{"id":2601,"date":"2025-09-22T14:20:21","date_gmt":"2025-09-22T07:20:21","guid":{"rendered":"https:\/\/nhathuocngocanh.com\/bp\/?p=2601"},"modified":"2025-11-15T12:54:25","modified_gmt":"2025-11-15T05:54:25","slug":"beclometasone-dipropionate-monohydrate","status":"publish","type":"post","link":"https:\/\/nhathuocngocanh.com\/bp\/beclometasone-dipropionate-monohydrate\/","title":{"rendered":"Beclometasone Dipropionate Monohydrate"},"content":{"rendered":"

(Ph. Eur. monograph 1709)<\/p>\n

C28<\/sub>H37<\/sub>ClO7<\/sub>,H2O\u00a0 \u00a0 539.1<\/p>\n

Action and use<\/strong><\/p>\n

Glucocorticoid.<\/p>\n

Preparations<\/p>\n

Beclometasone Aqueous Nasal Spray<\/p>\n

Beclometasone Inhalation Powder<\/p>\n

Beclometasone Inhalation Powder, pre-metered<\/h2>\n

DEFINITION<\/p>\n

9-Chloro-11\u03b2-hydroxy-16\u03b2-methyl-3,20-dioxopregna-1,4-diene-17,21-diyl dipropanoate monohydrate.<\/p>\n

Content<\/h3>\n

97.0 per cent to 102.0 per cent (dried substance).<\/p>\n

CHARACTERS<\/h2>\n

Appearance<\/h3>\n

White or almost white powder.<\/p>\n

Solubility<\/h3>\n

Beclometasone Dipropionate Monohydrate<\/p>\n

Practically insoluble in water, freely soluble in acetone, sparingly soluble in ethanol (96 per cent).<\/p>\n

IDENTIFICATION<\/h2>\n

A. Infrared absorption spectrophotometry (2.2.24).<\/p>\n

Comparison beclometasone dipropionate monohydrate CRS.<\/p>\n

B. Treat 25 mg by the oxygen-flask method (2.5.10). Use a mixture of 1 mL of 1 M sodium hydroxide and 20 mL of water R to absorb the combustion products. The solution gives reaction (a) of chlorides (2.3.1).<\/p>\n

C. Loss on drying (see Tests).<\/p>\n

TESTS<\/h2>\n

Specific optical rotation (2.2.7)<\/h3>\n

+ 108 to + 115 (dried substance).<\/p>\n

Dissolve 0.100 g in ethanol (96 per cent) R and dilute to 10.0 mL with the same solvent.<\/p>\n

Related substances<\/h3>\n

Liquid chromatography (2.2.29).<\/p>\n

Solvent mixture Mobile phase A, mobile phase B (45:55 V\/V).<\/p>\n

Test solution (a): Dissolve 50.0 mg of the substance to be examined in 28 mL of mobile phase B and dilute to 50.0 mL with mobile phase A.<\/p>\n

Test solution (b): Dilute 1.0 mL of test solution (a) to 50.0 mL with the solvent mixture.<\/p>\n

Reference solution (a): Dilute 5.0 mL of test solution (b) to 100.0 mL with the solvent mixture.<\/p>\n

Reference solution (b): Dissolve 5 mg of beclometasone dipropionate for system suitability CRS (containing impurity D) in 3 mL of mobile phase B and dilute to 5 mL with mobile phase A.
\nReference solution (c): Dissolve 5 mg of beclometasone dipropionate for peak identification CRS (containing impurities B, C and L) in 3 mL of mobile phase B and dilute to 5 mL with mobile phase A. Use 1 mL of this solution to dissolve the contents of a vial of beclometasone dipropionate impurities F and N CRS.<\/p>\n

Reference solution (d): Dissolve 50.0 mg of anhydrous beclometasone dipropionate CRS in 28 mL of mobile phase B and dilute to 50.0 mL with mobile phase A. Dilute 1.0 mL of this solution to 50.0 mL with the solvent mixture.<\/p>\n

Column:<\/p>\n

\u2014 size: l = 0.25 m, \u00d8 = 4.6 mm;<\/p>\n

\u2014 stationary phase: spherical difunctional bonded end-capped octadecylsilyl silica gel for chromatography R (5 \u03bcm);<\/p>\n

\u2014 temperature: 50 \u00b0C.<\/p>\n

Mobile phase:<\/p>\n

\u2014 mobile phase A: 2.72 g\/L solution of potassium dihydrogen phosphate R adjusted to pH 2.35 with phosphoric acid R;<\/p>\n

