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奥美拉唑钠EP

Omeprazole sodium EUROPEAN PHARMACOPOEIA

7.0

Wavelength :285.2nm.

Water (2.5.12):7.0per cent to 10.0per cent,determined on 0.200g.

ASSAY

Liquid chromatography (2.2.29).

Buffer pH 11.0.Mix 11mL of a 95.0g/L solution of trisodium phosphate dodecahydrate R and 22mL of a 179.1g/L solution of disodium hydrogen phosphate R .Dilute to 100.0mL with water R .

Test solution .Dissolve 10.0mg of the substance to be examined in about 10mL of methanol R .Add 10mL of buffer pH 11.0and dilute to 200.0mL with water R .

Reference solution .Dissolve 10.0mg of omeprazole CRS in about 10mL of methanol R .Add 10mL of buffer pH 11.0and dilute to 200.0mL with water R .Column :

—size :l =0.125m,?=4mm;

—stationary phase :octylsilyl silica gel for chromatography R (5μm).

Mobile phase :mix 35volumes of acetonitrile R and 65volumes of a 1.4g/L solution of disodium hydrogen phosphate R previously adjusted to pH 7.6with phosphoric acid R .Flow rate :1mL/min.

Detection :spectrophotometer at 280nm.Injection :20μL.

Run time :1.5times the retention time of omeprazole.Retention time :omeprazole =about 4min.

Calculate the percentage content of C 34H 36MgN 6O 6S 2from the declared content of omeprazole CRS .

1g of omeprazole is equivalent to 1.032g of omeprazole magnesium.

STORAGE

In an airtight container,protected from light.

IMPURITIES

Specified impurities :D,E .

Other detectable impurities (the following substances would,if present at a sufficient level,be detected by one or other of the tests in the monograph.They are limited by the general acceptance criterion for other/unspecified impurities and/or by the general monograph Substances for pharmaceutical use (2034).It is therefore not necessary to identify these impurities for demonstration of compliance.See also 5.10.Control of impurities in substances for pharmaceutical use ):A,B,C

A.5-methoxy-1H

-benzimidazole-2-thiol,

B.R =H,X =SO:2-[(RS )-[(3,5-dimethylpyridin-2-yl)methyl]sulfinyl]-5-methoxy-1H -benzimidazole,

C.R =OCH 3,X =S:5-methoxy-2-[[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]sulfanyl]-1H -benzimidazole,

D.R =OCH 3,X =SO 2:5-methoxy-2-[[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]sulfonyl]-1H

-benzimidazole, E.4-methoxy-2-[[(RS )-(5-methoxy-1H -benzimidazol-2-yl)sulfinyl]methyl]-3,5-dimethylpyridine 1-oxide.

01/2011:1032

OMEPRAZOLE SODIUM Omeprazolum

natricum

C 17H 18N 3NaO 3S,H 2O M r 385.4

[95510-70-6]

DEFINITION

Sodium 5-methoxy-2-[(RS )-[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]sulfinyl]-1H -benzimidazole monohydrate.

Content :98.0per cent to 101.0per cent (anhydrous substance).CHARACTERS

Appearance :white or almost white,hygroscopic powder.

Solubility :freely soluble in water and in ethanol (96per cent),soluble in propylene glycol,very slightly soluble in methylene chloride.

IDENTIFICATION

A.Optical rotation (2.2.7):?0.10°to +0.10°,determined on solution S.

B.Infrared absorption spectrophotometry (2.2.24).

Preparation :dissolve 0.50g of the substance to be examined in 1.50mL of water R ,add 3.0mL of methanol R and stir;while stirring,adjust to pH 8-9by adding,dropwise,dilute acetic acid R (about 0.4mL);continue stirring until crystallisation and isolate the crystalline precipitate by filtration;wash with 5mL of water R ,then 2mL of methanol R ,and dry in vacuo at 40°C for https://www.wendangku.net/doc/5a9657863.html,parison :omeprazole CRS .

If the spectra obtained in the solid state show differences,dissolve the crystalline precipitate and the reference

substance separately in methanol R ,evaporate to dryness and record new spectra using the residues.

C.Ignite 1g and cool.Add 1mL of water R to the residue and neutralise with hydrochloric acid R .Filter and dilute the filtrate to 4mL with water R .0.1mL of the solution gives reaction (b)of sodium (2.3.1).TESTS

Solution S .Dissolve 0.50g in carbon dioxide-free water R and dilute to 25mL with the same solvent.

Appearance of solution .Solution S is clear (2.2.1)and not more intensely coloured than reference solution B 6(2.2.2,Method II ).pH (2.2.3):10.3to 11.3for solution S.

