Identificación de impurezas en cápsulas de rifampicina por UHPLC-PDA-ESI-MS/MS
No Thumbnail Available
Date
2022
Authors
Journal Title
Journal ISSN
Volume Title
Publisher
Universidad Nacional de Trujillo
Abstract
El objetivo del presente informe fue identificar impurezas en cápsulas de rifampicina por UHPLC-PDA-ESI-MS/MS. Se analizó el polvo de cápsula con respecto a su estándar secundario. La separación cromatográfica se realizó en una columna C18 de 150 x 2,1 mm, utilizando ácido fórmico (AF) 0,1% (A) y AF 0,1% en metanol (B) como fases móviles en elución en gradiente. Las muestras se sometieron a un análisis espectrométrico en modo ESI positivo. Las relaciones masa carga (m/z) encontradas fueron 822, 781, 749 y 130 con tiempos de retención de 5,2 y 5,06 min. Estos resultados confirman la presencia rifampicina quinona, 25-desacetilrifampicina, rifampicina monooxigenada, N- demetilrifampicina, 4-metil-1-nitrosopiperazina y 4-metil-1-nitrosopiperazina, estas última en menor abundancia.
ABSTRACT The aim of this report was to identify impurities in rifampicin capsules by UHPLC-PDA- ESI-MS/MS. The capsule powder was analyzed against its secondary standard. Chromatographic separation was performed on a 150 x 2.1 mm C18 column, using 0.1% formic acid (FA) (A) and 0.1% FA in methanol (B) as mobile phases in gradient elution. Samples were subjected to spectrometric analysis in positive ESI mode. The mass-charge ratios (m/z) found were 822, 781, 749 and 130 with retention times of 5.2 and 5.06 min. These results confirm the presence of rifampicin quinone, 25-desacetylrifampicin, monooxygenated rifampicin, N-demethylrifampicin and 4-methyl-1-nitrosopiperazine and 4-methyl-1-nitrosopiperazine, the latter in less abundance.
ABSTRACT The aim of this report was to identify impurities in rifampicin capsules by UHPLC-PDA- ESI-MS/MS. The capsule powder was analyzed against its secondary standard. Chromatographic separation was performed on a 150 x 2.1 mm C18 column, using 0.1% formic acid (FA) (A) and 0.1% FA in methanol (B) as mobile phases in gradient elution. Samples were subjected to spectrometric analysis in positive ESI mode. The mass-charge ratios (m/z) found were 822, 781, 749 and 130 with retention times of 5.2 and 5.06 min. These results confirm the presence of rifampicin quinone, 25-desacetylrifampicin, monooxygenated rifampicin, N-demethylrifampicin and 4-methyl-1-nitrosopiperazine and 4-methyl-1-nitrosopiperazine, the latter in less abundance.
Description
Keywords
Impurezas, Espectrometría