CS262269B1 - Method for the determination of (2,5-dioxo-4-imidazolidines) -moxyne in the presence of a complex of iodine with polyvinylpyrrolidone - Google Patents
Method for the determination of (2,5-dioxo-4-imidazolidines) -moxyne in the presence of a complex of iodine with polyvinylpyrrolidone Download PDFInfo
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- CS262269B1 CS262269B1 CS867537A CS753786A CS262269B1 CS 262269 B1 CS262269 B1 CS 262269B1 CS 867537 A CS867537 A CS 867537A CS 753786 A CS753786 A CS 753786A CS 262269 B1 CS262269 B1 CS 262269B1
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- polyvinylpyrrolidone
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Abstract
Řešení se týká stanovení (2,5-dioxo- -4-imidazolidinyl)močoviny ve farmaceutických přípravcích, obsahujících komplex jódu s polyvinylpyrolidonem, který je většinou v nadbytku. Komplex jódu s polyvinylpyrolidonem se naadsorbuje na silikagel s kovalentně vázanými alkylovými skupinami a bezbarvý roztok se analyzuje kapalinovou chromatografií.The solution concerns the determination of (2,5-dioxo-4-imidazolidinyl)urea in pharmaceutical preparations containing an iodine complex with polyvinylpyrrolidone, which is usually in excess. The iodine complex with polyvinylpyrrolidone is adsorbed onto silica gel with covalently bound alkyl groups and the colorless solution is analyzed by liquid chromatography.
Description
Vynález se týká stanovení (2,5-dioxo-imidazolyl)močoviny (též 5-ureido-hydatoin respektive glyoxyldiureid, dále jen allantoin) v přítomnosti komplexu jódu s polyvinylpyrolidonem.The invention relates to the determination of (2,5-dioxo-imidazolyl) urea (also 5-ureido-hydatoin and glyoxyldiureide, hereinafter allantoin) in the presence of an iodine-polyvinylpyrrolidone complex.
Stanovení allantoinu ve farmaceutických přípravcích se provádí různými způsoby. Některá stanovení jsou založena na kolorimetrickém stanovení hydrolytických produktů allantoinu (E. Young, C. Conway: J. Biol. Chem. 142, 839 (1942); S. A. Katz, R. Turse, S. B. Mecca:The determination of allantoin in pharmaceutical preparations is carried out in various ways. Some assays are based on the colorimetric determination of allantoin hydrolytic products (E. Young, C. Conway, J. Biol. Chem. 142, 839 (1942); S.A. Katz, R.Turse, S. B. Mecca:
J. Soc. Cosmet. Chem. 15, 303 (1964); D. Zygmunt: Farm. Pol. 25, 255 (1969)). Podobně je popsáno fluorimetrické stanoveni kyseliny glyoxalové jako rozkladného produktu allantoinu (T. Kaito, K. Sagara, Y. Ito, K. Nakamura, T. Anno: Yakugaku Zasshi 97, 165 (1977)). Dále byl allantoin stanovován titračně (D. J. Weber, J. W. Higgins: J. Pharm. Sci. 59, 1 819 (1970);J. Soc. Cosmet. Chem. 15, 303 (1964); D. Zygmunt, Farm. Pole. 25, 255 (1969)). Similarly, a fluorimetric determination of glyoxalic acid as a decomposition product of allantoin is described (T. Kaito, K. Sagara, Y. Ito, K. Nakamura, T. Anno, Yakugaku Zasshi 97, 165 (1977)). Further, allantoin was determined by titration (D.J. Weber, J.W. Higgins: J. Pharm. Sci. 59, 1819 (1970);
A. Billabert, J. Willemot, G. Parry: Ann. Pharm. Fr. 34, 65 (1976)), tenkovrstevnou chromatografií (I. Bonadeo, G. Bottezzi: Riv. Ital. Essenzy Profumi 50, 78 (1968); J. Lutomski,Billabert A., Willemot J., Parry G.: Ann. Pharm. Fr. 34, 65 (1976)), by thin-layer chromatography (I. Bonadeo, G. Bottezzi: Riv. Ital. Essenzy Profumi 50, 78 (1968); J. Lutomski,
B. Jernas: Pharmazie 31, 131 (1976)) a vysokoúčinnou kapalinovou chromatografií (Z. R. Zaidi,B. Jernas: Pharmazie 31, 131 (1976)) and high performance liquid chromatography (Z. R. Zaidi,
F. J. Sena, C. P. Basilio: J. Pharm. Sci. 71, 997 (1982); J. Kawase, H. Weno, K. Tsuji:F. J. Sena, C. P. Basilio: J. Pharm. Sci. 71, 997 (1982); J. Kawase, H. Weno, and K. Tsuji:
J. Chromatogr. 253, 237 (1982)).J. Chromatogr. 253, 237 (1982)).
Žádný z uvedených způsobů stanovení však nedokáže stanovit allantoin vedle přebytku komplexu jódu s polyvinylpyrolidonem (5 až 25násobného). Dokonce ani redukce jódu na jodid pomocí thiosíranu sodného nepomohla vyřešit daný problém.However, none of these assay methods can detect allantoin in addition to the excess iodine / polyvinylpyrrolidone complex (5 to 25 fold). Even the reduction of iodine to iodide with sodium thiosulfate did not help solve the problem.
