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小木虫论坛-学术科研互动平台 » 生物医药区 » 新药研发 » 政策法规 » 替硝唑（tinidazole）2012年版英国药典标准
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Tinidazole.doc
http://kuai.xunlei.com/d/GRVPTRWWAXAG?p=130497
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http://www.drugfuture.com/standard/search.aspx

•        British Pharmacopoeia Volume I & II
•        Monographs: Medicinal and Pharmaceutical Substances
Tinidazole         
General Notices

(Ph. Eur. monograph 1051)


C8H13N3O4S    247.3    19387-91-8
Action and use
Antiprotozoal; antibacterial.
Ph Eur
DEFINITION
1-[2-(Ethylsulfonyl)ethyl]-2-methyl-5-nitro-1H-imidazole.
Content
98.0 per cent to 101.0 per cent (dried substance).
CHARACTERS
Appearance
Almost white or pale yellow, crystalline powder.
Solubility
Practically insoluble in water, soluble in acetone and in methylene chloride, sparingly soluble in methanol.
IDENTIFICATION
First identification  A, C.
Second identification  A, B, D, E.
A. Melting point (2.2.14): 125 °C to 128 °C.
B. Ultraviolet and visible absorption spectrophotometry (2.2.25).
Test solution  Dissolve 10.0 mg in methanol R and dilute to 100.0 mL with the same solvent. Dilute 1.0 mL of this solution to 10.0 mL with methanol R.
Spectral range  220-350 nm.
Absorption maximum  At 310 nm.
Specific absorbance at the absorption maximum  340 to 360.
C. Infrared absorption spectrophotometry (2.2.24).
Comparison  tinidazole CRS.
D. Thin-layer chromatography (2.2.27).
Test solution  Dissolve 20 mg of the substance to be examined in methanol R and dilute to 10 mL with the same solvent.
Reference solution  Dissolve 20 mg of tinidazole CRS in methanol R and dilute to 10 mL with the same solvent.
Plate  TLC silica gel GF254 plate R.
Pretreatment  Heat at 110 °C for 1 h and allow to cool.
Mobile phase  butanol R, ethyl acetate R (25:75 V/V).
Application  10 µL.
Development  Over 2/3 of the plate.
Drying  In air.
Detection  Examine in ultraviolet light at 254 nm.
Results  The principal spot in the chromatogram obtained with the test solution is similar in position and size to the principal spot in the chromatogram obtained with the reference solution.
E. To about 10 mg add about 10 mg of zinc powder R, 0.3 mL of hydrochloric acid R and 1 mL of water R. Heat in a water-bath for 5 min and cool. The solution gives the reaction of primary aromatic amines (2.3.1).
TESTS
Appearance of solution
The solution is clear (2.2.1) and not more intensely coloured than reference solution Y5 (2.2.2, Method II).
Dissolve 1.0 g in acetone R and dilute to 20 mL with the same solvent.
Related substances
Liquid chromatography (2.2.29). Protect solutions from light.
Test solution  Dissolve 10.0 mg of the substance to be examined in 10.0 mL of methanol R and dilute to 100.0 mL with the mobile phase.
Reference solution (a)  Dilute 1.0 mL of the test solution to 100.0 mL with the mobile phase. Dilute 1.0 mL of this solution to 10.0 mL with the mobile phase.
Reference solution (b)  Dissolve 5.0 mg of tinidazole impurity A CRS and 5.0 mg of tinidazole impurity B CRS in 10.0 mL of methanol R and dilute to 100.0 mL with the mobile phase. Dilute 2.0 mL of this solution to 10.0 mL with the mobile phase.
Reference solution (c)  Dilute 1.0 mL of reference solution (b) to 50.0 mL with the mobile phase.
Column:
•        — size: l = 0.25 m, Ø = 3.0 mm;
•        — stationary phase: octylsilyl silica gel for chromatography R (5 µm).
Regular column conditioning by subsequent flushing with 50 mL of water R, 100 mL of methanol R, 25 mL of water R and 100 mL of the mobile phase is recommended.
Mobile phase  acetonitrile R, methanol R, water R (10:20:70 V/V/V).
Flow rate  0.5 mL/min.
Detection  Spectrophotometer at 320 nm.
Injection  20 µL.
Run time  1.5 times the retention time of tinidazole.
Relative retention  With reference to tinidazole (retention time = about 6 min): impurity A = about 0.6; impurity B = about 0.7.
System suitability  Reference solution (b):
•        — resolution: minimum 2.0 between the peaks due to impurities A and B.
Limits:
•        — impurities A, B: for each impurity, not more than the area of the corresponding peak in the chromatogram obtained with reference solution (c) (0.2 per cent);
•        — unspecified impurities: for each impurity, not more than the area of the principal peak in the chromatogram obtained with reference solution (a) (0.10 per cent);
•        — total: not more than 4 times the area of the principal peak in the chromatogram obtained with reference solution (a) (0.4 per cent);
•        — disregard limit: 0.5 times the area of the principal peak in the chromatogram obtained with reference solution (a) (0.05 per cent).
Heavy metals (2.4.8)
Maximum 20 ppm.
1.0 g complies with test D. Prepare the reference solution using 2 mL of lead standard solution (10 ppm Pb) R.
Loss on drying (2.2.32)
Maximum 0.5 per cent, determined on 1.000 g by drying in an oven at 105 °C.
Sulfated ash (2.4.14)
Maximum 0.1 per cent, determined on 1.0 g.
ASSAY
Dissolve 0.150 g in 25 mL of anhydrous 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 24.73 mg of C8H13N3O4S.
STORAGE
Protected from light.
IMPURITIES
Specified impurities  A, B.


A. 2-methyl-5-nitro-1H-imidazole,


B. 1-[2-(ethylsulfonyl)ethyl]-2-methyl-4-nitro-1H-imidazole.
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