{"id":1132,"date":"2025-09-18T09:58:23","date_gmt":"2025-09-18T02:58:23","guid":{"rendered":"https:\/\/nhathuocngocanh.com\/bp\/?p=1132"},"modified":"2025-10-02T16:53:53","modified_gmt":"2025-10-02T09:53:53","slug":"aceclofenac","status":"publish","type":"post","link":"https:\/\/nhathuocngocanh.com\/bp\/aceclofenac\/","title":{"rendered":"Aceclofenac"},"content":{"rendered":"

(Ph. Eur. monograph 1281)<\/p>\n

C16<\/sub>H13<\/sub>Cl2<\/sub>NO4<\/sub>\u00a0 \u00a0 \u00a0 354.2\u00a0 \u00a0 \u00a0 89796-99-6<\/p>\n

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

Cyclo-oxygenase inhibitor; analgesic; anti-inflammatory.<\/p>\n

DEFINITION<\/h2>\n[[[2-[(2,6-Dichlorophenyl)amino]phenyl]acetyl]oxy]acetic acid.<\/p>\n

Content<\/h3>\n

99.0 per cent to 101.0 per cent (dried substance).<\/p>\n

CHARACTERS<\/h2>\n

Appearance<\/h3>\n

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

Solubility<\/h3>\n

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

IDENTIFICATION<\/h2>\n

First identification: B.<\/p>\n

Second identification: A, C.<\/p>\n

Aceclofenac<\/p>\n

A. Ultraviolet and visible absorption spectrophotometry (2.2.25).<\/p>\n

Test solution: Dissolve 50.0 mg in methanol R and dilute to 100.0 mL with the same solvent. Dilute 2.0 mL of the solution to 50.0 mL with methanol R.<\/p>\n

Spectral range: 220-370 nm.<\/p>\n

Absorption maximum: 275 nm.<\/p>\n

Specific absorbance: at the absorption maximum 320 to 350.<\/p>\n

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

Comparison: Ph. Eur. reference spectrum of aceclofenac.<\/p>\n

C. Dissolve about 10 mg in 10 mL of ethanol (96 per cent) R. To 1 mL of the solution, add 0.2 mL of a mixture, prepared immediately before use, of equal volumes of a 6 g\/L solution of potassium ferricyanide R and a 9 g\/L solution of ferric chloride R. Allow to stand protected from light for 5 min. Add 3 mL of a 10.0 g\/L solution of hydrochloric acid R. Allow to stand protected from light for 15 min. A blue colour develops and a precipitate is formed.<\/p>\n

TESTS<\/h2>\n

Related substances<\/h3>\n

Liquid chromatography (2.2.29). Prepare the solutions immediately before use.<\/p>\n

Solvent mixture Mobile phase A, mobile phase B (30:70 V\/V).<\/p>\n

Test solution Dissolve 50.0 mg of the substance to be examined in the solvent mixture and dilute to 25.0 mL with the solvent mixture.<\/p>\n

Reference solution (a): Dissolve 21.6 mg of diclofenac sodium CRS (impurity A) in the solvent mixture and dilute to 50.0 mL with the solvent mixture.<\/p>\n

Reference solution (b): Dilute 2.0 mL of the test solution to 10.0 mL with the solvent mixture.<\/p>\n

Reference solution (c): Mix 1.0 mL of reference solution (a) and 1.0 mL of reference solution (b) and dilute to 100.0 mL with the solvent mixture.<\/p>\n

Reference solution (d): Dissolve 4.0 mg of aceclofenac impurity F CRS in the solvent mixture and dilute to 10.0 mL with the solvent mixture.<\/p>\n

Reference solution (e): Dissolve 2.0 mg of aceclofenac impurity H CRS in the solvent mixture and dilute to 10.0 mL with the solvent mixture.<\/p>\n

Reference solution (f): Mix 1.0 mL of reference solution (b), 1.0 mL of reference solution (d) and 1.0 mL of reference solution (e) and dilute to 100.0 mL with the solvent mixture.<\/p>\n

