There are different testing methods for Ondansetron tablets, but a common one is the UV HPLC method This method should be performed by trained personnel in a controlled environment, and all necessary safety precautions should be taken. This SOP is intended to provide a standardized method for the testing of Ondansetron 8mg tablets by UV High Performance Liquid Chromatography (HPLC) method.
To describes the procedure for analysis at in-process and finished stage of Ondansetron 8mg Tablet.
This SAP gives detailed outline for the finished product analysis of Ondansetron 8mg Tablet and will cover In process testing activities on physical, chemical & instrumental basis.
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.
UNITED STATES PHARMACOPOEIA
MATERIAL AND EQIUPMENT:
- UV Spectrophotometer
- Dissolution apparatus
- Friability apparatus
- Hardness apparatus
- Disintegration Tester
- Vernier Caliper
- Analytical Balance
- Moisture analyzer
- Mortar and pestle
- Filter Paper
- Magnetic Stirrer & Hot Plate
- Vacuum Pump
- Methanol AR Grade
- Distilled water
SOP for Ondansetron 8mg Tablet Testing by UV HPLC Method
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: 160 mg /tablet
ASSAY BY HPLC:
Buffer: 2.7 g/L of monobasic potassium phosphate. Adjust with 1 N sodium hydroxide to a pH of 5.4.
Mobile phase: Acetonitrile and Buffer(1 :4)
Diluent: Acetonitrile and Buffer (1:1)
0.05 mg/mL of ondansetron (freebase) in Diluent from Ondansetron Hydrochloride WS
Sample stock solution:
Weigh and finely powder NLT 20 tablet. Transfer a portion of the powder, equivalent to 50 mg of ondansetron, based on the label claim, to a 100 mL volumetric flask. Add 70 mL of Diluent, and sonicate for about 20 min. Dilute with Diluent to volume. Centrifuge a portion of the solution.
Quantitatively dilute the supernatant with Diluent to obtain a solution having a nominal concentration of 0.05 mg/mL of ondansetron, based on the label claim.
Pass through a suitable nylon filter of 0.45-um pore size, and use the filtrate.
(See Chromatography (621), System Suitability.)
Detector: UV 216 nm
Column: 4.6-mm x 25-cm; 5-um packing L10
Flow rate: 1.5 mL/min
Injection size: 10 µL
Samples: Standard solution
Tailing factor: NMT 2.0
Relative standard deviation: NMT 2.0%
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: Ondansetron as HCl: 90%-110%of the labeled amount
ALTERNATE METHOD BY UV
Take 24.9 mg of Ondansetron HCl WS equivalent 20mg of ondansetron dissolved in 0.1N HCl and make up the volume to 100mL with 0.1N HCl. 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 0.1N HCl.
Take compression weight of finally grinded granules and dissolved in 0.1N HCl and make up the volume to 100mL with 0.1N HCl. 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 0.1N HCl. Take reading at UV spectrophotometer at 310 nm using 0.1N HCl as blank.
Sample Absorbance x Standard Concentration x Ave. Weight of Tablet x Potency
Standard Absorbance x Sample Concentration x Label Claim x Factor
Limit: Ondansetron as HCl: 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 = (WeightOf 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 06 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 06 tablets and take the average.
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
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.
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.
DISSOLUTION (As per Test II)
Medium: Water; 500 mL, deaerated
Apparatus 2: 50 rpm
Time: 30 min
Ondansetron Hydrochloride WS in Medium in a concentration similar to the one expected in the Sample solution.
Sample solution: Pass a portion of the solution under test through a suitable filter of 0.45-µm pore size, and dilute, if necessary, with Medium.
(See Ultraviolet-Visible Spectroscopy (857)
Analytical wavelength: 310 nm
Samples: Standard solution and Sample solution
Calculate the percentage of ondansetron (C18H19N3O)dissolved:
Result =(Au/As) x (Cs/L) x (M r1/M r2) x V x 100
Au =absorbance of the Sample solution
As = absorbance of the Standard solution
Cs = concentration of the Standard solution (mg/mL)
L = Label claim (mg/Tablet)
Mr1 = molecular weight of ondansetron, 293.36
Mr2 =molecular weight of ondansetron hydrochloride(anhydrous), 329.83
V = volume of Medium, 500 mL
Tolerances: NLT 80% (Q) of the labeled amount of C18H19N3O is dissolved.
CONTENT UNIFORMITY TEST: (By HPLC)
Proceed as directed in the Compressed Tablet.
Calculation of Acceptance Value (AV):
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