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[交流] 【求助】盐酸莫西沙星原料英国药典标准

求助盐酸莫西沙星原料英国药典标准。。。
或者哪位权限比较高 http://medchem.dxy.cn/bbs/topic/16727438 在这帮着下来。。。

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1楼 2010-08-31 10:16:42

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fengyan22(金币+5):谢了 2010-09-01 23:04:13

----------------------- 页面 1-----------------------

  Browse: British Pharmacopoeia 2009

         British Pharmacopoeia Volume I & II

               Monographs: Medicinal and Pharmaceutical Substances

                  Moxifloxacin Hydrochloride

Moxifloxacin Hydrochloride

General Notices

(Ph Eur monograph 2254)

C H ClFN O 437.9186826-86-8

  21  25    3  4

Action and use

Fluoroquinolone antibacterial.

Ph Eur

DEFINITION

1-Cyclopropyl-6-fluoro-8-methoxy-7-[(4aS,7aS)-octahydro-6H-pyrrolo[3,4-b]pyridin-6-yl]-4-

oxo-1,4-dihydroquinoline-3-carboxylic acid hydrochloride.

Content

98.0 per cent to 102.0 per cent (anhydrous substance).

PRODUCTION

The production method is validated to demonstrate the satisfactory enantiomeric purity of the

final product.

CHARACTERS

Appearance

Light yellow or yellow powder or crystals, slightly hygroscopic.

Solubility

Sparingly soluble in water, slightly soluble in ethanol (96 per cent), practically insoluble in

acetone.

IDENTIFICATION

(C)Crown Copyright 2006                                                                                        1

----------------------- 页面 2-----------------------

IDENTIFICATION

A. Specific optical rotation (see Tests).

B. Infrared absorption spectrophotometry (2.2.24).

Comparisonmoxifloxacin hydrochloride CRS.

C. Dissolve 50 mg in 5 ml of water R, add 1 ml of dilute nitric acid R, mix, allow to stand for

  5 min and filter. The filtrate gives reaction (a) of chlorides (2.3.1).

TESTS

Appearance of solution

The solution is not more opalescent than reference suspension II (2.2.1) and not more

intensely coloured than reference solution GY2  (2.2.2, Method II). If intended for use in the

manufacture of parenteral dosage forms, the solution is clear (2.2.1) and not more intensely

coloured than reference solution GY2  (2.2.2, Method II).

Dissolve 1.0 g in 20 ml of dilute sodium hydroxide solution R.

pH (2.2.3)

3.9 to 4.6.

Dissolve 0.10 g in 50 ml of carbon dioxide-free water R.

Specific optical rotation (2.2.7)

- 125 to - 138 (anhydrous substance).

Dissolve 0.200 g in 20.0 ml of a mixture of equal volumes of acetonitrile R and water R.

Related substances

Liquid chromatography (2.2.29). Carry out the test protected from light.

Solution ADissolve 0.50 g of tetrabutylammonium hydrogen sulphate R and 1.0 g of

potassium dihydrogen phosphate R in about 500 ml of  water R. Add 2 ml of phosphoric acid

R and 0.050 g of anhydrous sodium sulphite R, then dilute to 1000.0 ml with water R.

Test solution (a)Dissolve 50.0 mg of the substance to be examined in solution A and dilute

to 50.0 ml with the same solution.

Test solution (b)Dilute 2.0 ml of test solution (a) to 20.0 ml with solution A.

Reference solution (a)Dissolve 50.0 mg of moxifloxacin hydrochloride CRS in solution A and

dilute to 50.0 ml with the same solution. Dilute 2.0 ml of this solution to 20.0 ml with solution

A.

Reference solution (b)Dissolve 5 mg of moxifloxacin for peak identification CRS (containing

impurities A, B, C, D and E) in solution A and dilute to 5.0 ml with the same solution.

Reference solution (c)Dilute 1.0 ml of test solution (a) to 100.0 ml with solution A. Dilute 1.0

ml of this solution to 10.0 ml with solution A.

Column:

— size: l = 0.25 m, O = 4.6 mm;

— stationary phase: end-capped phenylsilyl silica gel for chromatography R (5 μm);

— temperature: 45 °C.

(C)Crown Copyright 2006                                                                                     2

----------------------- 页面 3-----------------------

— temperature: 45 °C.

Mobile phaseMix 28 volumes of methanol R and 72 volumes of a solution containing 0.5 g/l

of tetrabutylammonium hydrogen sulphate R, 1.0 g/l of potassium dihydrogen phosphate R

and 3.4 g/l of phosphoric acid R.

Flow rate1.3 ml/min.

DetectionSpectrophotometer at 293 nm.

Injection10 μl of test solution (a) and reference solutions (b) and (c).

Run time2.5 times the retention time of moxifloxacin.

