Edition: BP 2025 (Ph. Eur. 11.6 update)<\/p>\n
C21<\/sub>H24<\/sub>ClN2<\/sub>NaO4<\/sub>S 458.9 30123-17-2<\/p>\n Action and use<\/strong><\/p>\n Antidepressant.<\/p>\n Sodium 7-[[(11RS)-3-chloro-6-methyl-6,11-dihydrodibenzo[c,f][1,2]thiazepin-11-yl]amino]heptanoate S,S-dioxide.<\/p>\n Content<\/strong><\/p>\n 99.0 per cent to 101.0 per cent (anhydrous substance).<\/p>\n White or yellowish powder, very hygroscopic.<\/p>\n Freely soluble in water, in methanol and in methylene chloride.<\/p>\n A. Infrared absorption spectrophotometry (2.2.24).<\/p>\n Comparison Ph. Eur. reference spectrum of tianeptine sodium.<\/p>\n B. It gives reaction (a) of sodium (2.3.1).<\/p>\n Gas chromatography (2.2.28).<\/p>\n Internal standard solution Dilute 1 mL of ethyl 5-bromovalerate R in anhydrous ethanol R and dilute to 100.0 mL with the same solvent. Dilute 1.0 mL of the solution to 250.0 mL with anhydrous ethanol R.<\/p>\n Test solution Dissolve 0.1000 g of the substance to be examined in the internal standard solution and dilute to 2.0 mL with the same solution.<\/p>\n Reference solution Dissolve 10.0 mg of tianeptine impurity A CRS in the internal standard solution and dilute to 200.0 mL with the same solution.<\/p>\n Column:<\/p>\n \u2014 material: fused silica,<\/p>\n \u2014 size: l = 25 m, \u00d8 = 0.25 mm,<\/p>\n \u2014 stationary phase: cyanopropylpolysiloxane R (film thickness 0.2 \u03bcm).<\/p>\n Carrier gas helium for chromatography R.<\/p>\n Linear velocity 26 cm\/s.<\/p>\n Split ratio 1:100.<\/p>\n Temperature:<\/p>\n \u2014 column: 150 \u00b0C,<\/p>\n \u2014 injection port and detector: 210 \u00b0C.<\/p>\n Detection Flame ionisation.<\/p>\n Injection 1 \u03bcL.<\/p>\n Run time Twice the retention time of ethyl 5-bromovalerate.<\/p>\n System suitability Reference solution:<\/p>\n \u2014 elution order: ethanol, ethyl 5-bromovalerate, impurity A,<\/p>\n \u2014 resolution: minimum 10 between the peaks due to ethyl 5-bromovalerate and impurity A,<\/p>\n \u2014 signal-to-noise ratio: minimum 20 for the peak due to impurity A.<\/p>\n Limit:<\/p>\n \u2014 impurity A: not more than the area of the corresponding peak in the chromatogram obtained with the reference solution (0.1 per cent).<\/p>\n Liquid chromatography (2.2.29).<\/p>\n Solvent mixture Mix 50 volumes of methanol R and 50 volumes of water R.<\/p>\n Test solution Dissolve 50.0 mg of the substance to be examined in the solvent mixture and dilute to 50.0 mL with the solvent mixture.<\/p>\n Reference solution (a) Dilute 1.0 mL of the test solution to 100.0 mL with the solvent mixture. Dilute 1.0 mL of this solution to 20.0 mL with the solvent mixture.<\/p>\n Reference solution (b) Dissolve 20 mg of sodium tianeptine for system suitability CRS in the solvent mixture and dilute to 200 mL with the solvent mixture.<\/p>\n Column:<\/p>\n \u2014 size: l = 0.15 m, \u00d8 = 4.6 mm,<\/p>\n \u2014 stationary phase: octadecylsilyl silica gel for chromatography R (3 \u03bcm) with a pore size of 0.01 \u03bcm,<\/p>\n \u2014 temperature: 30 \u00b0C.<\/p>\n Mobile phase:<\/p>\n \u2014 mobile phase A: mix 21 volumes of methanol R1, 31.5 volumes of acetonitrile R1 and 47.5 volumes of a 2 g\/L solution of sodium laurilsulfate R, adjusted to pH 2.5 with phosphoric acid R,<\/p>\n \u2014 mobile phase B: mix 20 volumes of methanol R1, 20 volumes of a 2 g\/L solution of sodium laurilsulfate R, adjusted to pH 2.5 with phosphoric acid R and 60 volumes of acetonitrile R1,<\/p>\n (min)<\/strong><\/td>\n (per cent V\/V)<\/strong><\/td>\n (per cent V\/V)<\/strong><\/td>\n<\/tr>\n 35 – 45<\/p>\n 45 – 60<\/p>\n 60 – 70<\/td>\n 100 \u2192 40<\/p>\n 40<\/p>\n 40 \u2192 100<\/td>\n 0 \u2192 60<\/p>\n 60<\/p>\n 60 \u2192 0<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n Flow rate 1 mL\/min.<\/p>\n Detection Spectrophotometer at 220 nm.