\u2014 mobile phase B: tetrahydrofuran R, acetonitrile R, methanol R (5:23:25 V\/V\/V);<\/p>\n\n\n\n\n\n\n
Time
\n(min)<\/td>\n		Mobile phase A
\n(per cent V\/V)<\/td>\n		Mobile phase B
\n(per cent V\/V)<\/td>\n<\/tr>\n
0 – 4<\/td>\n40<\/td>\n60<\/td>\n<\/tr>\n
4 – 12<\/td>\n\u00a040 \u2192 45<\/td>\n\u00a060 \u2192 55<\/td>\n<\/tr>\n
12 – 59<\/td>\n45<\/td>\n55<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n

Flow rate: 1.4 mL\/min.<\/p>\n

Detection: Spectrophotometer at 254 nm.<\/p>\n

Injection 20 \u03bcl of test solution (a) and reference solutions (a), (b) and (c).<\/p>\n

Identification of impurities: Use the chromatogram supplied with beclometasone dipropionate for peak identification CRS and the chromatogram obtained with reference solution (c) to identify the peaks due to impurities B, C, F and L; use the chromatogram supplied with beclometasone dipropionate for system suitability CRS and the chromatogram obtained with reference solution (b) to identify the peak due to impurity D.
\nRelative retention With reference to beclometasone dipropionate (retention time = about 25 min): impurity B = about 0.6; impurity D = about 1.1; impurity L = about 1.3; impurity C = about 1.8; impurity F = about 2.2.<\/p>\n

System suitability Reference solution (b):<\/p>\n

\u2014 peak-to-valley ratio: minimum 1.5, where Hp = height above the baseline of the peak due to impurity D and Hv = height above the baseline of the lowest point of the curve separating this peak from the peak due to
\nbeclometasone dipropionate.<\/p>\n

Limits:<\/p>\n

\u2014 correction factor: for the calculation of content, multiply the peak area of impurity F by 1.3;<\/p>\n

\u2014 impurity B: not more than 5 times the area of the principal peak in the chromatogram obtained with reference
\nsolution (a) (0.5 per cent);<\/p>\n

\u2014 impurities C, F, L: for each impurity, not more than 1.5 times the area of the principal peak in the chromatogram obtained with reference solution (a) (0.15 per cent);<\/p>\n

\u2014 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);<\/p>\n

\u2014 total: not more than 10 times the area of the principal peak in the chromatogram obtained with reference
\nsolution (a) (1.0 per cent);<\/p>\n

\u2014 disregard limit: 0.5 times the area of the principal peak in the chromatogram obtained with reference solution (a) (0.05 per cent).<\/p>\n

Loss on drying (2.2.32)<\/h4>\n

2.8 per cent to 3.8 per cent, determined on 1.000 g by drying in an oven at 105 \u00b0C for 3 h.<\/p>\n

ASSAY<\/h2>\n

Liquid chromatography (2.2.29) as described in the test for related substances with the following modification.
\nInjection Test solution (b) and reference solution (d).<\/p>\n

Calculate the percentage content of C28<\/sub>H37<\/sub>ClO7<\/sub> from the declared content of anhydrous beclometasone dipropionate CRS.<\/p>\n

IMPURITIES<\/p>\n

Specified impurities B, C, F, L.<\/p>\n

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, D, E, H, I, J, M, N, O, Q, R, S, U, V.<\/p>\n

\"Beclometasone<\/p>\n

A. 9-chloro-11\u03b2,17-dihydroxy-16\u03b2-methyl-3,20-dioxopregna-1,4-dien-21-yl propanoate (beclometasone 21-propionate),<\/p>\n

\"Beclometasone<\/p>\n

B. 21-(acetyloxy)-9-chloro-11\u03b2-hydroxy-16\u03b2-methyl-3,20-dioxopregna-1,4-dien-17-yl propanoate (beclometasone 21-acetate 17-propionate),<\/p>\n

\"Beclometasone<\/p>\n

C. 9-chloro-11\u03b2-hydroxy-16\u03b2-methyl-3,20-dioxo-17-(propanoyloxy)-pregna-1,4-dien-21-yl butanoate (beclometasone 21-butyrate 17-propionate),<\/p>\n

\"Beclometasone<\/p>\n

D. 9-bromo-11\u03b2-hydroxy-16\u03b2-methyl-3,20-dioxopregna-1,4-diene-17,21-diyl dipropanoate,<\/p>\n

\"Beclometasone<\/p>\n

E. 6\u03b1,9-dichloro-11\u03b2-hydroxy-16\u03b2-methyl-3,20-dioxopregna-1,4-diene-17,21-diyl dipropanoate,<\/p>\n

\"Beclometasone<\/p>\n

F. 6\u03b1-bromo-9-chloro-11\u03b2-hydroxy-16\u03b2-methyl-3,20-dioxopregna-1,4-diene-17,21-diyl dipropanoate,<\/p>\n

\"Beclometasone<\/p>\n

H. 9-chloro-11\u03b2,21-dihydroxy-16\u03b2-methyl-3,20-dioxopregna-1,4-dien-17-yl propanoate (beclometasone 17-propionate),<\/p>\n

