## STP FOR PANTOPRAZOLE GASTRO-RESISTANT TABLETS

1.0) Description: Visual

2.0) Average Weight: Check weight of 20 tablets at randomly. And calculate the average weight by formula :

wt of 20 tablets (gm) x 1000 / 20. found avg. wt in mg

3.0) Uniformity of weight:

Weigh 20 tablets selected at random and calculate the average weight. Not more than two of the individual weights deviate from the average weight by more than the percentage shown in table.

Weigh the tablets individually and calculate the percentage of deviation for each tablet. By using formula

= (experimental weight – theoretical weight)    x 100%

Theoretical weight

 Average weight of tablets Percentage deviation More than 80mg but Less than 250mg 7.5% 250mg or More 5%

4.0)      Identification Test:

1. In the assay the principal peak in the chromatogram obtained with the test solution corresponds to the principal peak in the chromatogram obtained with the reference solution.
2. When examined in the range 230nm to 350nm, a 0.001 percent w/v solution in methanol shows absorption maxima at about 289nm.

5.0)      Hardness:

The standard method used for tablet hardness testing is compression testing. The tablet is placed between two jaws that crush the tablet. The machine measures the force applied to the tablet and detects when it fractures. Although compressive force is applied to the tablet, along the diameter of the tablet at right angles to the applied force.

6.0)      Disintegration Time

Unless otherwise stated in the individual monograph, introduce one tablet in each of the basket and if the tablet has a soluble external coating, immerse the basket in water at room temperature for 5 minutes. Then operate the apparatus using simulated gastric fluid temperature maintained at 37±2° as the immersion fluid. After 2 hour of operation in simulated gastric fluid, lift the basket from the fluid, and observe the tablets. The tablets show no evidence of disintegration, cracking, or softening. Operate the apparatus, using simulated intestinal fluid temperature maintained at 37±2° as the immersion fluid, for the time specified in the monograph. Lift the basket from the fluid and observe the tablets. All of the tablets disintegrate add a disc to each tube. The assembly is suspended in the liquid medium in a suitable vessel, preferably a 1-litre beaker. The volume of liquid is such that the wire mesh at its highest point is at least 15mm below the surface of the liquid, and at its lower point is at least 25mm above the bottom of the beaker. At no time should the top of the basket-rack assembly become submerged. There is a thermostatic arrangement for heating the liquid and maintaining the temperature at 37±2°.

If 1 or 2 tablets fail to disintegrate, repeat the test on 12 additional tablets; not less than 16 of the total of 18 tablets tested disintegrate.

If the tablets adhere to the disc and the preparation under examination fails to comply, repeat the test omitting the disc. The preparation complies with the test if all the tablets in the repeat test disintegrate.

7.0)      Dimension of Tablet:

Length, breadth and thickness are determined by vernier in mm

8.0)      Dissolution:

Medium: 0.1 M hydrochloric acid; 1000ml

Speed: 100 rpm

Time: 120 minutes

Determined by liquid chromatography

Test solution: Withdraw the medium completely and disperse the intact tablet in 100ml of   the mobile phase and filter.

Reference Solution: Dissolve a weighed quantity of  Pantoprazole sodium reference standard in the mobile phase and dilute with mobile phase to obtained a solution having a known concentration similar to the test solution.

Chromatographic system:

• A stainless steel column 25cm X4.6mm, packed with octadecylsilane bonded to porous silica (5µm)
• Mobile Phase: A mixture of 50 volumes of buffer solution prepared by dissolving 6.8gm of potassium dihydrogen orthophosphate and 1 gm of hexane sulphonic acid sodium salt in 1000ml of water. Adjusted to pH 7.3 with 1M sodium hydroxide and 50 volumes of acetonitrile,
• Flow rate: 1.5ml per minute,
• Spectrophotometer set at 290nm,
• Injection volume: 10µl

Inject the reference solution and the test solution.

Calculate the content of Pantoprazole released in the acid medium by subtracting the content of Pantoprazole in the test solution from the             total content of Pantoprazole.

Limit: NMT 15% of Pantopraole should be dissolved.

