RESUMO
An accurate, sensitive and selective reversed-phase micellar liquid chromatographic method was developed for simultaneous determination of benzyl alcohol and benzaldehyde. This method was applied in different injectable formulations containing diclofenac, piroxicam, lincomycin and clindamycin. The method showed excellent linearity in the range of 10-100 microg mL(-1) and 1-20 microg mL(-1) with the limit of detection (S/N = 3) 0.25 microg mL(-1) (2.3 x 10(-6) mol L(-1)) and 0.12 microg mL(-1) (1.13 x 10(-6) mol L(-1)) for benzyl alcohol and benzaldehyde, respectively. The suggested method was successfully applied to the analysis of the studied drugs in bulk with average recoveries of 100.1 +/- 1.0% for benzyl alcohol and 100.4 +/- 1.6% for benzaldehyde, and to the determination of benzyl alcohol and benzaldehyde in injectable formulations with the respective average recoveries of 99.8 +/- 0.3 and 100.0 +/- 0.4%.
Assuntos
Anestésicos Locais/análise , Benzaldeídos/análise , Álcool Benzílico/análise , Cromatografia Capilar Eletrocinética Micelar/métodos , 1-Propanol/análise , 1-Propanol/química , Algoritmos , Anestésicos Locais/administração & dosagem , Anestésicos Locais/química , Benzaldeídos/metabolismo , Benzaldeídos/normas , Álcool Benzílico/administração & dosagem , Álcool Benzílico/química , Calibragem , Cromatografia Capilar Eletrocinética Micelar/instrumentação , Cromatografia Capilar Eletrocinética Micelar/normas , Injeções , Modelos Lineares , Oxirredução , Conservantes Farmacêuticos/análise , Conservantes Farmacêuticos/química , Reprodutibilidade dos Testes , Dodecilsulfato de Sódio/análise , Dodecilsulfato de Sódio/químicaRESUMO
Semicarbazide-sensitive amine oxidase (SSAO; EC 1.4.3.6) is a copper-containing enzyme predominantly expressed by vascular smooth muscle cells. SSAO deaminates primary amines to produce aldehydes and oxygen peroxides, and may thus play a role in vascular damage. SSAO activity can be quantified by assaying benzaldehyde production using fluorescent derivatisation and separation by HPLC. We performed the derivatisation step in polypropylene or borosilicate glass tubes over 45 min at 95 degrees C. High and obstructing background levels of benzaldehyde were found in one batch of polypropylene vials, as opposed to its alternatives. Treatment and handling of product shipment into the country did not account for introduction of contaminant into packaged vials nor did any reagent used in the assay. We conclude that the source of contamination was most likely due to variation in the commercial production process. Use of borosilicate vials for assays based on aldehyde production and derivatisation is recommended.
