CS215581B1 - A method for determining the content of anthrimides in a drug product - Google Patents
A method for determining the content of anthrimides in a drug product Download PDFInfo
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- CS215581B1 CS215581B1 CS154580A CS154580A CS215581B1 CS 215581 B1 CS215581 B1 CS 215581B1 CS 154580 A CS154580 A CS 154580A CS 154580 A CS154580 A CS 154580A CS 215581 B1 CS215581 B1 CS 215581B1
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Abstract
Vynález se týká způsobu stanovení obsahu antrimidů v technickém výrobku (chemie). Z technického produktu se extrahují nečistoty směsí obsahující toluen-dimetylfonnamid-etanol, tyto se oddělí na krátkém sloupci silikagelu, naadsorbovaný antrimid se rozpustí v koncentrované kyselině sírové a roztok se kolorimetruje. Způsob se využívá pří výrobě autradeinonových berviv.The invention relates to a method for determining the content of anthrimides in a technical product (chemistry). Impurities are extracted from the technical product with a mixture containing toluene-dimethylformamide-ethanol, these are separated on a short column of silica gel, the adsorbed anthrimide is dissolved in concentrated sulfuric acid and the solution is colorimetrically measured. The method is used in the production of autradeinone dyes.
Description
Vynález se týká způsobu stanovení obsahu antrimidú v technickém produktu.The invention relates to a method for determining the anthimide content of a technical product.
Různě substituované dl- a triantrimidy tvoři jednu důležitou skupinu v kategorii antraohinonovýeh barviv, a to převážně jako meziprodukty těchto barviv. Jedná se hlavně o 4,4z-<Ubenzoyldiamino-l,l'-diantrimid, benzimid, 1,4- -triantrimid, 1,5-triantrimid,The variously substituted dl- and triantrimides form one important group in the anthraquinone dye category, mainly as intermediates of these dyes. These are mainly 4,4 z - <Ubenzoyldiamino-1,1'-diantrimide, benzimide, 1,4-triantrimide, 1,5-triantrimide,
1,1'-diantrimid apod.1,1'-diantrimide and the like.
Fři jejich výrobě je zapotřebí zjistit obsah příslušného antrimidu v teóhniokém produktu, aby mohly být vypočteny přídavky dalších chemikálií do následujících reakcí. Teto doposud nebylo možné a další reakoe se prováděly naslepo, protože neexistovala vhodná metoda na jejioh .stanovení. Jediná práce, která se zabývá vůbec analytikou dl- a triantrimidů je od F. Brodmana a epol. (Rev, Chim. Buoharest 14 (1$63) 222j Anal Abstr.To produce these anthimides, the content of the anthimide in the thiourea product must be determined in order to calculate the additions of other chemicals to the following reactions. This has so far not been possible and further reactivations were carried out blindly, as there was no suitable method for determining this. The only work that deals with the analysis of dl- and triantrimides is by F. Brodman and epol. (Rev, Chim. Buoharest 14 ($ 1) 222j Anal Abstr.
(1964) 3211), která se však týká prostého dělení některých antrlmldů papírovou ohromatografií. 0 kvantitativní analýzu se zde nejedná. Analytika těohto látek je neobyčejně ztížena jejioh praktiokou nerozpustností ve většině běžných rozpouštědel. Dokonalé rozpouštědlo v tomto případě je konoentrovená kyselina sírová,(1964) 3211), which relates, however, to the simple separation of some anthracides by paper chromatography. Quantitative analysis is not discussed here. The analysis of these substances is extremely complicated by its practical insolubility in most common solvents. The perfect solvent in this case is concentrated sulfuric acid,
Způsob stanovení antrimidú v technickém produktu spočívá podle vynálezu v tom, že se nečistoty Λ technického produktu extrahují směsí obsahující toluen-di metylformamid-etanol a na chromatografiokém sloupci silikagelu 0,5 až 5 om se oddělí od antrimidu, naadsorbovaný antrimid se rozpustí koncentrovanou kyselinou sírovou a obsah látek v roztoku se stanoví kolorimetricky.The method for the determination of anthimides in the technical product is according to the invention in that the impurities of the technical product are extracted with a mixture containing toluene-dimethylformamide-ethanol and separated from the anthimide on a silica gel chromatography column of 0.5 to 5 µm. and the content of the substances in the solution is determined colorimetrically.