Medium: Tris-acetate buffer solution pH: 8.5; 1000ml

Speed: 75 rpm

Time: 60 minutes

Determined by liquid chromatography

Run method A on another 6 tablets and discard the medium completely and fill the empty vessel with the dissolution medium. Withdraw a suitable volume of the medium and filter.

Dilute the filtrate, if necessary, with the dissolution medium. Measure the absorbance at the maximum at about 290nm. Calculate the content of Pantoprazole in the medium from the absorbance obtained from a solution of known concentration of Pantoprazole sodium reference standard.

Limit: NLT less than 80 percent of the stated amount of Pantoprazole Sodium.

9.0)      Leak test:

The apparatus is used to test for the integrity of packed strips, blisters and Alu-Alu Blister pack containing tablets. Ensure apparatus bath is filled with purified water upto mark indicated and add 0.5% crystal violet solution in water. Samples are placed into the desiccators and the lid is placed in position. The pump starts to produce a vacuum 15inHg inside the desiccators and the vacuum is held for 1 minute. The sample remains at the required vacuum level for given time interval buzzer will sound after time is over and will cut off the vacuum pump. As the package is immersed in a colored dye solution the venting of the desiccators will allow any holes to be penetrated by the dye and the contents of the flexible packaging will also be stained with the same coloring material.

Examine all the strips for any leakage by opening the pockets manually. If anyone pocket shows evidence of leakage, reject the sample, stop the Blister / Strip machine and immediately take corrective action.

10.0)    Assay: Determined by liquid chromatography.

NOTE: Prepare the solutions immediately before use. Protect the solutions from light. Reference solution: A 0.02% percent w/v solution of Pantoprazole sodium reference standard in the mobile phase.

Test solution: Weigh and powder 20 tablets. Weigh a quantity of powder containing about 20mg of Pantoprazole Sodium, disperse in 100ml of the mobile phase and filter.

Chromatographic system:

• A stainless steel column 25cm X4.6mm, packed with octadecylsilane bonded to porous silica (5µm)
• Mobile Phase: A mixture of 50 volumes of buffer solution prepared by dissolving 6.8gm of potassium dihydrogen orthophosphate and 1 gm of hexane sulphonic acid sodium salt in 1000ml of water. Adjusted to pH 7.3 with 1M sodium hydroxide and 50 volumes of acetonitrile,
• Flow rate: 1.5ml per minute,
• Spectrophotometer set at 290nm,
• Injection volume: 10µl

Inject the reference solution. The rest is not valid unless the theoretical plates are not less than 2000, the tailing factor is not more than 2.0 and the relative standard deviation for replicate injections is not more than 2.0 percent.

Inject the reference solution and the test solution.

Calculate the content of Pantoprazole sodium in the tablets.

Alternative Method: By UV Spectrophotometer

Test Solution: Weigh and powder 20 tablets. Weight sample equivalent to 40mg of Pantoprazole in 100ml volumetric flask add l0ml 0.1 M HCl into it and sonicate to dissolve the test sample. Make up to mark with 0.1 M HCl. Filter and dilute 1ml of this solution to 25ml in 0.1 M HCl.

Reference Solution: Weigh 40mg of reference standard of Pantoprazole sodium in 100ml of volumetric flask. Add 10ml 0.1 M HCl into it and sonicate to dissolve. Make up to mark with 0.1 M HCl. Dilute 1ml of this solution to 25ml with 0.1 M HCl.

Check Absorbance of test as well as reference standard at 296nm in UV Spectrophotometer.

Calculate the content of Pantoprazole in the tablets.

Formula for calculation:

Absorbance of TEST       STD wt. (mg)                1               100                     25               Potency

—————————-X——————–X———X—————–X———–X—————-X Avg. Wt.

Absorbance of STD            100                             25       Test wt (mg)             1                     100

Acceptance criteria: 90.0%-110.0%

Abbreviations:

Wt.: Weight

mg: Miligram

ml: Milileter

HCl: Hydrochloric acid

inHg: Inch of Mercury

STD: standard

Avg: average

UV: ultraviolet