Supercritical fluid extraction and chromatographic analysis (HRGC-FID and HRGC-MS) of Lupinus spp. alkaloids

Abstract

Os extratos de alcalóides de Lupinus spp., obtidos por métodos convencionais (maceração/ sonicação -extração em fase sólida; maceração/sonicação -extração líquido-líquido) e por SFE (extração com fluido supercrítico) usando CO 2 e CO 2 modificado (CO 2 /MeOH, CO 2 /EtOH, CO 2 / i PrOH e CO 2 /H 2 O) foram analisados por CGAR-DIC (cromatografia gasosa de alta resolução com detector de ionização de chama) e CGAR-EM (cromatografia gasosa de alta resolução acoplada à espectrometria de massas). As análises quantitativas por CGAR-DIC foram feitas pelo método do padrão interno, para a quantificação de lupanina, multiflorina e um alcalóide derivado da esparteína. CGAR-EM permitiu a identificação dos constituintes químicos (alcalóides e outras substâncias) destes extratos.The alkaloid extracts from Lupinus spp., obtained by conventional methods (maceration/sonication -solid phase extraction; maceration/sonication -liquid-liquid extraction) and SFE (supercritical fluid extraction) using CO 2 and modified CO 2 (CO 2 /MeOH, CO 2 /EtOH, CO 2 / i PrOH and CO 2 / H 2 O) were analysed by HRGC-FID (high resolution gas chromatography -flame ionization detector) and HRGC-MS (high resolution gas chromatography -mass spectrometry). The HRGC-FID quantitative analyses were performed with an internal standard method for quantification of lupanine, multiflorine and a spartein-like alkaloid. HRGC-MS allowed identification of the chemical constituents (alkaloids and other compounds) from these extracts.

Supercritical Fluid Extraction of Bioactive Compounds: Fundamentals, Applications and Economic Perspectives

“…Water is frequently used as a co-solvent (Bicchi et al 1991;Brachet et al 2000;Park et al 2007). Nonetheless, difficulties related to foam formation and other problems have been reported by some authors (Nossack et al 2000;Pereira et al 2003;Schaeffer et al 1989). The reasons for these problems were explained by the phase equilibria of the CO 2 /H 2 O and CO 2 /H 2 O/alcohol systems .…”

Characterization and effect of year of harvest on the nutritional properties of three varieties of white lupine (Lupinus albusL.)

“…Helium was used as carrier gas at an average linear velocity of 35 cm · s −1 and a flow rate of 1 mL · min −1 . Alkaloid quantification was performed in full‐scan mode by the internal standard method using caffeine as analytical standard . In the standard solutions the limit of quantification (signal/noise ratio >7) was 0.2 mg kg −1 for sparteine and 0.4 mg kg −1 for all other alkaloids …”

Lupin Seed for the Crop-Livestock Food Chain

“…The extraction was repeated twice and the supernatants decanted while the precipitate was discarded (Oboh et al, 1998). The alkaloids in the sample extract were extracted with dicholorometane and analysed by HRGC-MS (Nossack et al, 2000) performed using a 5973 inert mass selective detector (Agilent technologies USA), coupled to a 6890N GC (Agilent technologies USA). The capillary column used was a 95% methyl, 5% phenylpolysiloxane, HP-5 (Agilent J&W GC Columns) of 30 m length, 0.25 mm i.d., 0,25 µm film thickness.…”

“…Lupinus extracts were diluted to 1.0 mL in methanol and 0.3 mL of a caffeine standard solution (1 mg mL -1 ) was added to the sample, which was analysed by GC-MS (Nossack et al, 2000). In the standard solutions the Limit Of Quantification (L.O.Q.…”