Supercritical fluids in extraction, purification, and separation of selected Amaryllidaceae alkaloids

Kód výsledku v IS VaVaI

<a href="https://www.isvavai.cz/riv?ss=detail&h=RIV%2F00216208%3A11160%2F25%3A10505645" target="_blank" >RIV/00216208:11160/25:10505645 - isvavai.cz</a>

Výsledek na webu

<a href="https://verso.is.cuni.cz/pub/verso.fpl?fname=obd_publikace_handle&handle=tvfKBsP_nz" target="_blank" >https://verso.is.cuni.cz/pub/verso.fpl?fname=obd_publikace_handle&handle=tvfKBsP_nz</a>

DOI - Digital Object Identifier

<a href="http://dx.doi.org/10.1016/j.seppur.2025.133968" target="_blank" >10.1016/j.seppur.2025.133968</a>

Jazyk výsledku

angličtina

Název v původním jazyce

Supercritical fluids in extraction, purification, and separation of selected Amaryllidaceae alkaloids

Popis výsledku v původním jazyce

This study proposes a novel workflow using supercritical fluids in both extraction and analysis steps, focusing on the selective isolation of alkaloids from different parts of the family Amaryllidaceae plant species. This workflow reports supercritical fluid extraction (SFE) and ultra-high performance supercritical fluid chromatography-tandem mass spectrometry (UHPSFC-MS/MS) combined to enable a green, rapid, and selective analysis of Amaryllidaceae alkaloids. The SFE of selected alkaloids from bulbs, the model plant Narcissus cv. Delnashaugh and leaves from the plant Crinum asiaticum L., used CO2, ethanol, and water. It was achieved in only 30 min under the following conditions, i.e., 50 degrees C and 107 bar for bulbs and 67 degrees C and 217 bar for leaves, with repeatability expressed as relative standard deviation &lt; 12.5 %. The optimized SFE method was applied to several Amaryllidaceae plant species from South Africa, with determined alkaloid amounts varying from 20 mu g to 3 mg per 1 g of the dried sample. The plants provided different alkaloid profiles with various dominant alkaloids. The analysis of SFE extracts was carried out on UHPSFC using a 2-picolylamine stationary phase and gradient elution with organic modifier consisting of methanol/acetonitrile (50/50; v/v) containing 20 mmol/l ammonia. The 10 min analysis provided sufficient selectivity and sensitivity of 29 selected alkaloids, which were analyzed within one method without derivatization for the first time. The UHPSFC method with analytes evenly covering the retention window was orthogonal to the 10 min ultra-high performance liquid chromatography (UHPLC) method. MS/MS enabled sensitive analysis with lower limits of quantification (LLOQ) ranging from 0.05 to 10 ng/mL and upper limits of quantification (ULOQ) from 100 to 500 ng/mL for UHPSFC-MS/MS and LLOQ 0.01 - 0.1 ng/mL and ULOQ 50 - 200 ng/mL for UHPLC-MS/MS. Despite a better sensitivity of the UHPLC-MS/MS method for most analytes, the UHPSFC-MS/MS response provided excellent linearity with R^2 &gt; 0.999 in a broad calibration range. The UHPSFC method was scaled up to a preparative purification of SFE extracts. Six fractions with one to three individual alkaloids were obtained in 35 min when using a preparative 100 mm column and in 90 min when using a longer 250 mm column. The study showed the applicability of techniques using supercritical fluids and proved that they can be green alternatives for the isolation of Amaryllidaceae alkaloids from different plant sources with the potential for medicinal applications.

Název v anglickém jazyce

Supercritical fluids in extraction, purification, and separation of selected Amaryllidaceae alkaloids

Popis výsledku anglicky

This study proposes a novel workflow using supercritical fluids in both extraction and analysis steps, focusing on the selective isolation of alkaloids from different parts of the family Amaryllidaceae plant species. This workflow reports supercritical fluid extraction (SFE) and ultra-high performance supercritical fluid chromatography-tandem mass spectrometry (UHPSFC-MS/MS) combined to enable a green, rapid, and selective analysis of Amaryllidaceae alkaloids. The SFE of selected alkaloids from bulbs, the model plant Narcissus cv. Delnashaugh and leaves from the plant Crinum asiaticum L., used CO2, ethanol, and water. It was achieved in only 30 min under the following conditions, i.e., 50 degrees C and 107 bar for bulbs and 67 degrees C and 217 bar for leaves, with repeatability expressed as relative standard deviation &lt; 12.5 %. The optimized SFE method was applied to several Amaryllidaceae plant species from South Africa, with determined alkaloid amounts varying from 20 mu g to 3 mg per 1 g of the dried sample. The plants provided different alkaloid profiles with various dominant alkaloids. The analysis of SFE extracts was carried out on UHPSFC using a 2-picolylamine stationary phase and gradient elution with organic modifier consisting of methanol/acetonitrile (50/50; v/v) containing 20 mmol/l ammonia. The 10 min analysis provided sufficient selectivity and sensitivity of 29 selected alkaloids, which were analyzed within one method without derivatization for the first time. The UHPSFC method with analytes evenly covering the retention window was orthogonal to the 10 min ultra-high performance liquid chromatography (UHPLC) method. MS/MS enabled sensitive analysis with lower limits of quantification (LLOQ) ranging from 0.05 to 10 ng/mL and upper limits of quantification (ULOQ) from 100 to 500 ng/mL for UHPSFC-MS/MS and LLOQ 0.01 - 0.1 ng/mL and ULOQ 50 - 200 ng/mL for UHPLC-MS/MS. Despite a better sensitivity of the UHPLC-MS/MS method for most analytes, the UHPSFC-MS/MS response provided excellent linearity with R^2 &gt; 0.999 in a broad calibration range. The UHPSFC method was scaled up to a preparative purification of SFE extracts. Six fractions with one to three individual alkaloids were obtained in 35 min when using a preparative 100 mm column and in 90 min when using a longer 250 mm column. The study showed the applicability of techniques using supercritical fluids and proved that they can be green alternatives for the isolation of Amaryllidaceae alkaloids from different plant sources with the potential for medicinal applications.

Druh

J_imp - Článek v periodiku v databázi Web of Science

CEP obor

—

OECD FORD obor

30104 - Pharmacology and pharmacy

Projekt

—

Návaznosti

S - Specificky vyzkum na vysokych skolach<br>I - Institucionalni podpora na dlouhodoby koncepcni rozvoj vyzkumne organizace

Rok uplatnění

2025

Kód důvěrnosti údajů

S - Úplné a pravdivé údaje o projektu nepodléhají ochraně podle zvláštních právních předpisů

Název periodika

Separation and Purification Technology

ISSN

1383-5866

e-ISSN

1873-3794

Svazek periodika

377

Číslo periodika v rámci svazku

December

Stát vydavatele periodika

NL - Nizozemsko

Počet stran výsledku

17

Strana od-do

133968

Kód UT WoS článku

001533495800013

EID výsledku v databázi Scopus

2-s2.0-105010566363