Aysa Abbasalizadeh, Mohammad Reza Afshar Mogaddam, Mir Ali Farajzadeh, Mahboob Nemati, Saeed Mohammad Sorouraddin
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Among the tested sorbents, UiO-66-NH<sub>2</sub> prepared in dimethylformamide in the presence of acetic acid was found to be the best sorbent in this method for the extraction of apixaban with high extraction efficiency comparable to other types of UiO-66-NH<sub>2</sub> metal organic frameworks. The extraction and preconcentration of apixaban were carried out by adding 5 mg of synthesized sorbent to a 5 mL sample solution, followed by vortexing for 3 min. After discarding the supernatant, the adsorbed analyte was eluted from the sorbent surface using 60 µL acetonitrile under vortexing for 2 min. The effective parameters of the offered method were optimized and validated using a one-parameter-at-a- time strategy. The detection and quantification limits of the method were 9.9 and 32 ng mL<sup>-1</sup> in plasma and 1.5 and 4.9 ng mL<sup>-1</sup> in deionized water, respectively. The method was linear ranging from 4.9 to 1000 ng mL<sup>-1</sup> in deionized water and from 32 to 500 ng mL<sup>-1</sup> in plasma, respectively. The enrichment factor and extraction recovery values were 44 % and 53 %, respectively. The relative standard deviations were ≤6.2 % for intra- and inter-day precisions. Finally, the proposed method was successfully employed to quantify apixaban in human plasma samples.</p>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1251 ","pages":"124417"},"PeriodicalIF":2.8000,"publicationDate":"2025-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Dispersive solid phase extraction of apixaban from human plasma samples prior to capillary electrophoresis determination using zirconium-based metal organic frameworks prepared by different modulator and solvent.\",\"authors\":\"Aysa Abbasalizadeh, Mohammad Reza Afshar Mogaddam, Mir Ali Farajzadeh, Mahboob Nemati, Saeed Mohammad Sorouraddin\",\"doi\":\"10.1016/j.jchromb.2024.124417\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p><p>Here, a zirconium-based metal organic framework-dispersive solid phase extraction method was established as an efficient, robust, and accurate approach for quantifying apixabanin human plasma samples prior to capillary electrophoresis with diode array detection. 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引用次数: 0
摘要
本文建立了一种基于锆基金属有机骨架-分散固相萃取的方法,该方法是一种高效、稳健、准确的方法,可用于毛细管电泳二极管阵列检测前的阿哌沙巴宁人血浆样品的定量。通过改变调制剂和溶剂,合成了以UiO-66-NH2为基础的多种金属有机骨架,并将其作为吸附剂应用于萃取过程中。在所测试的吸附剂中,二甲甲酰胺中醋酸存在下制备的UiO-66-NH2是本方法提取阿哌沙班的最佳吸附剂,其提取效率与其他类型的UiO-66-NH2金属有机骨架相当。在5 mL样品溶液中加入5 mg合成的吸附剂,旋涡萃取3 min,丢弃上清后,用60µL乙腈涡流洗脱吸附物2 min,对阿哌沙班的提取和预富集进行了优化,并采用一次一参数的策略对所提方法的有效参数进行了优化和验证。该方法在血浆中的检测限和定量限分别为9.9和32 ng mL-1,在去离子水中的检测限和定量限分别为1.5和4.9 ng mL-1。该方法在去离子水和血浆中分别在4.9 ~ 1000 ng mL-1和32 ~ 500 ng mL-1范围内呈线性关系。富集系数为44%,提取回收率为53%。日内、日间精密度的相对标准偏差≤6.2%。最后,该方法成功地用于定量人血浆样品中的阿哌沙班。
Dispersive solid phase extraction of apixaban from human plasma samples prior to capillary electrophoresis determination using zirconium-based metal organic frameworks prepared by different modulator and solvent.
Here, a zirconium-based metal organic framework-dispersive solid phase extraction method was established as an efficient, robust, and accurate approach for quantifying apixabanin human plasma samples prior to capillary electrophoresis with diode array detection. Various types of metal organic frameworks based on UiO-66-NH2 were synthesized by altering modulators and solvents and applied as sorbents in the extraction procedure. Among the tested sorbents, UiO-66-NH2 prepared in dimethylformamide in the presence of acetic acid was found to be the best sorbent in this method for the extraction of apixaban with high extraction efficiency comparable to other types of UiO-66-NH2 metal organic frameworks. The extraction and preconcentration of apixaban were carried out by adding 5 mg of synthesized sorbent to a 5 mL sample solution, followed by vortexing for 3 min. After discarding the supernatant, the adsorbed analyte was eluted from the sorbent surface using 60 µL acetonitrile under vortexing for 2 min. The effective parameters of the offered method were optimized and validated using a one-parameter-at-a- time strategy. The detection and quantification limits of the method were 9.9 and 32 ng mL-1 in plasma and 1.5 and 4.9 ng mL-1 in deionized water, respectively. The method was linear ranging from 4.9 to 1000 ng mL-1 in deionized water and from 32 to 500 ng mL-1 in plasma, respectively. The enrichment factor and extraction recovery values were 44 % and 53 %, respectively. The relative standard deviations were ≤6.2 % for intra- and inter-day precisions. Finally, the proposed method was successfully employed to quantify apixaban in human plasma samples.
期刊介绍:
The Journal of Chromatography B publishes papers on developments in separation science relevant to biology and biomedical research including both fundamental advances and applications. Analytical techniques which may be considered include the various facets of chromatography, electrophoresis and related methods, affinity and immunoaffinity-based methodologies, hyphenated and other multi-dimensional techniques, and microanalytical approaches. The journal also considers articles reporting developments in sample preparation, detection techniques including mass spectrometry, and data handling and analysis.
Developments related to preparative separations for the isolation and purification of components of biological systems may be published, including chromatographic and electrophoretic methods, affinity separations, field flow fractionation and other preparative approaches.
Applications to the analysis of biological systems and samples will be considered when the analytical science contains a significant element of novelty, e.g. a new approach to the separation of a compound, novel combination of analytical techniques, or significantly improved analytical performance.