\"Beclometasone<\/p>\n

I. 16\u03b2-methyl-3,20-dioxopregna-1,4,9(11)-triene-17,21-diyl dipropanoate,<\/p>\n

\"Beclometasone<\/p>\n

J. 9,11\u03b2-epoxy-16\u03b2-methyl-3,20-dioxo-9\u03b2-pregna-1,4-diene-17,21-diyl dipropanoate,<\/p>\n

\"Beclometasone<\/p>\n

L. 9-chloro-11\u03b2-hydroxy-16\u03b2-methyl-3,20-dioxopregn-4-ene-17,21-diyl dipropanoate,<\/p>\n

\"Beclometasone<\/p>\n

M. 9-chloro-11\u03b2-hydroxy-16\u03b2-methyl-3,20-dioxopregna-4,6-diene-17,21-diyl dipropanoate,<\/p>\n

\"Beclometasone<\/p>\n

N. 2-bromo-9-chloro-11\u03b2-hydroxy-16\u03b2-methyl-3,20-dioxopregna-1,4-diene-17,21-diyl dipropanoate,<\/p>\n

\"Beclometasone<\/p>\n

O. 9,11\u03b2-dichloro-16\u03b2-methyl-3,20-dioxopregna-1,4-diene-17,21-diyl dipropanoate,<\/p>\n

\"Beclometasone<\/p>\n

Q. 16\u03b2-methyl-3,20-dioxopregna-1,4-diene-17,21-diyl dipropanoate,<\/p>\n

\"Beclometasone<\/p>\n

R. 9,11\u03b2-epoxy-17,21-dihydroxy-16\u03b2-methyl-9\u03b2-pregna-1,4-diene-3,20-dione,<\/p>\n

\"Beclometasone<\/p>\n

S. 9-chloro-16\u03b2-methyl-3,20-dioxopregna-1,4-diene-11\u03b2,17,21-triyl tripropanoate (beclometasone tripropionate),<\/p>\n

\"Beclometasone<\/p>\n

U. 9,11\u03b2-epoxy-21-hydroxy-16\u03b2-methyl-3,20-dioxo-9\u03b2-pregna-1,4-dien-17-yl propanoate,<\/p>\n

\"Beclometasone<\/p>\n

V. 9,11\u03b2-epoxy-17-hydroxy-16\u03b2-methyl-3,20-dioxo-9\u03b2-pregna-1,4-dien-21-yl propanoate.<\/p>\n","protected":false},"excerpt":{"rendered":"

(Ph. Eur. monograph 1709) C28H37ClO7,H2O\u00a0 \u00a0 539.1 Action and use Glucocorticoid. Preparations Beclometasone Aqueous Nasal Spray Beclometasone Inhalation Powder Beclometasone Inhalation Powder, pre-metered DEFINITION 9-Chloro-11\u03b2-hydroxy-16\u03b2-methyl-3,20-dioxopregna-1,4-diene-17,21-diyl dipropanoate monohydrate. Content 97.0 per cent to 102.0 per cent (dried substance). CHARACTERS Appearance White or almost white powder. Solubility Beclometasone Dipropionate Monohydrate Practically insoluble in water, freely soluble in…<\/p>\n","protected":false},"author":3,"featured_media":2642,"comment_status":"open","ping_status":"open","sticky":false,"template":"","format":"standard","meta":{"_acf_changed":false,"footnotes":""},"categories":[174],"tags":[],"class_list":["post-2601","post","type-post","status-publish","format-standard","has-post-thumbnail","hentry","category-medicinal-substances"],"acf":[],"_links":{"self":[{"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/posts\/2601","targetHints":{"allow":["GET"]}}],"collection":[{"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/posts"}],"about":[{"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/types\/post"}],"author":[{"embeddable":true,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/users\/3"}],"replies":[{"embeddable":true,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/comments?post=2601"}],"version-history":[{"count":5,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/posts\/2601\/revisions"}],"predecessor-version":[{"id":7752,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/posts\/2601\/revisions\/7752"}],"wp:featuredmedia":[{"embeddable":true,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/media\/2642"}],"wp:attachment":[{"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/media?parent=2601"}],"wp:term":[{"taxonomy":"category","embeddable":true,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/categories?post=2601"},{"taxonomy":"post_tag","embeddable":true,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/tags?post=2601"}],"curies":[{"name":"wp","href":"https:\/\/api.w.org\/{rel}","templated":true}]}}