Abstract
Considerando a necessidade de um método rápido, barato e poderoso para a rotina de controle de qualidade, a Densitometria / Cromatografia de Camada Delgada foi um método escolhido para atender a essas solicitações. No entanto, essa técnica tem suas limitações quando usada para ensaios de determinação de substâncias em matrizes complexas, como extratos vegetais. Considerando a restrição da técnica cromatográfica durante o desenvolvimento de metodologias analíticas para medicamentos, foi desenvolvido um novo procedimento para superar a dificuldade em obter os parâmetros de validação dentro dos critérios internacionais de aceitação, principalmente os parâmetros de seletividade e repetibilidade. O método desenvolvido foi aplicado na quantificação de ácido betulínico (BA) a partir de extratos de produtos naturais. Todas as separações foram obtidas nas cromatoplacas Si60 F254 com n-hexano: acetato de etila: ácido acético (7: 3: 0,3) a 560 nm, após derivatização com reagente vanilina-sulfúrica. O sistema forneceu pontos compactos para BA (Rf. 0,5) e exibiu linearidade (R2 = 0,999). A metodologia foi comparada com uma metodologia de cromatografia gasosa validada e nenhuma diferença estatística foi observada.
Highlights
Many analytical techniques have been developed for drugs analyses in complex matrices
To determine the best solvent or mixture of solvents to develop the thin-layer chromatography (TLC) plate, a literature research was performed and the solvent system selection was based on the Betulinic acid (BA) solubility combined with its toxicity, cost, and flammability
Trial runs were performed by changing polarity in each solvent system, but none of the systems mentioned in literature presented the center of spot nearest to the BA separated from it by at least one-half sum of spot diameters, with visual appearance of analyte indistinguishable from the reference material
Summary
Many analytical techniques have been developed for drugs analyses in complex matrices. Gas chromatography (GC) is described as the best option for assay and purity testing of natural matrices [1,2,3], while the thin-layer chromatography (TLC) is commonly used for its qualitative analysis [4,5,6]. Most of the manuscripts described in the literature since 1993 fail to demonstrate the fitness for purpose to the TLC methods reported [7,8]. While some studies apply inappropriate validation procedures for TLC methods, others compare their results to traditional techniques without the appropriate statistical treatment to meet international acceptance standards [9,10,11,12]. A wide range of biological activities is reported for BA, including antiviral [20], antibacterial [21] and antiinflammatory properties [22,23], and breast cancer [24,25,26,27]
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