An efficient and target-oriented sample enrichment method for preparative separation of minor alkaloids by pH-zone-refining counter-current chromatography

Agro-industrial wastes are abundant and low-cost sources of energy and chemicals. Biomass account for 14% of the world's energy production. Industrial residues of production of soluble coffee (spent coffee grounds -SCG) have great potential due to its large-scale production and can be transformed by pyrolysis, in liquid, solid and gaseous products with applications from energy to chemicals. This work has the objective of producing bio-oil from the pyrolysis of industrial SCG, characterize it by chromatography and indicate its possible applications. As SGC contains a large amount of glycerides, they were extracted from SGC before the pyrolysis, aiming to obtain a better bio-oil from the residue. The yield in vegetable oil was 5.2% and its analyses showed that 50% are saturated acids (mainly palmitic 27.6%) and other 50% are unsaturated ones (mainly linoleic acid 35.3%). This composition qualifies this oil for biodiesel purposes. The residue (SGC after extraction) was submitted to pyrolysis, yielding 30% in liquid products, being 6% bio-oil. The bio-oil was analyzed by gas chromatography being identified free fatty acids, hydrocarbons, phenols and N-compounds. The heteroatomic compounds limit the use as biofuel but can be interesting for the pharmaceutical, agrochemical and fine chemicals industries.

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“…41 On the other hand, nitrogenous compounds have great importance in the pharmaceutical and agrochemical industry. 13,[42][43][44][45][46][47]…”

Section: Characterization Of the Solid Residue From The Soxhlet Extramentioning

confidence: 99%

Production and Characterization of the Bio-Oil Obtained by the Fast Pyrolysis of Spent Coffee Grounds of the Soluble Coffee Industry

Krause

Moitinho

Ferreira

et al. 2019

J. Braz. Chem. Soc.

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“…Five indole alkaloids, including VCA, DHC, HTE, HTI, and GSM, were prepared in our laboratory as reported previously [20]. IC and C were purchased from Yuanye Bio-Technology Co., Ltd. R and IR were from Nature Standard Co., Ltd.…”

Section: Chemicals Reagents and Materialsmentioning

confidence: 99%

Characteristic Chromatogram: A Method of Discriminate and Quantitative Analysis for Quality Evaluation of Uncaria Stem with Hooks

et al. 2017

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It remains a challenge to establish new monographs for herbal drugs derived from multiple botanical sources. Specifically, the difficulty involves discriminating and quantifying these herbs with components whose levels vary markedly among different samples. Using stem with hooks as an example, a characteristic chromatogram was proposed to discriminate its five botanical origins and to quantify its characteristic components in the chromatogram. The characteristic chromatogram with respect to the components of stem with hooks with the five botanical origins was established using 0.02% diethylamine and acetonitrile as the mobile phase. The total analysis time was 50 min and the detection wavelength was 245 nm. Using the same chromatogram parameters, the single standard to determine multicomponents method was validated to simultaneously quantify nine indole alkaloids, including vincosamide, 3-dihydrocadambine, isocorynoxeine, corynoxeine, isorhynchophylline, rhynchophylline, hirsuteine, hirsutine, and geissoschizine methyl ether. The results showed that only the stem with hooks from, the most widely used in the herbal market, showed the presence of these nine alkaloids. The conversion factors were 1.27, 2.32, 0.98, 1.04, 1.00, 1.02, 1.26, 1.33, and 1.25, respectively. The limits of quantitation were lower than 700 ng/mL. The total contents of 31 batches of stem with hooks were in the range of 0.1 - 0.6%, except for Havil and (Oliv.) Havil. The results also showed that the total content of indole alkaloids tended to decrease with an increase in the hook diameter. This showed that the characteristic chromatogram is practical for controlling the quality of traditional Chinese medicines with multiple botanical origins.

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“…The solvent system selection is the most important step for a successful PZRCCC procedure. Ideal partition coefficient in both basic (K base ≫ 1) and acidic (K acid ≪ 1) and good solubility of the sample in the solvent system are essential for a suitable solvent system [33][34][35][36][37]. Based on the optimization of LLE solvent systems, n-hexane/ethyl acetate/methanol/water at volume ratios of 7:3:7:3 and 8:4:8:4 were tested, it was found the systems could not give small enough K acid , indicating the targets could not distribute well in aqueous phase when the pH was adjusted lower than 2.…”

Section: Selection Of Two-phase Solvent Systemmentioning

confidence: 99%

An efficient strategy based on liquid‐liquid extraction and pH‐zone‐refining counter‐current chromatography for selective enrichment, separation, and purification of alkaloids and organic Acids from natural products

et al. 2020

J of Separation Science

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This study presents an efficient strategy based on liquid‐liquid extraction and pH‐zone‐refining counter‐current chromatography for selective enrichment, separation, and purification of alkaloids and organic acids from natural products. First, an acid or base modified two‐phase solvent system with maximum or minimum partition coefficient was developed for the liquid‐liquid extraction of the crude extract. As a result, alkaloids or organic acids could be selectively enriched in the upper or lower phase. Then pH‐zone‐refining counter‐current chromatography was employed to separate and purify the selectively enriched alkaloids or organic acids efficiently. The selective enrichment and separation of five bufadienolide from toad venom of Bufo marinus was used as an example to show the advantage of this strategy. As a result, 759 mg of selectively enriched bufadienolide was obtained from 2 g of crude extract and the total content of five targets was increased from 14.64 to 83%. A total of 31 mg of marinobufagin‐3‐adipoyl‐l‐arginine, 42 mg of telocinobufagin‐3‐pimeloyl‐l‐arginine, 51 mg of telocinobufagin‐3‐suberoyl‐l‐arginine, 132 mg of marinobufagin‐3‐suberoyl‐l‐arginine, and 57 mg of bufalin‐3‐suberoyl‐l‐arginine were all simultaneously separated from 500 mg of selectively enriched sample, with the purity of 92.4, 97.5, 90.3, 92.1, and 92.8%, respectively.

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An efficient and target-oriented sample enrichment method for preparative separation of minor alkaloids by pH-zone-refining counter-current chromatography

Cited by 18 publications

References 21 publications

Production and Characterization of the Bio-Oil Obtained by the Fast Pyrolysis of Spent Coffee Grounds of the Soluble Coffee Industry

Production and Characterization of the Bio-Oil Obtained by the Fast Pyrolysis of Spent Coffee Grounds of the Soluble Coffee Industry

Characteristic Chromatogram: A Method of Discriminate and Quantitative Analysis for Quality Evaluation of Uncaria Stem with Hooks

An efficient strategy based on liquid‐liquid extraction and pH‐zone‐refining counter‐current chromatography for selective enrichment, separation, and purification of alkaloids and organic Acids from natural products

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