Níže uvedený příklad ilustruje provedení podle vynálezu Příklad provedeníThe example below illustrates an embodiment of the invention
Za účelem stanovení 4,4'-dibenzoyldiamino-l,l -diantrimidu se do 25 ml baničky se zábrusem naváží 0,1000 g rozetřeného vzorku, přidá se 15 ml extrakčního činidla (toluen - 30 % dimetylformamid v etanolu, poměr 10 : 2) a třepe se na třepačce 15 min. Poté se oelý obsah přeleje přes ohromatografioký sloupeo silikagelu vysoký 1 až 1,5 om, kde se zachytí antrimid a odsává se extrakční činidlo. Sloupeo se promyje ještě 75 ml extrakčnlho činidla vždy po 15 ml dávkách. Eluáty je možno jednotlivě jímat a zkoušet tenkovrstvou chromatografií, zda neobsahují již vymývané nečistoty,To determine 4,4'-dibenzoyldiamino-1,1-diantrimide, weigh 0.1000 g of the ground sample into a 25 ml ground-glass flask, add 15 ml of extraction agent (toluene - 30% dimethylformamide in ethanol, 10: 2 ratio) and shake on a shaker for 15 min. The oily content is then passed through a 1 to 1.5 .mu.m silica gel column, where the anthimide is collected and the extractant is aspirated. The column is washed with a further 75 ml of extractant in 15 ml portions. The eluates can be collected individually and tested by thin-layer chromatography for impurities already eluted,
Pak se přes sloupec přelije ooa 100 ml koncentrované kyseliny sírové, která antrimid rozpustí. Eluát se jímá a přelije do 250 ml odměmé baňky, která se pak doplní po značku koncentrovanou kyselinou sírovou. Z tohoto roztoku se pipetuje 3x po 1 ml do 25 ml odměmýoh baněk, které se doplní po značku koncentrovanou kyselinou sírovou. Vzniklé zelenohnědé zabarnení se měří na Langeho kolorimetru při oranžovém filtru <s rozsahem 588 až 833 nm) v 10 ml kyvetě Naměřená extinkoe se porovnává s oejohovní křivkou získanou přesně stejným postupem se standardní látkou.100 ml of concentrated sulfuric acid are then poured over the column to dissolve the anthimide. Collect the eluate and pour into a 250 ml graduated flask, which is then made up to the mark with concentrated sulfuric acid. Pipette 3 ml of this solution into 25 ml volumetric flasks and make up to volume with concentrated sulfuric acid. The resulting greenish-brown coloration is measured on a Lange colorimeter using an orange filter (588-833 nm) in a 10 ml cuvette. The measured extinkoe is compared to the oejohave curve obtained in exactly the same procedure with the standard substance.
Tímto postupem je možno analyzovat veškeré antrimidy, které se za denýoh podmínek sorbují na slikagelu.This procedure can be used to analyze any anthimides which are adsorbed onto slag under the given conditions.
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Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS154580A CS215581B1 (en) | 1980-03-06 | 1980-03-06 | A method for determining the content of anthrimides in a drug product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS154580A CS215581B1 (en) | 1980-03-06 | 1980-03-06 | A method for determining the content of anthrimides in a drug product |
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| Publication Number | Publication Date |
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| CS215581B1 true CS215581B1 (en) | 1982-08-27 |
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| CS154580A CS215581B1 (en) | 1980-03-06 | 1980-03-06 | A method for determining the content of anthrimides in a drug product |
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1980
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