## STP FOR CIPROFLOXACIN 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 peak in the chromatogram obtained with the reference solution.

B  Determine by thin-layer chromatography, coating the plate with silica gel GF254. Place the plate in an atmosphere of ammonia for about 15 minutes and transfer it to an unsaturated chamber.

Mobile phase: A mixture of 40 volumes of dichloromethane, 40 volumes of methanol, 20 volumes of strong ammonia solution and 10 volumes of acetonitrile.

Test solution: Shake a quantity of the powdered tablets containing about 0.15g of

ciprofloxacin with 75ml of water for 20 minutes, dilute to 100ml with water, mix, centrifuge

and use the clear supernatant liquid.

Reference solution: A 0.15 per cent w/v solution of ciprofloxacin HCl reference standard in

water.

Apply to the plate, as 1-cm bands, 5µl of each solution. Place the plate in an atmosphere of

ammonia for about 15 minutes and transfer it to an unsaturated chamber containing the mobile

phase. Allow the mobile phase to rise 12cm. Dry the plate in air for 15 minutes and examine

under ultraviolet light at 254nm and at 365nm. The principal band in the chromatogram

obtained with the test solution corresponds to that in the chromatogram obtained with the

reference solution.

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 into each tube and 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: 900ml of water

Time: 30 minutes

Speed: 50 rpm

Limit: NLT 85% of the stated amount of Ciprofloxacin.

Withdraw a suitable volume of the medium and filter. Measure the absorbance of the filtrate, suitably diluted with water if necessary, at the maximum at about 276nm. Calculate the content of ciprofloxacin, in the medium from the absorbance obtained by repeating the determination using a solution of known concentration of Ciprofloxacin HCl reference standard.

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 up to 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.

Test solution: Weigh and powder 20 tablets. Weigh accurately a quantity of the powder containing about 1.25 g of ciprofloxacin, add about 400ml of 0.01 M HCl, shake for 20 minutes, dilute to 500ml with 0.01M HCl and filter. Dilute 10ml of the filtrate to 100ml with 0.01 M HCl.

Reference solution (a):  A 003 per cent w/v solution of ciprofloxacin HCl reference standard in 0.01 M HCl.

Reference solution (b): A 0.05 per cent w/v solution of ciprofloxacin ethlylenediamine analog reference standard (a).

Chromatographic system:

• A stainless steel column 25cm X4mm, packed with octadecylsilane bonded to porous silica (5µm)
• Column temperature: 30±1°
• Mobile phase: a mixture of 87 volumes of 0.025M phosphoric acid, previously adjusted with triethylamine to a pH of 3.0±0.1, and 13 volumes of acetonitrile,
• Flow rate: 1.5ml per minute,
• Spectrophotometer set at 278nm,
• Injection volume: 10µl

Inject reference solution (b) and record the chromatogram adjusting the sensitivity and flow rate suitably so that the retention time for ciprofloxacin is between 6.4 and 10.8 minutes, the relative retention time are about 0.7 for ciprofloxacin ethylenediamine analog and 1.0 for ciprofloxacin and the resolution between ciprofloxacin ethylenediamine analog peak and ciprofloxacin peak is not less than 6.

Inject reference solution (a). The column efficiency determined from ciprofloaxin peak, is not less than 2500 theoretical plates, the tailing factor for the ciprofloxacin peak is not more than 2.0 and the relative standard deviation for replicate injections is not more than 1.5 per cent.

Inject reference solution (a) and test solution.

Alternative Method: By UV Spectrophotometer

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

Reference Solution: Weigh 100mg of reference standard of Ciprofloxacin HCl in 100ml of volumetric flask. Add 20ml 0.1 M HCl into it and sonicate to dissolve. Dilute 1ml of this solution to 100ml with 0.1 M HCl.

Check Absorbance of test as well as reference standard at about 276nm in UV Spectrophotometer.

Calculate the content of Cilnidipine in the tablets.

Formula:

Abs. of Test      STD Wt.(mg) 1            100              100       Potency

—————–X————–X——-X—————X——–X———–X Average wt.

Abs. of STD        100            100      Test Wt.(mg)     1            100

Acceptance criteria: 90.0%-110.0%

11.0)    MICROBIOLOGICAL PURITY

Perform the test according to requirements of IP,

Total aerobic Microbial count (TAMC): NMT 103 CFU/g

Total combined yeasts/Moulds count (TYMC): NMT 102 CFU/g

Pathogens: in 1gm drug.

Escherichia Coli – Should be absent

Pseudomonas aeroginosa – Should be absent

Salmonella – Should be absent

Staphylococcus aureus– Should be absent

Abbreviations:

Wt.: Weight

mg: Miligram

ml: Milileter

STD: Standard

inHg: Inch of Mercury

rpm: Rounds per minute

CFU: Colony forming unit

HCl: Hydrochloric acid

w/v: Weight/VolumeAbs. Absorbance