IF 1.5 4区 化学 Q4 BIOCHEMICAL RESEARCH METHODS
Durga Panikumar Anumolu, Jampana Ramatulasi, Gorja Ashok, Syed Sara Afreen, Ceema Mathew, Pulusu Veera Shakar
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引用次数: 0

摘要

采用分子印迹鬼聚合物-固相萃取法(MISPE)和液相色谱法建立了分析血清/血浆/尿液中恩格列净的有效方法。在自由基聚合过程中,使用甲基丙烯酸(MAA)作为单体,2,2-偶氮二异丁腈作为引发剂,乙二醇二甲基丙烯酸酯作为交联剂。Empagliflozin 被负载到聚合物上,并用 1 mL 9:1 MeOH:acetic acid 溶液洗脱。PRONTOSIL C8(250 × 4 mm × 5u)用于设计优化的高效液相色谱技术。磷酸盐缓冲液(pH -5):流动相为 ACN(40:60),流速为 0.8 mL/min,检测波长为 230 nm。Empagliflozin 的校准曲线在 0.08 至 200 μg/mL 之间呈线性关系。定量阈值(定量限)和检测阈值(检测限)分别为 0.002 和 0.006 μg/mL。该聚合物显示出很高的结合亲和力和选择性,在 pH 值为 8 时,聚合物的再结合效率很高。研究发现,采用所开发的分子印迹固相萃取-高效液相色谱技术,分析物的萃取回收率为 93%,相对标准偏差为 (RSD)。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Synthesis and Characterization of MIP Ghost Approach for Selective Extraction of Empagliflozin and Quantification by Liquid Chromatography.

The valid method was developed for analyzing empagliflozin in serum/plasma/urine using a molecularly imprinted ghost polymer-solid-phase extraction approach (MISPE) with liquid chromatographic methodology. Methacrylic acid (MAA) was used as the monomer, 2,2 azobis isobutyronitrile as the initiator and ethylene glycol dimethacrylate as the cross-linker in the free radical polymerization procedure. Empagliflozin was loaded onto the polymer and eluted with 1 mL of a 9:1 MeOH:acetic acid solution. The PRONTOSIL C8 (250 × 4 mm × 5u) was used to design the optimized HPLC technique. Phosphate buffer (pH -5): ACN (40:60) was used as the mobile phase with a flow rate of 0.8 mL/min, and 230 nm was used for detection. Empagliflozin's calibration curve is linear between 0.08 and 200 μg/mL. The thresholds for quantification (limit of quantification) and detection (limit of detection) were 0.002 and 0.006 μg/mL, respectively. High binding affinity and selectivity were displayed by the polymer, and, at pH 8, the polymer's rebinding efficiency was effective. It was discovered that the extraction recovery of the analyte employing the molecular-imprinted solid-phase extraction coupled with high-performance liquid chromatography developed technique was 93% with relative standard deviation (RSD) <2%.

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来源期刊
CiteScore
2.90
自引率
7.70%
发文量
94
审稿时长
5.6 months
期刊介绍: The Journal of Chromatographic Science is devoted to the dissemination of information concerning all methods of chromatographic analysis. The standard manuscript is a description of recent original research that covers any or all phases of a specific separation problem, principle, or method. Manuscripts which have a high degree of novelty and fundamental significance to the field of separation science are particularly encouraged. It is expected the authors will clearly state in the Introduction how their method compares in some markedly new and improved way to previous published related methods. Analytical performance characteristics of new methods including sensitivity, tested limits of detection or quantification, accuracy, precision, and specificity should be provided. Manuscripts which describe a straightforward extension of a known analytical method or an application to a previously analyzed and/or uncomplicated sample matrix will not normally be reviewed favorably. Manuscripts in which mass spectrometry is the dominant analytical method and chromatography is of marked secondary importance may be declined.
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