than 16 of the total of 18 tablets tested disintegrate completely.
Dissolution Test:
Normal Hydrochloric Acid: Dissolve 8.5 mL of Hydrochloric acid to 1000mL beaker and volume make up up to 1000 mL with Water.
Hydrochloric Acid Buffer pH 3.0:14.91g/L of potassium chloride ± 45mL 0.1N HCl make up volume 1000mL with water.
USP Apparatus: USP Apparatus II Peddle
Medium: 900mL ( 0.1N HCl )
Speed: 75 rpm
Time: 20 Minute
Medium Temperature: 37º ± 0.5º
Recommended Sampling Time: Clopidogrel: 20 Minute
Diluent: Dissolution medium
Standard solution:.
Take 52.1 mg of clopidogrel hydrogen sulfate WS equivalent to 40 mg of clopidogrel into a 50 volumetric flask, then make up volume with medium.
Take 5 mL from standard stock solution and make up the volume upto50 mL with medium. Pass through a membrane filter of 0.45-µm pore size.
Sample solution:
Pass a portion of solution under through a suitable filter of 0.45-um pore size.
Mobile Phase: Methanol and Distilled Water (750:250)
Chromatographic system
Mode: LC
Detector: UV 225 nm.
Column: 4.6-mm x 25-cm; 5-µm packing L1
Temperatures: Column: 30°C
Flow rate: 1.0 mL/min
Injection volume: 20 µL
Calculations:
Sample AUC x Standard Concentration x Potency
Standard AUC x Sample Concentration
Tolerance:
The amount of drug dissolve in solution for each tablet is not less Than 80% Q of the amount stated on the label for Clopidogrelat20 minute.
BLISTER STAGE: 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.