{"id":28316,"date":"2025-11-08T11:47:34","date_gmt":"2025-11-08T04:47:34","guid":{"rendered":"https:\/\/nhathuocngocanh.com\/bp\/?p=28316"},"modified":"2025-11-08T11:47:34","modified_gmt":"2025-11-08T04:47:34","slug":"prednisolone-pivalate","status":"publish","type":"post","link":"https:\/\/nhathuocngocanh.com\/bp\/prednisolone-pivalate\/","title":{"rendered":"Prednisolone Pivalate"},"content":{"rendered":"<p><em>(Ph. Eur. monograph 0736)<\/em><\/p>\n<p>C<sub>26<\/sub>H<sub>36<\/sub>O<sub>6<\/sub> 444.6 1107-99-9<\/p>\n<p><strong>Action and use<\/strong><\/p>\n<p>Glucocorticoid.<\/p>\n<h2>DEFINITION<\/h2>\n<p>11\u03b2,17-Dihydroxy-3,20-dioxopregna-1,4-dien-21-yl 2,2-dimethylpropanoate.<\/p>\n<h3>Content<\/h3>\n<p>97.0 per cent to 103.0 per cent (dried substance).<\/p>\n<h2>CHARACTERS<\/h2>\n<h3>Appearance<\/h3>\n<p>White or almost white, crystalline powder.<\/p>\n<h3>Solubility<\/h3>\n<p>Practically insoluble in water, slightly soluble in ethanol (96 per cent), soluble in methylene chloride.<\/p>\n<h3>mp<\/h3>\n<p>About 229 \u00b0C, with decomposition.<\/p>\n<h2>IDENTIFICATION<\/h2>\n<p>First identification: B, C.<\/p>\n<p>Second identification: A, C, D.<\/p>\n<p>A. Dissolve 10.0 mg in anhydrous ethanol R and dilute to 100.0 mL with the same solvent. Place 2.0 mL of this solution in a ground-glass-stoppered tube, add 10.0 mL of phenylhydrazine-sulfuric acid solution R, mix and heat in a water-bath at 60 \u00b0C for 20 min. Cool immediately. The absorbance (2.2.25) at the absorption maximum at 415 nm is 0.20 to 0.30.<\/p>\n<p>B. Infrared absorption spectrophotometry (2.2.24).<\/p>\n<p>Comparison: prednisolone pivalate CRS.<\/p>\n<p>If the spectra obtained in the solid state show differences, dissolve the substance to be examined and the reference substance separately in the minimum volume of ethanol (96 per cent) R, evaporate to dryness on a water-bath and record new spectra using the residues.<\/p>\n<p>C. Thin-layer chromatography (2.2.27).<\/p>\n<p>Solvent mixture methanol R, methylene chloride R (1:9 V\/V).<\/p>\n<p>Test solution: Dissolve 10 mg of the substance to be examined in the solvent mixture and dilute to 10 mL with the solvent mixture.<\/p>\n<p>Reference solution (a): Dissolve 10 mg of prednisolone pivalate CRS in the solvent mixture and dilute to 10 mL with the solvent mixture.<\/p>\n<p>Reference solution (b): Dissolve 10 mg of prednisolone acetate CRS in the solvent mixture and dilute to 10 mL with the solvent mixture. Dilute 5 mL of this solution to 10 mL with reference solution (a).<\/p>\n<p>Plate: TLC silica gel F254 plate R.<\/p>\n<p>Mobile phase: Add a mixture of 1.2 volumes of water R and 8 volumes of methanol R to a mixture of 15 volumes of ether R and 77 volumes of methylene chloride R.<\/p>\n<p>Application: 5 \u03bcL.<\/p>\n<p>Development: Over a path of 15 cm.<\/p>\n<p>Drying: In air.<\/p>\n<p>Detection A: Examine in ultraviolet light at 254 nm.Results A 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 reference solution (a).<\/p>\n<p>Detection B: Spray with alcoholic solution of sulfuric acid R, heat at 120 \u00b0C for 10 min or until the spots appear, and allow to cool; examine in daylight and in ultraviolet light at 365 nm.<\/p>\n<p>Results B: The principal spot in the chromatogram obtained with the test solution is similar in position, colour in daylight, fluorescence in ultraviolet light at 365 nm and size to the principal spot in the chromatogram obtained with reference solution (a).<\/p>\n<p>System suitability: Reference solution (b):<\/p>\n<p>\u2014 the chromatogram shows 2 clearly separated spots.<\/p>\n<p>D. To 2 mL of sulfuric acid R, add about 2 mg and shake to dissolve. Within 5 min, an intense red colour develops. When examined in ultraviolet light at 365 nm, a reddish-brown fluorescence is seen. Add this solution to 10 mL of water R and mix. The colour fades and there is greenish-yellow fluorescence in ultraviolet light at 365 nm.<\/p>\n<h2>TESTS<\/h2>\n<h3>Specific optical rotation (2.2.7)<\/h3>\n<p>+ 104 to + 112 (dried substance).<\/p>\n<p>Dissolve 0.250 g in dioxan R and dilute to 25.0 mL with the same solvent.<\/p>\n<h3>Related substances<\/h3>\n<p>Liquid chromatography (2.2.29).<\/p>\n<p>Test solution: Dissolve 62.5 mg of the substance to be examined in 2 mL of a mixture of 1 volume of water R and 4 volumes of tetrahydrofuran R and dilute to 25.0 mL with the mobile phase.