Naslov
Ion chromatography of azide in pharmaceutical protein samples with high chloride concentration using suppressed conductivity detection

Autori
Vinković, Kristinka ; Drevenkar, Vlasta

Izvornik
Journal of chromatography. B (1570-0232) 864 (2008), 1-2; 102-108

Vrsta, podvrsta i kategorija rada
Radovi u časopisima, članak, znanstveni

Ključne riječi
Ion chromatography of azide ; Suppressed conductivity detection ; Pharmaceutical protein samples ; Nitrobenzoyl azide derivatives

Sažetak
Methods based on reversed-phase liquid chromatography with UV detection of 4-nitrobenzoyl- or 3, 5-dinitrobenzoyl azide derivatives lack in accuracy and stability of derivatives to be applied for azide determination in pharmaceutical protein samples with high sodium chloride concentrations. This paper describes a sensitive and selective ion chromatographic method, with simple sample preparation and suppressed conductivity detection, developed for trace determination of azide in protein samples containing sodium chloride in concentrations as high as 11.6gL−1. Anion exchange stationary phase with quaternary alkyl amine functional groups and gradient elution with sodium hydroxide enabled goodresolutionofanionswithsimilarretentiontimes:azide, bromideandnitrate, aswellaschloridewhoseretentiontimewasshorterthanazide’s. Anions with high affinity to stationary phase (phosphate and citrate) were also eluted within acceptable analysis time of 32min. The stability of sample solutions and the method selectivity, accuracy, precision and sensitivity satisfied the validation criteria of international organizations competent for pharmaceutical industry. The detection and quantitation limit ranges of sodium azide in protein samples were 0.007–0.02mgL−1 and 0.02–0.06mgL−1, respectively. Both limits increased with the concentration of sodium chloride.

Izvorni jezik
Engleski

Znanstvena područja
Kemija

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