A powder X-ray diffraction method for detection of polyprenylated benzophenones in plant extracts associated with HPLC for quantitative analysis

A robust, direct, rapid and non-destructive X-ray diffraction crystallography method to detect the polyprenylated benzophenones 7-epi-clusianone (1) and guttiferone A (2) in extracts from Garcinia brasiliensis is presented. Powder samples of benzophenones 1 and 2, dried hexane extracts from G. brasiliensis seeds and fruit`s pericarp, and the dried ethanolic extract from G. brasiliensis seeds were unambiguously characterized by powder X-ray diffractometry. The calculated X-ray diffraction peaks from crystal structures of analytes 1 and 2, previously determined by single-crystal X-ray diffraction technique, were overlaid to those of the experimental powder diffractograms, providing a practical identification of these compounds in the analyzed material and confirming the pure contents of the powder samples. Using the X-ray diffraction crystallography method, the studied polyprenylated benzophenones were selectively and simultaneously detected in the extracts which were mounted directly on sample holder. In addition, reference materials of the analytes were not required for analyses since the crystal structures of the compounds are known. High performance liquid chromatography analyses also were comparatively carried out to quantify the analytes in the same plant extracts showing to be in agreement with X-ray diffraction crystallography method. (C) 2010 Elsevier B.V. All rights reserved.

FAPESP (Fundacao de Amparo a Pesquisa do Estado de Sao Paulo)

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Brazilian Research Council CNPq (Conselho Nacional de Desenvolvimento Cientifico e Tecnologico)

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

FAPEMIG (Fundacao de Amparo Pesquisa do Estado de Minas Gerais)[APQ-2011-5.02/07]

Fundação de Amparo à Pesquisa do Estado de Minas Gerais (FAPEMIG)

Fundação de Amparo à Pesquisa do Estado de Minas Gerais (FAPEMIG)

FAPEMIG (Fundacao de Amparo Pesquisa do Estado de Minas Gerais)[APQ-6010-5.02/07]

FAPEMIG (Fundacao de Amparo Pesquisa do Estado de Minas Gerais)[APQ-02685-09]

Fundação de Amparo à Pesquisa do Estado de Minas Gerais (FAPEMIG)

Fundação de Amparo à Pesquisa do Estado de Minas Gerais (FAPEMIG)

FAPEMIG (Fundacao de Amparo Pesquisa do Estado de Minas Gerais)[CAG-00028/01]

FINEP (Financiadora de Estudos e Projetos)[0134/08]

Financiadora de Estudos e Projetos (FINEP)

FINEP (Financiadora de Estudos e Projetos)[0336/09]

Financiadora de Estudos e Projetos (FINEP)

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

CAPES (Coordenacao de Aperfeicoamento de Pessoal de Nivel Superior)