Reference solution (g): Dissolve 5.0 mg of aceclofenac impurity I CRS in the solvent mixture and dilute to 50.0 mL with solvent mixture. Dilute 1.0 mL of the solution to 50.0 mL with the solvent mixture.<\/p>\n

Reference solution (h): Dissolve 4 mg of aceclofenac for peak identification CRS (containing impurities B, C, D, E and G) in 2 mL of the solvent mixture.<\/p>\n

Column:<\/p>\n

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

\u2014 stationary phase: spherical end-capped octadecylsilyl silica gel for chromatography R (5 \u03bcm) with a pore size of 10 nm and a carbon loading of 19 per cent;<\/p>\n

\u2014 temperature: 40 \u00b0C.<\/p>\n

Mobile phase:<\/p>\n

\u2014 mobile phase A: 1.12 g\/L solution of phosphoric acid R adjusted to pH 7.0 with a 42 g\/L solution of sodium hydroxide R;<\/p>\n

\u2014 mobile phase B: water R, acetonitrile R (10:90 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 – 25<\/td>\n\u00a070 \u2192 50<\/td>\n\u00a030 \u2192 50<\/td>\n<\/tr>\n
25 – 30<\/td>\n\u00a050 \u2192 20<\/td>\n\u00a050 \u2192 80<\/td>\n<\/tr>\n
30 – 50<\/td>\n\u00a020<\/td>\n\u00a080<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n

Flow rate 1.0 mL\/min.<\/p>\n

Detection Spectrophotometer at 275 nm.<\/p>\n

Injection 10 \u03bcL of the test solution and reference solutions (c), (d), (e), (f), (g) and (h).<\/p>\n

Identification of impurities Use the chromatogram obtained with reference solution (c) to identify the peak due to impurity A; use the chromatogram supplied with aceclofenac for peak identification CRS and the chromatogram obtained with reference solution (h) to identify the peaks due to impurities B, C, D, E and G; use the chromatogram obtained with reference solution (d) to identify the peak due to impurity F; use the chromatogram obtained with reference solution (e) to identify the peak due to impurity H; use the chromatogram obtained with reference solution (g) to identify the peak due to impurity I.<\/p>\n

Relative retention With reference to aceclofenac (retention time = about 11 min): impurity A = about 0.8;<\/p>\n

impurity G = about 1.3; impurity H = about 1.5; impurity I = about 2.3; impurity D = about 3.1; impurity B = about 3.2;<\/p>\n

impurity E = about 3.3; impurity C = about 3.5; impurity F = about 3.7.<\/p>\n

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

\u2014 resolution: minimum 5.0 between the peaks due to impurity A and aceclofenac.<\/p>\n

Limits:<\/p>\n

\u2014 impurity A: not more than the area of the corresponding peak in the chromatogram obtained with reference solution (c) (0.2 per cent);<\/p>\n

\u2014 impurities B, C, D, E, G: for each impurity, not more than the area of the peak due to aceclofenac in the chromatogram obtained with reference solution (f) (0.2 per cent);<\/p>\n

\u2014 impurity F: not more than the area of the corresponding peak in the chromatogram obtained with reference solution (f) (0.2 per cent);<\/p>\n

\u2014 impurity H: not more than 1.5 times the area of the corresponding peak in the chromatogram obtained with reference solution (f) (0.15 per cent);<\/p>\n

\u2014 impurity I: not more than 1.5 times the area of the corresponding peak in the chromatogram obtained with reference solution (g) (0.15 per cent);<\/p>\n

\u2014 unspecified impurities: for each impurity, not more than 0.5 times the area of the peak due to aceclofenac in the chromatogram obtained with reference solution (f) (0.10 per cent);<\/p>\n

\u2014 total: maximum 0.7 per cent;<\/p>\n

\u2014 disregard limit: 0.25 times the area of the peak due to aceclofenac in the chromatogram obtained with reference solution (f) (0.05 per cent).<\/p>\n

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

Maximum 0.5 per cent, determined on 1.000 g by drying in an oven at 105 \u00b0C.<\/p>\n

