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Advancements in Biosample Preparation: Implementing SPE for the Sustainable Analysis of Ritlecitinib

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Bibliographic Details
Title: Advancements in Biosample Preparation: Implementing SPE for the Sustainable Analysis of Ritlecitinib
Authors: Mornar Turk, Ana, Amidžić Klarić, Daniela, Zubčić, Snježana, Kovačić, Jelena
Publisher Information: 2025.
Publication Year: 2025
Subject Terms: MEPS, SPE, ritlecitinib
Description: Solid-phase extraction (SPE) leverages a solid sorbent material to selectively bind the analyte of interest from a liquid matrix. This binding mechanism facilitates the effective separation of the target compound from matrix interferences. Following this capture step, the retained compound is recovered through elution using a suitable solvent. This elution step serves to isolate and concentrate the analyte. The fundamental principles of SPE have been adapted and significantly advanced in related methodologies, including dispersive solid-phase extraction (dSPE), microextraction by packed sorbent (MEPS), and in-tip solid phase extraction (in-tip SPE), all of which are garnering increasing research interest. Their capacity for efficient analyte pre-concentration, and sample purification has established SPE and related methodologies as preferred sample preparation procedures in contemporary bioanalysis [1, 2]. The aim of our work is to use the above-mentioned sample preparation methodologies to efficiently isolate ritlecitinib, a new Janus kinase 3 and tyrosine kinase inhibitor used to treat severe alopecia areata, from human plasma samples. The analysis was performed using an Agilent 1260 HPLC and a Kinetex EVO C18 Core-Shell column [3]. SPE sample preparation was done using various sorbent materials: octadecyl (C18) and octyl (C8) silane-bonded silica, hydrophilic-lipophilic balanced (HLB) co-polymers, mixed- mode sorbent with nonpolar and cation-exchange functionality (PCX), and hybrid sorbents for protein and phospholipid removal. MEPS procedure included cross-linked polystyrene divinylbenzene copolymer (HDVB) and polystyrene-divinylbenzene copolymer (SDVB) sorbents. In-tip SPE was done using sorbent designed to remove phospholipids from biological samples. The octadecyl (C18) silane-bonded silica powder was employed for dSPE. The results of SPE optimization support the use of protein and phospholipid removal sorbents (HybridSPE DPX Tips: 95.9%; Isolute® PLD+: 97.0%; and Free Phospholipid Removal: 101.1%). Other sorbents showed discouraging extraction efficiencies (PCX: ≤52.3%; C8: ≤54.0%; polymers: ≤69.9%; and C18: ≤88.0%).
Document Type: Conference object
Accession Number: edsair.dris...01492..cb3890d5d65b589afa73a5b8f3e269c2
Database: OpenAIRE
Description
Abstract:Solid-phase extraction (SPE) leverages a solid sorbent material to selectively bind the analyte of interest from a liquid matrix. This binding mechanism facilitates the effective separation of the target compound from matrix interferences. Following this capture step, the retained compound is recovered through elution using a suitable solvent. This elution step serves to isolate and concentrate the analyte. The fundamental principles of SPE have been adapted and significantly advanced in related methodologies, including dispersive solid-phase extraction (dSPE), microextraction by packed sorbent (MEPS), and in-tip solid phase extraction (in-tip SPE), all of which are garnering increasing research interest. Their capacity for efficient analyte pre-concentration, and sample purification has established SPE and related methodologies as preferred sample preparation procedures in contemporary bioanalysis [1, 2]. The aim of our work is to use the above-mentioned sample preparation methodologies to efficiently isolate ritlecitinib, a new Janus kinase 3 and tyrosine kinase inhibitor used to treat severe alopecia areata, from human plasma samples. The analysis was performed using an Agilent 1260 HPLC and a Kinetex EVO C18 Core-Shell column [3]. SPE sample preparation was done using various sorbent materials: octadecyl (C18) and octyl (C8) silane-bonded silica, hydrophilic-lipophilic balanced (HLB) co-polymers, mixed- mode sorbent with nonpolar and cation-exchange functionality (PCX), and hybrid sorbents for protein and phospholipid removal. MEPS procedure included cross-linked polystyrene divinylbenzene copolymer (HDVB) and polystyrene-divinylbenzene copolymer (SDVB) sorbents. In-tip SPE was done using sorbent designed to remove phospholipids from biological samples. The octadecyl (C18) silane-bonded silica powder was employed for dSPE. The results of SPE optimization support the use of protein and phospholipid removal sorbents (HybridSPE DPX Tips: 95.9%; Isolute® PLD+: 97.0%; and Free Phospholipid Removal: 101.1%). Other sorbents showed discouraging extraction efficiencies (PCX: ≤52.3%; C8: ≤54.0%; polymers: ≤69.9%; and C18: ≤88.0%).