Both UV spectrophotometry and HPLC methods provide reliable and accurate results for the determination of Nimesulide in pharmaceutical dosage forms. The choice of method depends on factors such as the required sensitivity, specificity, and available equipment. Determination of Nimesulide in Pharmaceutical Dosage Forms by UV Spectrophotometry and HPLC Method is recommended to follow official pharmacopoeial methods or validated analytical procedures for accurate and precise analysis.
PURPOSE:
To describe the procedure for analysis at the in-process and finished stage of the Nimesulide Tablet.
SCOPE:
This SAP gives a detailed outline for the finished product analysis of the Nimesulide Tablet 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
- 0.1N HCl
- Distilled methanol
- Methanol AR grade
PROCEDURE:
FINAL MIX
Determination of Nimesulide in Pharmaceutical Dosage Forms by UV Spectrophotometry and HPLC Method
Description:
A light-yellow 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:
The spectrum of the sample preparation corresponds to spectrum of the standard preparation as obtained in the assay.
Assay: (Limit: 90%-110%)Compression Weight of Powder/Tablet: …mg /tablet
Procedure:
Standard Solution:
Take 25 mg of Nimesulide WS dissolved in methanol and make up the volume to 50mL with methanol. Shake, and sonicate for 5 minutes to facilitate dissolution
Take 1 mL from standard stock solution and make up the volume to 25 mL with methanol.
Sample solution:
Take 5gram of sample grind them to fine powder. Take weight of finally grinded powder equivalent to 50 mg of Nimesulide and dissolved in methanol and make up the volume to100 mL with methanol. 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 1 mL of filtrate to a 25mL volumetric flask make up volume with methanol. Take reading at UV spectrophotometer at 298 nm using methanol as blank.
Calculations:
Sample Absorbance x Standard Concentration x Ave. Weight of Tablet x Potency
Standard Absorbance x Sample Concentration x Label Claim
Limit: Nimesulide: 90%-110%of the labeled amount
CORE TABLET
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: ± 7.50%
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:
Thickness 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 methanol 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 370C ± 20C
Acceptance criteria of disintegration for tablets:
If 1 or 2 tablets fail to disintegrate completely repeat the test on 12 additional tablets, not less than 16 of the totals of 18 tablets tested disintegrate completely.
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 methanol. Create vacuum 250 mmHg and hold for one minute. Release vacuum and check the penetration of methanol inside the blisters. All blisters should be free of methanol.
Dissolution Test:
Preparation of Phosphate Buffer pH 7.40 with 1% Tween 80:
Dissolve 6.8045 g of KH2PO4dissolved in 1000 mL of water. Add 10mL of tween 80 and then add 195.5 mL 0.2 Molar sodium hydroxide and volume make up up to 1000 mL with Water. Adjust with phosphoric acid to a pH of 7.40, if necessary.
USP Apparatus : USP Apparatus II Peddle
Medium: : 900mL Phosphate Buffer pH 7.40
Speed: : 75 rpm
Time: : 30 Minute
Medium Temperature : 37º ± 0.5º
Standard solution:
Take 27.8 mg Nimesulide WS in 100mL volumetric flask add 100 mL medium to dissolve Nimesulide then make up volume with medium.
Take 5mL from standard stock solution and make up the volume upto50 mL with medium.
Sample solution:
Pass a portion of solution under through a suitable filter of 0.45-um pore size.
Transfer the 5 mL of filtrate to a 20 mL volumetric flask make up volume with medium. Instrumental Conditions
Mode: UV
Analytical wavelength: UV 327 nm
Blank: Medium
Calculations:
Sample Absorbance x Standard Concentration x Potency
Standard Absorbance 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 Nimesulidein 30 minutes.
Assay Test:
Procedure:
Standard Solution:
Take 25 mg of Nimesulide WS dissolved in methanol and make up the volume to 50mL with methanol. Shake, and sonicate for 5 minutes to facilitate dissolution
Take 1 mL from standard stock solution and make up the volume to 25 mL with methanol.
Sample solution:
Weigh 20 tablets and calculate average weight per tablet, grind them to fine powder take weight of powder equivalent to 50 mg of Nimesulide and dissolved in methanol and make up the volume to 100 mL with methanol. 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 1 mL of filtrate to a 25mL volumetric flask make up volume with methanol. Take reading at UV spectrophotometer at 298 nm using methanol as blank.
Calculations:
Sample Absorbance x Standard Concentration x Ave. Weight of Tablet x Potency
Standard Absorbance x Sample Concentration x Label Claim
Limit: Nimesulide: 90%-110%of the labeled amount
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