{"title":"Synthesis and Characterization of MIP Ghost Approach for Selective Extraction of Empagliflozin and Quantification by Liquid Chromatography.","authors":"Durga Panikumar Anumolu, Jampana Ramatulasi, Gorja Ashok, Syed Sara Afreen, Ceema Mathew, Pulusu Veera Shakar","doi":"10.1093/chromsci/bmaf008","DOIUrl":null,"url":null,"abstract":"<p><p>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%.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 2","pages":""},"PeriodicalIF":1.5000,"publicationDate":"2025-01-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of chromatographic science","FirstCategoryId":"92","ListUrlMain":"https://doi.org/10.1093/chromsci/bmaf008","RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"BIOCHEMICAL RESEARCH METHODS","Score":null,"Total":0}
引用次数: 0
Abstract
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%.
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.