standard test procedure ciprofloxacin injection

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standard test procedure ciprofloxacin injection

Product Name : STANDARD TEST PROCEDURE CIPROFLOXACIN INJECTION
Label Claim : 5 %

1. PROCEDURE
1.1 CIPROFLOXACIN INJECTION: Ciprofloxacin Injection is a sterile solution of Ciprofloxacin in 5% Dextrose Injection or in

Sodium Chloride Injection prepared with the aid of Lactic Acid.
1.2 Usual strength
1.2.1 2 mg per ml.
1.3 Storage
1.3.1 Store in light-resistant containers in a cool place. The contents should not be allowed to freeze.
1.4 STANDARDS
1.4.1 Ciprofloxacin Injection contains not less than 90.0 per cent and not more than 110.0 per cent of the stated amount of ciprofloxacin, C17H18FN3O3.
1.5 Identification
1.5.1 Complies with test B described under Ciprofloxacin applying 10 µl of each of the following solutions as 1-cm bands. For solution (1) dilute sufficient of the

injection with water to obtain a solution containing the equivalent of 0.05% w/v of Ciprofloxacin. Solution (2) is a 0.05% w/v solution of ciprofloxacin RS in 6M ammonia.
1.6 pH
1.6.1 Between 3.5 and 4.6,
1.7 Ciprofloxacin ethylenediamine analog
1.7.1 Not more than 0.5%, determined by the method described in Assay. Calculate the percentage of ciprofloxacin ethylenediamine analog from

the chromatogram obtained with solution (1) from the following expression:
% of the analog = 100[0.7 x ra /(0.7 x ra + rc)],
where 0.7 is the response factor for ciprofloxacin ethylenediamine analog relative to that of ciprofloxacin, ra and rc are the responses

of ciprofloxacin ethylenediamine analog peak and the ciprofloxacin peak respectively.
1.7.2 Lactic acid : Between 0.288 mg and 0.352 mg for each mg of Ciprofloxacin stated on the label, determined by the following method.

Carry out the method for high performance liquid chromatography, using the following solutions. Solution (1) is the substance being examined.

Solution (2) is a 0.08% w/v solution of sodium lactate RS in water.The chromatographic procedure may be carried out using (a) stainless steel

column (30 cm x 7.8 mm) packed with a strong cation-exchange resin consisting of sulphonated cross-linked styrene-divinylbenzene copolymer in the

hydrogen form (7 to 11 mm) operated at 40o ± 1o, (b) as the mobile phase a degassed mixture of 85 volumes of 0.0025M sulphuric acid

and 15 volumes of acetonitrile with a flow rate of about 0.6 ml per minute and (c) a detection wavelength of about 208 nm.

Inject 20 µl of solution (2) and record the chromatograms adjusting the sensitivity and flow rate suitably so that the tailing factor is

not more than 2.0 and the relative standard deviation for replicate injections is not more than 2.0%.Separately inject 20 µl of solutions (1) and (2),

record the chromatograms and measure the peak responses for the major peaks. Calculate the content of lactic acid, C3H6O3, in the

substance being examined.NOTE — After each analysis, the column should be rinsed with a mixture of 85 volumes of 0.005M sulphuric

acid and 15 volumes of acetonitrile to elute the ciprofloxacin from the column. The column may be regenerated with 0.005M sulphuric acid

and may be reused or stored.
1.7.3 Dextrose:(if present): Between 4.75 and 5.25% w/v of C6H12O6,H2O, determined by the following method. To 50.0 ml add 0.2 ml of 6M ammonia

and dilute to 100.0 ml. Mix well and determine the optical rotation at 25o in a 2-dm tube, The observed rotation in degrees

multiplied by 2.085 represents the percentage of dextrose monohydrate, C6H12O6,H2O, in the preparation being examined.
1.7.4 Sodium chloride:(if present): Between 0.855 and 0.945% w/v of NaCl, determined by the following method. To 10.0 ml

add 150 ml of water and titrate with 0.1M silver nitrate using potassium chromate solution as indicator. Each ml of 0.1M silver nitrate is equivalent to 0.005844 g of NaCl.
1.8 Bacterial endotoxins :
1.8.1 Not more than 0.25 Endotoxin Unit per mg of ciprofloxacin ,
1.9 Sterility
1.9.1 Complies with the tests for sterility, using Method A (Membrane Filtration)
1.10 Particulate matter
1.10.1 (for packs containing 100 ml or more): Complies with the limit test for particulate matter, .
1.11 Other requirement
1.11.1 Complies with the requirements of tests stated under Injectable Preparations (Injections).
1.12 Assay
1.12.1 Carry out the Assay described under Ciprofloxacin using the following solutions. For solution (1) dilute a quantity of the injection

equivalent to 25 mg of Ciprofloxacin to 100 ml with the mobile phase and mix. Solution (2) is a 0.03% w/v solution of ciprofloxacin

hydrochloride RS in the mobile phase. For Solution (3) dissolve a sufficient quantity of ciprofloxacin ethylenediamine analog RS in solution (2) so

as to obtain a solution containing 0.025% w/v of the reference substance.Calculate the content of C17H18FN3O3 from the declared content of C17H18FN3O3 in ciprofloxacin RS.
1.13 Labelling
1.13.1 The label states whether Dextrose or Sodium Chloride has been used for preparing the injection.
2. HISTORY