<\/p>\n<p>Reference solution (a): Dissolve 25 mg of prednisolone acetate CRS, 25 mg of cortisone acetate CRS and 25 mg of prednisolone pivalate CRS in 2 mL of a mixture of 1 volume of water R and 4 volumes of tetrahydrofuran R and dilute to 25.0 mL with the mobile phase. Dilute 1.0 mL of this solution to 25.0 mL with the mobile phase.<\/p>\n<p>Reference solution (b): Dilute 1.0 mL of the test solution to 50.0 mL with the mobile phase.<\/p>\n<p>Column:<\/p>\n<p>\u2014 size: l = 0.15 m, \u00d8 = 4.6 mm;<\/p>\n<p>\u2014 stationary phase: octadecylsilyl silica gel for chromatography R (5 \u03bcm).<\/p>\n<p>Mobile phase: Carefully mix 19 mL of butyl acetate R1 with 37 mL of tetrahydrofuran R and 213 mL of ethylene glycol monomethyl ether R, then add with 231 mL of water R; mix, allow to equilibrate for 1 h and filter through a 0.45 \u03bcm filter.<\/p>\n<p>Flow rate: 1 mL\/min.<\/p>\n<p>Detection: Spectrophotometer at 254 nm.<\/p>\n<p>Equilibration: With the mobile phase for about 30 min.<\/p>\n<p>Injection: 20 \u03bcL.<\/p>\n<p>Run time: 1.5 times the retention time of prednisolone pivalate.<\/p>\n<p>Retention time: Prednisolone acetate = about 3.5 min; cortisone acetate = about 4.5 min; prednisolone pivalate = about13 min.<\/p>\n<p>System suitability: Reference solution (a):<\/p>\n<p>\u2014 resolution: minimum 2.5 between the peaks due to prednisolone acetate and cortisone acetate; if necessary, adjust the concentration of water in the mobile phase.<\/p>\n<p>Limits:<\/p>\n<p>\u2014 any impurity: for each impurity, not more than the area of the principal peak in the chromatogram obtained with reference solution (b) (2.0 per cent), and not more than one such peak has an area greater than 0.5 times the area of the principal peak in the chromatogram obtained with reference solution (b) (1.0 per cent);<\/p>\n<p>\u2014 total: not more than 1.25 times the area of the principal peak in the chromatogram obtained with reference solution (b) (2.5 per cent);<\/p>\n<p>\u2014 disregard limit: 0.025 times the area of the principal peak in the chromatogram obtained with reference solution (b) (0.05 per cent).<\/p>\n<h3>Loss on drying (2.2.32)<\/h3>\n<p>Maximum 0.5 per cent, determined on 1.000 g by drying in an oven at 105 \u00b0C.<\/p>\n<h2>ASSAY<\/h2>\n<p>Dissolve 0.100 g in ethanol (96 per cent) R and dilute to 100.0 mL with the same solvent. Dilute 5.0 mL of this solution to 250.0 mL with ethanol (96 per cent) R. Measure the absorbance (2.2.25) at the absorption maximum at 243 nm.<\/p>\n<p>Calculate the content of C<sub>26<\/sub>H<sub>36<\/sub>O<sub>6<\/sub>6 taking the specific absorbance to be 337.<\/p>\n<h2>STORAGE<\/h2>\n<p>Protected from light.<\/p>\n","protected":false},"excerpt":{"rendered":"<p>(Ph. Eur. monograph 0736) C26H36O6 444.6 1107-99-9 Action and use Glucocorticoid. DEFINITION 11\u03b2,17-Dihydroxy-3,20-dioxopregna-1,4-dien-21-yl 2,2-dimethylpropanoate. Content 97.0 per cent to 103.0 per cent (dried substance). CHARACTERS Appearance White or almost white, crystalline powder. Solubility Practically insoluble in water, slightly soluble in ethanol (96 per cent), soluble in methylene chloride. mp About 229 \u00b0C, with decomposition. IDENTIFICATION&#8230;<\/p>\n","protected":false},"author":4,"featured_media":28322,"comment_status":"open","ping_status":"open","sticky":false,"template":"","format":"standard","meta":{"_acf_changed":false,"footnotes":""},"categories":[174],"tags":[],"class_list":["post-28316","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\/28316","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\/4"}],"replies":[{"embeddable":true,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/comments?post=28316"}],"version-history":[{"count":2,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/posts\/28316\/revisions"}],"predecessor-version":[{"id":28324,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/posts\/28316\/revisions\/28324"}],"wp:featuredmedia":[{"embeddable":true,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/media\/28322"}],"wp:attachment":[{"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/media?parent=28316"}],"wp:term":[{"taxonomy":"category","embeddable":true,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/categories?post=28316"},{"taxonomy":"post_tag","embeddable":true,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/tags?post=28316"}],"curies":[{"name":"wp","href":"https:\/\/api.w.org\/{rel}","templated":true}]}}