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

Result code in 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>

Result on the web

<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>

Result language

angličtina

Original language name

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

Original language description

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.

Czech name

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Czech description

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Type

J_imp - Article in a specialist periodical, which is included in the Web of Science database

CEP classification

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OECD FORD branch

30104 - Pharmacology and pharmacy

Project

—

Continuities

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

Publication year

2025

Confidentiality

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

Name of the periodical

Separation and Purification Technology

ISSN

1383-5866

e-ISSN

1873-3794

Volume of the periodical

377

Issue of the periodical within the volume

December

Country of publishing house

NL - THE KINGDOM OF THE NETHERLANDS

Number of pages

17

Pages from-to

133968

UT code for WoS article

001533495800013

EID of the result in the Scopus database

2-s2.0-105010566363