A validated higher-performance liquid chromatography method for quantification of cinchonain Ib in bark and phytopharmaceuticals of Trichilia catigua used as Catuaba.
The hydroalcoholic extract, prepared from authentic chopped barks of Trichilia catigua, was evaluated by high-performance liquid chromatography using a diode array detector (200-400 mn). The crude extract was purified by rotation locular counter-current chromatography and the chloroform fraction obtained was clean-up by solid-phase extraction. With the aim of getting preliminary structure information on-line, the methanol fraction thus obtained was analyzed by gradient elution using the diode array detector coupled to a mass spectrometer. The presence of flavalignan in this extract was inferred by the chromatographic band, in the total ion current trace, that had an [M-H](-) = 451. With this information, cinchonain Ib was isolated as a pure compound from the crude hydroalcoholic extract using a solid-phase extraction procedure for the sample clean-up followed by a semi-preparative separation using the reverse mode of elution. The isolated compound, after complete characterization, was used as an external standard for the development and validation of a method for the analysis of this compound in herbal medicines using the ultraviolet as the detector. The validated method has been successfully applied for quantification of cinchonain Ib in commercialized herbal medicines sold as Catuaba in Brazil and also in standard chopped barks of T. catigua.
Beltrame
Flávio Luís
FL
Departamento de Química, Universidade Federal de Sao Carlos, SP, Brazil.
Filho
Edson Rodrigues
ER
Barros
Fabio A Proença
FA
Cortez
Diógenes Aparíciogarcia
DA
Cass
Quezia Bezerra
QB
D002396:Catechols / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003377:Countercurrent Distribution; D029582:Meliaceae / Q000737:chemistry*; D024301:Plant Bark / Q000737:chemistry*; D010936:Plant Extracts / Q000032:analysis / Q000302:isolation & purification; D011753:Pyrones / Q000032:analysis*
D002396:Catechols; C437663:Catuama; D010936:Plant Extracts; D011753:Pyrones; C513224:cinchonain Ib