<\/p>\n Injection 10 \u03bcL.<\/p>\n Relative retention with reference to tianeptine (retention time = about 30 min): impurity C = about 0.4; impurity D1 = about 0.6; impurity D2 = about 0.8; impurity E = about 1.1; impurity B = about 1.7.<\/p>\n System suitability Reference solution (b):<\/p>\n \u2014 resolution: minimum 2.5 between the peaks due to tianeptine and impurity E.<\/p>\n Limits:<\/p>\n \u2014 any impurity: not more than twice the area of the principal peak in the chromatogram obtained with reference \u2014 total: not more than 8 times the area of the principal peak in the chromatogram obtained with reference solution (a) (0.4 per cent),<\/p>\n \u2014 disregard limit: area of the principal peak in the chromatogram obtained with reference solution (a) (0.05 per cent).<\/p>\n Water (2.5.12)<\/p>\n Maximum 5.0 per cent, determined on 0.100 g.<\/p>\n Dissolve 0.165 g in 50 mL of anhydrous acetic acid R. Titrate with 0.1 M perchloric acid, determining the end-point potentiometrically (2.2.20).<\/p>\n 1 mL of 0.1 M perchloric acid is equivalent to 22.95 mg of C21H24ClN2NaO4S.<\/p>\n In an airtight container.<\/p>\n A. ethyl 7-bromoheptanoate,<\/p>\n B. ethyl 7-[[(11RS)-3-chloro-6-methyl-6,11-dihydrodibenzo[c,f][1,2]thiazepin-11-yl]amino]heptanoate S,S-dioxide,<\/p>\n C. 3-chloro-6-methyldibenzo[c,f][1,2]thiazepin-11(6H)-one S,S-dioxide,<\/p>\n D. 7-[[(11RS)-3-chloro-6-methyldibenzo[c,f][1,2]thiazepin-11(6H)-ylidene]amino]heptanoic acid S,S-dioxide,<\/p>\n E. 7,7\u2032-[[(11RS)-3-chloro-6-methyl-6,11-dihydrodibenzo[c,f][1,2]thiazepin-11-yl]imino]diheptanoic acid S,S-dioxide.<\/p>\n","protected":false},"excerpt":{"rendered":" Edition: BP 2025 (Ph. Eur. 11.6 update) C21H24ClN2NaO4S 458.9 30123-17-2 Action and use Antidepressant. DEFINITION Sodium 7-[[(11RS)-3-chloro-6-methyl-6,11-dihydrodibenzo[c,f][1,2]thiazepin-11-yl]amino]heptanoate S,S-dioxide. Content 99.0 per cent to 101.0 per cent (anhydrous substance). CHARACTERS Appearance White or yellowish powder, very hygroscopic. Solubility Freely soluble in water, in methanol and in methylene chloride. IDENTIFICATION A. Infrared absorption spectrophotometry (2.2.24). Comparison Ph….<\/p>\n","protected":false},"author":5,"featured_media":31024,"comment_status":"open","ping_status":"open","sticky":false,"template":"","format":"standard","meta":{"_acf_changed":false,"footnotes":""},"categories":[174],"tags":[],"class_list":["post-30972","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\/30972","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\/5"}],"replies":[{"embeddable":true,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/comments?post=30972"}],"version-history":[{"count":2,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/posts\/30972\/revisions"}],"predecessor-version":[{"id":31032,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/posts\/30972\/revisions\/31032"}],"wp:featuredmedia":[{"embeddable":true,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/media\/31024"}],"wp:attachment":[{"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/media?parent=30972"}],"wp:term":[{"taxonomy":"category","embeddable":true,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/categories?post=30972"},{"taxonomy":"post_tag","embeddable":true,"href":"https:\/\/nhathuocngocanh.com\/bp\/wp-json\/wp\/v2\/tags?post=30972"}],"curies":[{"name":"wp","href":"https:\/\/api.w.org\/{rel}","templated":true}]}}DEFINITION<\/h2>\n
CHARACTERS<\/h2>\n
Appearance<\/h3>\n
Solubility<\/h3>\n
IDENTIFICATION<\/h2>\n
TESTS<\/h2>\n
Impurity A<\/h3>\n
Related substances<\/h3>\n
\n\n
\n Time<\/strong><\/p>\n Mobile phase A<\/strong><\/p>\n Mobile phase B<\/strong><\/p>\n \n 0 – 35<\/p>\n 100<\/p>\n 0<\/p>\n
\nsolution (a) (0.1 per cent),<\/p>\nASSAY<\/h2>\n
STORAGE<\/h2>\n
IMPURITIES<\/h2>\n