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DEFINITION
9-Fluoro-3-methyl-10-(4-methylpiperazin-1-yl)-7-oxo-2,3-
dihydro-7H-pyrido[3,2,1-ij][4,1,2]benzoxadiazine-6-carboxylic
acid.
Content: 99.0 per cent to 101.0 per cent (dried substance).
CHARACTERS
Appearance: light yellow, crystalline powder.
Solubility : slightly soluble in water, sparingly soluble or
slightly soluble in methylene chloride, very slightly soluble
in ethanol (96 per cent).
IDENTIFICATION
Infrared absorption spectrophotometry (2.2.24).
Comparison : marbofloxacin CRS.
TESTS
Absorbance (2.2.25) : maximum 0.20, determined at 450 nm.
Dissolve 0.400 g in borate buffer solution pH 10.4 R and
dilute to 10.0 ml with the same buffer solution.
Related substances. Liquid chromatography (2.2.29). Carry
out the test protected from light.
Solvent mixture : methanol R, water R (23:77 V/V).
Test solution. To 0.100 g of the substance to be examined
add 80 ml of the solvent mixture, sonicate until dissolution
and dilute to 100.0 ml with the solvent mixture.
Reference solution (a). Dilute 5.0 ml of the test solution
to 100.0 ml with the solvent mixture. Dilute 1.0 ml of this
solution to 50.0 ml with the solvent mixture.
Reference solution (b). Dissolve 10 mg of marbofloxacin
for peak identification CRS (containing impurities A, B, C,
D and E) in the solvent mixture and dilute to 10 ml with the
solvent mixture.
Column:
— size: l = 0.15 m, Ø = 4.6 mm;
— stationary phase: end-capped polar-embedded
octadecylsilyl amorphous organosilica polymer R
(3.5 μm);
— temperature: 40 °C.
Mobile phase: mix 230 volumes of methanol R and
5 volumes of glacial acetic acid R with 770 volumes of
a 2.70 g/l solution of sodium dihydrogen phosphate R
containing 3.50 g/l of sodium octanesulphonate R and
previously adjusted to pH 2.5 with phosphoric acid R.
Flow rate: 1.2ml/min.
Detection: spectrophotometer at 315 nm.
Injection: 10 μl.
Run time: 2.5 times the retention time of marbofloxacin.
Relative retention with reference to marbofloxacin
(retention time = about 33 min) : impurity B = about 0.5 ;
impurity A = about 0.7 ; impurity C = about 0.9 ;
impurity D = about 1.3; impurity E = about 1.5.
System suitability : reference solution (b) :
— resolution: minimum 1.5 between the peaks due to
impurity C and marbofloxacin, and minimum 4.0 between
the peaks due to marbofloxacin and impurity D.
Limits :
— correction factor : for the calculation of content, multiply
the peak area of impurity E by 1.5;
— impurities C, D, E: for each impurity, not more than
twice the area of the principal peak in the chromatogram
obtained with reference solution (a) (0.2 per cent) ;
— impurities A, B: for each impurity, not more than the
area of the principal peak in the chromatogram obtained
with reference solution (a) (0.1 per cent) ;
— unspecified impurities : for each impurity, not more than
twice the area of the principal peak in the chromatogram
obtained with reference solution (a) (0.2 per cent) ;
— total : not more than 5 times the area of the principal peak
in the chromatogram obtained with reference solution (a)
(0.5 per cent) ;
— disregard limit : the area of the principal peak in the
chromatogram obtained with reference solution (a)
(0.1 per cent).
Heavy metals (2.4.8) : maximum 20 ppm.
Dissolve 0.5 g in dilute acetic acid R and dilute to 30 ml with
the same solvent. Adding 2 ml of water R instead of 2 ml of
buffer solution pH 3.5 R, the filtrate complies with test E.
Prepare the reference solution using 5 ml of lead standard
solution (2 ppm Pb) R.
Loss on drying (2.2.32) : maximum 0.5 per cent, determined
on 1.000 g by drying at 105 °C for 4 h.
Sulphated ash (2.4.14) : maximum 0.1 per cent, determined
on 1.0 g in a platinum crucible.
ASSAY
Dissolve 0.300 g in 80 ml of glacial acetic acid R. Titrate
with 0.1 M perchloric acid, determining the end-point
potentiometrically (2.2.20).
1 ml of 0.1 M perchloric acid is equivalent to 36.24 mg of
C17H19FN4O4.
STORAGE
Protected from light.
[ Last edited by shich68 on 2008-12-23 at 16:31 ] |
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