The testing procedures for pharmaceutical products like Lornoxicam 8mg Tablets typically involve a series of rigorous steps to ensure the safety, efficacy, and quality of the medication. These procedures are conducted during the development, manufacturing, and quality control phases.
Determination of lornoxicam in pharmaceutical preparations by UV and HPLC spectrophotometric methods Before the tablet is manufactured, researchers and pharmaceutical companies work on developing the appropriate formulation. This includes determining the active ingredient (Lornoxicam, in this case) and other excipients (inactive ingredients) that will make up the tablet.
PURPOSE:
To describe the procedure for analysis at the in-process and finished stage of Lornoxicam 8mg Tablet.
SCOPE:
This SAP gives a detailed outline for the finished product analysis of Lornoxicam 8mg Tablet and will cover process testing activities on a physical, chemical & instrumental basis.
RESPONSIBILITY:
QC Analyst is responsible for physical/chemical testing and preparing standard analytical procedures.
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
- HPLC
- 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
- Phosphoric Acid
- Sodium hydroxide
- Monobasic Potassium Phosphate
PROCEDURE:
FINAL MIX
Determination of lornoxicam in pharmaceutical preparations by UV and HPLC spectrophotometric methods
Description:
A 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: (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 but-ton.
NMT 5.0% when determined by LOD Apparatus, Use 2.0 g of powder.
Assay: (Limit: 90%-110%) Compression Weight of Powder
Assay By UV SPECTROPHOTOMETER
Preparation of 0.1 normal sodium hydroxide:
Take 4.2 g of sodium hydroxide and dissolve in 1000 mL water
Standard Solution:
Take 40 mg of Lornoxicam WS dissolved in 0.1 normal sodium hydroxide and make up the volume to 100mL with 0.1 normal sodium hydroxide. Shake, and sonicate for 5 minutes to facilitate dissolution.
Take 2 mL from standard stock solution and make up the volume to 50 mL with 0.1 normal sodium hydroxide.
Sample solution:
Take weight of finally grinded granules equivalent to 16 mg of Lornoxicam and dissolved in 0.1 normal sodium hydroxide and make up the volume to 100mL with 0.1 normal 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 5 mL of filtrate to a 50mL volumetric flask make up volume with 0.1 normal sodium hydroxide. Take reading at UV spectrophotometer at 289 nm using 0.1 normal 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
Limit: Lornoxicam: 90%-110%of the labeled amount
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:—–
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: ———-
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 de dusted 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 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.
Dissolution Test:
Preparation of Phosphate Buffer pH 6.8:
Dissolve 6.8045 g of KH2PO4dissolved in 1000 mL of water. Add 112 mL 0.2 Molar sodium hydroxide and volume make up up to 1000 mL with Water. Adjust with phosphoric acid to a pH of 6.8, if necessary.
- USP Apparatus: USP Apparatus II Peddle
- Medium: 900mL Phosphate Buffer pH 6.8
- Speed: 50 rpm
- Time: 45 Minute
- Medium Temperature: 37º ± 0.5º
- Recommended Sampling Time: Lornoxicam: 45Minutes
- Diluent: Dissolution medium
Standard solution: Take 44.4 mg Lornoxicam WS in 50mL volumetric flask then make up volume with 0.1N NaOH.
Take 1 mL from standard stock solution and make up the volume upto100 mL with medium.
Sample solution: Pass a portion of solution under through a suitable filter of 0.45-um pore size.
Instrumental Conditions
- Mode: UV
- Analytical wavelength: UV 375 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% of the amount stated on the label for Lornoxicam at 45 minutes.
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.
NOTE:
It’s important to note that the specific testing procedures may vary depending on the country, regulatory agency, and pharmaceutical company. The goal of these tests is to ensure that the medication is safe, effective, and consistent in its quality. Additionally, pharmaceutical companies must comply with good manufacturing practices (GMP) to maintain the quality and integrity of their products.