Identification of impuritiesUse the chromatogram supplied with moxifloxacin for peak

identification CRS and the chromatogram obtained with reference solution (b) to identify the

peaks due to impurities A, B, C, D and E.

Relative retentionWith reference to moxifloxacin (retention time = about 14 min): impurity A =

about 1.1; impurity B = about 1.3; impurity C = about 1.4; impurity D = about 1.6; impurity E =

about 1.7.

System suitabilityReference solution (b):

— resolution: minimum 1.5 between the peaks due to moxifloxacin and impurity A;

— the chromatogram obtained is similar to the chromatogram supplied with moxifloxacin for

  peak identification CRS.

Limits:

— correction factors: for the calculation of content, multiply the peak areas of the following

  impurities by the corresponding correction factor: impurity B = 1.4; impurity E = 3.5;

— impurities A, B, C, D, E: for each impurity, not more than the area of the principal peak in

  the chromatogram obtained with reference solution (c) (0.1 per cent);

— unspecified impurities: for each impurity, not more than the area of the principal peak in

  the chromatogram obtained with reference solution (c) (0.10 per cent);

— total: not more than 3 times the area of the principal peak in the chromatogram obtained

  with reference solution (c) (0.3 per cent);

— disregard limit: 0.5 times the area of the principal peak in the chromatogram obtained

  with reference solution (c) (0.05 per cent).

Water (2.5.12)

Maximum 4.5 per cent, determined on 0.200 g.

Sulphated ash (2.4.14)

Maximum 0.1 per cent, determined on 1.0 g in a platinum crucible.

ASSAY

Liquid chromatography (2.2.29) as described in the test for related substances with the

following modification.

InjectionTest solution (b) and reference solution (a).

Calculate the percentage content of C       H ClFN O  from the declared content of moxifloxacin

                                          21  25    3  4

hydrochloride CRS.

(C)Crown Copyright 2006                                                                                              3

----------------------- 页面 4-----------------------

STORAGE

In an airtight container , protected from light.

LABELLING

The label states, where applicable, that the substance is suitable for use in the manufacture

of parenteral dosage forms.

IMPURITIES

Specified impuritiesA, B, C, D, E.

A. R = R  = F: 1-cyclopropyl-6,8-difluoro-7-[(4aS,7aS)-octahydro-6H-pyrrolo[3,4-b]pyridin-6-

            ′

  yl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid,

B. R = R  = OCH  : 1-cyclopropyl-6,8-dimethoxy-7-[(4aS,7aS)-octahydro-6H-pyrrolo[3,4-b]

            ′

                     3

  pyridin-6-yl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid,

C. R = F, R  = OC  H : 1-cyclopropyl-8-ethoxy-6-fluoro-7-[(4aS,7aS)-octahydro-6H-pyrrolo[3,

               ′

                        2 5

  4-b]pyridin-6-yl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid,

D. R = OCH , R = F: 1-cyclopropyl-8-fluoro-6-methoxy-7-[(4aS,7aS)-octahydro-6H-pyrrolo

                     ′

               3

  [3,4-b]pyridin-6-yl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid,

E. R = F, R  = OH: 1-cyclopropyl-6-fluoro-8-hydroxy-7-[(4aS,7aS)-octahydro-6H-pyrrolo[3,

               ′

  4-b]pyridin-6-yl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid.

Ph Eur

(C)Crown Copyright 2006                                                                                                             4

----------------------- 页面 5-----------------------

  Browse: British Pharmacopoeia 2009

         British Pharmacopoeia Volume I & II

               Monographs: Medicinal and Pharmaceutical Substances

                  Moxisylyte Hydrochloride

Moxisylyte Hydrochloride

General Notices

C H NO ,HCl315.8964-52-3

  16  25 3

Action and use

Alpha-adrenoceptor antagonist.

Preparation

Moxisylyte Tablets

DEFINITION

Moxisylyte Hydrochloride is 4-(2-dimethylaminoethoxy)-5-isopropyl-2-methylphenyl acetate

hydrochloride. It contains not less than 99.0% and not more than 101.0% of C             H NO ,HCl,

                                                                                    16  25 3

calculated with reference to the dried substance.

CHARACTERISTICS

A white, crystalline powder.

Freely soluble in water and in chloroform; soluble in ethanol (96%); practically insoluble in

ether and in petroleum spirit.

IDENTIFICATION

A. The infrared absorption spectrum, Appendix II A, is concordant with the reference

  spectrum of moxisylyte hydrochloride  (RS 238).

B. Yields reaction A characteristic of chlorides, Appendix VI.

TESTS

Acidity

pH of a 5% w/v solution, 4.5 to 5.5, Appendix V L.

(C)Crown Copyright 2006                                                                                           1

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2楼2010-08-31 10:48:23

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lemonin2008

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fengyan22(金币+5):点编辑有附件上传 2010-09-01 23:04:39

对不住啊，我不知道该怎么上传上去，我的是PDF格式

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