Způsob podle vynálezu se provádí tak, že se vzorek s přebytkem komplexu jódu s polyvinylpyrolidonem převede na kolonu s vhodným sorbentem, jako například silikagelem s kovalentně vázanými oktadecylovými nebo oktylovými skupinami. Na sorbentu dojde k adsorbci komplexu jódu s polyvinylpyrolidonem a všechen allantoin je eluován vhodným eluentem, například destilovanou vodou. Eluát je nakonec analyzován kapalinovou chromatografií na koloně naplněné silikagelovým sorbentem s kovalentně vázanými aminopropylovými skupinami.The process of the invention is carried out by converting a sample with an excess of the iodine-polyvinylpyrrolidone complex to a column with a suitable sorbent, such as silica gel with covalently bonded octadecyl or octyl groups. The iodine complex with polyvinylpyrrolidone is adsorbed on the sorbent and all allantoin is eluted with a suitable eluent, for example distilled water. The eluate is finally analyzed by liquid chromatography on a column packed with silica gel sorbent with covalently bonded aminopropyl groups.
Následující příklad způsob stanovení pouze dokládá, ale neomezuje.The following example illustrates the method of determination but does not limit it.
Příklad provedeníExemplary embodiment
Deklarovaná koncentrace allantoinu ve vzorku byla 1 g/1, koncentrace komplexu jódu s polyvinylpyrolidonem byla 25 g/1.The declared concentration of allantoin in the sample was 1 g / l, the concentration of the iodine-polyvinylpyrrolidone complex was 25 g / l.
0,5 ml vzorku bylo protlačeno přes čtyři sériově zapojené kolony naplněné sorbentem silikagelového typu s kovalentně vázanými oktadecylovými skupinami o zrnění 60 jUm. Potom byly kolony promyty destilovanou vodou, až celkový objem eluátu byl přesně 10 ml (vzorek byl 20krát zředěn).0.5 ml of the sample was passed through four serially connected columns packed with a silica gel type sorbent with covalently bonded octadecyl groups of 60 µm. The columns were then washed with distilled water until the total eluate volume was exactly 10 ml (the sample was diluted 20 times).
Takto získaný zředěný roztok vzorku bez komplexu jódu s polyvinylpyrolidonem byl analyzován vysokoúčinnou kapalinovou chromatografií metodou absolutní kalibrace, za těchto podmínek: kolona: skleněná, délka 150 mm, průměr 3,2 mm, sorbent: silikagel s vázanými aminopropylovými skupinami, mobilní fáze: acetonitril + voda (75:25 obj.) , průtok: 0,5 ml/min, detekce: UV, 220 nm, nástřik: 10 ^ul.The thus obtained diluted iodine-free sample solution with polyvinylpyrrolidone was analyzed by high performance liquid chromatography using the absolute calibration method under the following conditions: column: glass, length 150 mm, diameter 3.2 mm, sorbent: silica gel with bonded aminopropyl groups, mobile phase: acetonitrile + water (75:25 v / v), flow rate: 0.5 ml / min, detection: UV, 220 nm, injection: 10 µl.
Koncentrace kalibračních roztoků 0,01 resp. 0,05 a 0,10 g/1. Takto byla stanovena koncentrace allantoinu ve vzorku 0,99 g/1, což odpovídá deklarované hodnotě.Concentration of the calibration solutions 0,01 resp. 0.05 and 0.10 g / L respectively. Thus, the concentration of allantoin in the sample was determined to be 0.99 g / l, which corresponds to the declared value.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS867537A CS262269B1 (en) | 1986-10-17 | 1986-10-17 | Method for the determination of (2,5-dioxo-4-imidazolidines) -moxyne in the presence of a complex of iodine with polyvinylpyrrolidone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS867537A CS262269B1 (en) | 1986-10-17 | 1986-10-17 | Method for the determination of (2,5-dioxo-4-imidazolidines) -moxyne in the presence of a complex of iodine with polyvinylpyrrolidone |
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| Publication Number | Publication Date |
|---|---|
| CS753786A1 CS753786A1 (en) | 1988-08-16 |
| CS262269B1 true CS262269B1 (en) | 1989-03-14 |
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| Application Number | Title | Priority Date | Filing Date |
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| CS867537A CS262269B1 (en) | 1986-10-17 | 1986-10-17 | Method for the determination of (2,5-dioxo-4-imidazolidines) -moxyne in the presence of a complex of iodine with polyvinylpyrrolidone |
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- 1986-10-17 CS CS867537A patent/CS262269B1/en unknown
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| CS753786A1 (en) | 1988-08-16 |
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