Sulfated ash (2.4.14)<\/h4>\n

Maximum 0.1 per cent, determined on 1.0 g.<\/p>\n

ASSAY<\/h2>\n

Dissolve 0.300 g in 40 mL of methanol R. Titrate with 0.1 M sodium hydroxide, determining the end-point potentiometrically (2.2.20).<\/p>\n

1 mL of 0.1 M sodium hydroxide is equivalent to 35.42 mg of C16<\/sub>H13<\/sub>Cl2<\/sub>NO4<\/sub><\/p>\n

STORAGE<\/h2>\n

Protected from light.<\/p>\n

IMPURITIES<\/h2>\n

Specified impurities A, B, C, D, E, F, G, H, I.<\/p>\n

\"Aceclofenac\"<\/p>\n

A. [2-[(2,6-dichlorophenyl)amino]phenyl]acetic acid (diclofenac),<\/p>\n

\"Aceclofenac\"<\/p>\n

B. methyl [2-[(2,6-dichlorophenyl)amino]phenyl]acetate (methyl ester of diclofenac),<\/p>\n

\"Aceclofenac\"<\/p>\n

C. ethyl [2-[(2,6-dichlorophenyl)amino]phenyl]acetate (ethyl ester of diclofenac),<\/p>\n

\"Aceclofenac\"<\/p>\n

D. methyl [[[2-[(2,6-dichlorophenyl)amino]phenyl]acetyl]oxy]acetate (methyl ester of aceclofenac),<\/p>\n

\"Aceclofenac\"<\/p>\n

E. ethyl [[[2-[(2,6-dichlorophenyl)amino]phenyl]acetyl]oxy]acetate (ethyl ester of aceclofenac),<\/p>\n

\"Aceclofenac\"<\/p>\n

F. benzyl [[[2-[(2,6-dichlorophenyl)amino]phenyl]acetyl]oxy]acetate (benzyl ester of aceclofenac),<\/p>\n

\"Aceclofenac\"<\/p>\n

G. [[[[[2-[(2,6-dichlorophenyl)amino]phenyl]acetyl]oxy]acetyl]oxy]acetic acid (acetic aceclofenac),<\/p>\n

\"Aceclofenac\"<\/p>\n

H. [[[[[[[2-[(2,6-dichlorophenyl)amino]phenyl]acetyl]oxy]acetyl]oxy]acetyl]oxy]acetic acid (diacetic aceclofenac),<\/p>\n

\"Aceclofenac\"<\/p>\n

I. 1-(2,6-dichlorophenyl)-1,3-dihydro-2H-indol-2-one.<\/p>\n","protected":false},"excerpt":{"rendered":"

(Ph. Eur. monograph 1281) C16H13Cl2NO4\u00a0 \u00a0 \u00a0 354.2\u00a0 \u00a0 \u00a0 89796-99-6 Action and use Cyclo-oxygenase inhibitor; analgesic; anti-inflammatory. DEFINITION [[[2-[(2,6-Dichlorophenyl)amino]phenyl]acetyl]oxy]acetic acid. Content 99.0 per cent to 101.0 per cent (dried substance). CHARACTERS Appearance White or almost white, crystalline powder. Solubility Practically insoluble in water, freely soluble in acetone, soluble in ethanol (96 per cent). IDENTIFICATION…<\/p>\n","protected":false},"author":2,"featured_media":1134,"comment_status":"open","ping_status":"open","sticky":false,"template":"","format":"standard","meta":{"_acf_changed":false,"footnotes":""},"categories":[174],"tags":[],"class_list":["post-1132","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\/1132","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\/2"}],"replies":[{"embeddable":true,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/comments?post=1132"}],"version-history":[{"count":6,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/posts\/1132\/revisions"}],"predecessor-version":[{"id":6884,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/posts\/1132\/revisions\/6884"}],"wp:featuredmedia":[{"embeddable":true,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/media\/1134"}],"wp:attachment":[{"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/media?parent=1132"}],"wp:term":[{"taxonomy":"category","embeddable":true,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/categories?post=1132"},{"taxonomy":"post_tag","embeddable":true,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/tags?post=1132"}],"curies":[{"name":"wp","href":"https:\/\/api.w.org\/{rel}","templated":true}]}}