Abstract
Our study aimed at the development of a method based on ultra-performance liquid chromatography coupled to mass spectrometry (UPLC-ESI-MS) using selected ion monitoring for the simultaneous quantitation of the alkaloids galantamine, pseudolycorine, sanguinine and narciclasine in Amaryllidaceae species (Hippeastrum elegans, Habranthus cf. irwinianus, Hymenocallis littoralis and Griffinia nocturna). The alkaloids were extracted from dried and ground bulbs (100 mg) using liquid-liquid microextraction followed by solid phase extraction in cation exchange cartridges. The quantification method showed good linearity (correlation coefficient, R ≥ 0.9968) and selectivity for a run time of 10 min. All values were within the acceptable limits for recovery (87.5-96.2%), interday (coefficient of variation, CV%, 1.3-8.4%) and intraday precision (CV% 5.7-8.1%), except narciclasine (70%). The limits of detection and quantification were 5-100 and 20-350 ng mL-1, respectively. Our method demonstrated to be rapid, sensitive and reliable, therefore appropriate for being employed in the prospection of new source of galantamine and other alkaloids.
Highlights
Galantamine is one of the main drugs used for the clinical treatment of Alzheimer’s disease, acting as a selective, reversible and competitive inhibitor of acetylcholinesterase.[1]
Chemicals and solvents The analytical standards galantamine and codeine-d3 (98% purity) were purchased from Sigma-Aldrich (Saint Louis, USA), while standards of pseudolycorine, sanguinine and narciclasine were isolated from H. elegans earlier (90-95% purity) (Figure 1 and S1, Supplementary Information (SI) section).[22]
Three extraction methods were assessed in quintuplicate using 100 mg of dried bulb powder from H. elegans: (I) acid-base liquid-liquid partition (II) solid-liquid extraction and (III) solid-liquid extraction followed by solid-phase extraction
Summary
Galantamine is one of the main drugs used for the clinical treatment of Alzheimer’s disease, acting as a selective, reversible and competitive inhibitor of acetylcholinesterase.[1]. MS analysis provides more structural information on the chemical profile than the conventional chromatographic detectors, allowing for a more reliable identification.[15] For quantitative MS analysis, the method of choice relies on tandem systems, mainly composed of triple quadrupole detectors, since higher sensitivity is achieved by monitoring specific ions transitions (the so‐called multiple reaction monitoringMRM). This approach has been successfully employed for analyzing drugs such as galantamine in biological matrices.[16] Alternatively, it is possible to filter the m/z from a targetion employing a single MS detector. Pseudolycorine is an opened dioxole ring derivative from lycorine, which has exhibited antitumoral activities in pre-clinical and in vitro experiments.[20]
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