Related substances .Liquid chromatography (2.2.29).Prepare solutions immediately before use.

Test solution .Dissolve 3mg of the substance to be examined in the mobile phase and dilute to 25.0mL with the mobile phase.Reference solution (a).Dissolve 1mg of omeprazole CRS and 1mg of omeprazole impurity D CRS in the mobile phase and dilute to 10.0mL with the mobile phase.

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See the information section on general monographs (cover pages)

EUROPEAN PHARMACOPOEIA 7.0Ondansetron hydrochloride

dihydrate

Reference solution (b).Dilute 1.0mL of the test solution to 100.0mL with the mobile phase.Dilute 1.0mL of this solution to 10.0mL with the mobile phase.

Reference solution (c).Dissolve 3mg of omeprazole for peak identification CRS (containing impurity E)in the mobile phase and dilute to 25.0mL with the mobile phase.Column :

—size :l =0.125m,?=4.6mm;

—stationary phase :octylsilyl silica gel for chromatography R (5μm).

Mobile phase :mix 27volumes of acetonitrile R and 73volumes of a 1.4g/L solution of disodium hydrogen phosphate R ,previously adjusted to pH 7.6with phosphoric acid R .Flow rate :1mL/min.

Detection :spectrophotometer at 280nm.Injection :40μL.

Run time :5times the retention time of omeprazole.

Identification of impurities :use the chromatogram supplied with omeprazole for peak identification CRS and the

chromatogram obtained with reference solution (c)to identify the peak due to impurity E;use the chromatogram obtained with reference solution (a)to identify the peak due to impurity D.Relative retention with reference to omeprazole

(retention time =about 9min):impurity E =about 0.6;impurity D =about 0.8.

System suitability :reference solution (a):

—resolution :minimum 3.0between the peaks due to

impurity D and omeprazole;if necessary adjust the pH of the aqueous part of the mobile phase or the concentration of acetonitrile R ;an increase in the pH will improve the resolution.Limits :

—impurities D,E :for each impurity,not more than 1.5times the area of the principal peak in the chromatogram obtained with reference solution (b)(0.15per cent);

—unspecified impurities :for each impurity,not more than the area of the principal peak in the chromatogram obtained with reference solution (b)(0.10per cent);

—total :not more than 5times the area of the principal peak in the chromatogram obtained with reference solution (b)(0.5per cent);

—disregard limit :0.5times the area of the principal peak in the chromatogram obtained with reference solution (b)(0.05per cent).

Heavy metals (2.4.8):maximum 20ppm.

1.0g complies with test C.Prepare the reference solution using 2mL of lead standard solution (10ppm Pb)R .

Water (2.5.12):4.5per cent to 10.0per cent,determined on 0.300g.

ASSAY

Dissolve 0.300g in 50mL of water R .Titrate with 0.1M

hydrochloric acid ,determining the end-point potentiometrically (2.2.20).

1mL of 0.1M hydrochloric acid corresponds to 36.74mg of C 17H 18N 3NaO 3S.

STORAGE

In an airtight container,protected from light.

IMPURITIES

Specified impurities:D,E.

A.5-methoxy-1H

-benzimidazole-2-thiol,

B.2-[(RS )-[(3,5-dimethylpyridin-2-yl)methyl]sulfinyl]-5-methoxy-1H

-benzimidazole,

C.5-methoxy-2-[[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]sulfanyl]-1H -benzimidazole

(ufiprazole),

D.5-methoxy-2-[[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]sulfonyl]-1H -benzimidazole

(omeprazole-sulfone),

E.4-methoxy-2-[[(RS )-(5-methoxy-1H -benzimidazol-2-yl)sulfinyl]methyl]-3,5-dimethylpyridine 1-oxide.

01/2008:2016

ONDANSETRON HYDROCHLORIDE

DIHYDRATE Ondansetroni hydrochloridum

dihydricum

C 18H 20ClN 3O,2H 2O M r 365.9

DEFINITION

(3RS )-9-Methyl-3-[(2-methyl-1H -imidazol-1-yl)methyl]-1,2,3,9-tetrahydro-4H -carbazol-4-one hydrochloride dihydrate.

Content :97.5per cent to 102.0per cent (anhydrous substance).CHARACTERS

Appearance :white or almost white powder.

Solubility :sparingly soluble in water and in alcohol,soluble in methanol,slightly soluble in methylene chloride.

IDENTIFICATION

A.Infrared absorption spectrophotometry (2.2.24).

Comparison :ondansetron hydrochloride dihydrate CRS .B.It gives reaction (a)of chlorides (2.3.1).

General Notices (1)apply to all monographs and other texts

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