Zheng Wang, Yi Ren, Mingchang Jia, Siqi Hao, Lihong Wu, Xiangfu Meng and Xiaofei Zhang
{"title":"Study on the removal of Cr(vi) from ethylene wastewater using stabilized nanoscale zero-valent iron based on porous basalt material","authors":"Zheng Wang, Yi Ren, Mingchang Jia, Siqi Hao, Lihong Wu, Xiangfu Meng and Xiaofei Zhang","doi":"10.1039/D4AY02298J","DOIUrl":"https://doi.org/10.1039/D4AY02298J","url":null,"abstract":"<p >In this research, the authors prepared stabilized nanoscale zero-valent iron based on natural basalt material and used it to remove Cr(<small>VI</small>) from ethylene wastewater. SEM, TEM, FTIR, XRD, BET and other means were used to characterize the material (BM-nZVI-CMC) before and after loading. The results showed that under the action of CMC, the Fe<small><sup>0</sup></small> particles after loading were all nano-sized (particle size between 43 and 119 nm), and FTIR and XRD results show that compared with BM-nZVI, Fe<small><sup>0</sup></small> in the stabilized material (BM-nZVI-CMC) is more likely to remain in the form of zero valence without being oxidized, that is, the stability is significantly enhanced. BM-nZVI-CMC had a large specific surface area (433.29 m<small><sup>2</sup></small> g<small><sup>−1</sup></small>) and suitable pore size (51.05 nm). In the experiments of Cr(<small>VI</small>) removal by adsorption, the acidity experiment results show that, except under strong acidic conditions, BM-nZVI-CMC has good adsorption effect on Cr(<small>VI</small>); the isotherm experiment results show that BM-nZVI-CMC's adsorption of Cr(<small>VI</small>) more fits the Langmuir model (Langmuir <em>R</em><small><sup>2</sup></small> = 0.991), indicating a tendency towards chemical adsorption; the kinetic experiment results show that BM-nZVI-CMC's porous structure and large specific surface area are conducive to improving the adsorption rate, and the adsorption of Cr(<small>VI</small>) by BM-nZVI-CMC is the result of both physical and chemical processes (pseudo first order <em>R</em><small><sup>2</sup></small> = 0.997; pseudo second-order <em>R</em><small><sup>2</sup></small> = 0.995); BM-nZVI-CMC has a high removal rate for Cr(<small>VI</small>) in different types of ethylene wastewater (quench water and ground oil-bearing water, more than 87%; DS discharge water, more than 73%), and after 120 hours of storage, the adsorption effect of BM-nZVI-CMC for Cr(<small>VI</small>) remains at a high level.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 13","pages":" 2749-2762"},"PeriodicalIF":2.7,"publicationDate":"2025-03-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143716595","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Wenlanqi Du, Jia Jia, Yinghong Zhao, Ailing Ning, Nan Chen, Rongfu Huang and Jin Luo
{"title":"Novel derivatized cyclodextrin as a stationary phase in gas chromatography for separating chiral and achiral compounds","authors":"Wenlanqi Du, Jia Jia, Yinghong Zhao, Ailing Ning, Nan Chen, Rongfu Huang and Jin Luo","doi":"10.1039/D5AY00256G","DOIUrl":"10.1039/D5AY00256G","url":null,"abstract":"<p >The development of efficient techniques for chiral separation has become increasingly vital, especially with the increasing demand for optically pure substances in the pharmaceutical industry and other fields. In this study, we present a novel gas chromatography (GC) stationary phase that utilizes porous polymers containing β-cyclodextrin (β-CD). The material, referred to as P-CDP, was synthesized through a bottom-up approach, incorporating β-cyclodextrin and tetrafluoroterephthalonitrile (TFTPN). The resulting P-CDP material boasts several impressive properties. It has high thermal stability, a substantial specific surface area, and a mesoporous structure, all of which contribute to its effectiveness in enantioselective separations. Various characterization techniques, such as FT-IR, TGA, PXRD, and BET analysis, confirmed the successful synthesis and desirable features of P-CDP. Several kinds of analytes were tested by P-CDP-based capillary columns, including Grob reagents, <em>n</em>-alkanes, <em>n</em>-alcohols, fatty acid methyl esters, aldehydes, and several racemic compounds. The results were promising: the columns demonstrated excellent separation efficiency and consistent reproducibility, with strong enantioselective performance. These characteristics underscore the potential of P-CDP as a versatile stationary phase for chiral GC analysis. This work provides a new approach for integrating β-CD derivatives into GC applications, offering promising prospects for further development of chiral stationary phases with enhanced selectivity and stability.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 16","pages":" 3164-3170"},"PeriodicalIF":2.7,"publicationDate":"2025-03-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143794178","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Hongming Tang, Hongjian Kang, Weijia Zhou, Tao Hou, Zhixin Guo, Yanfang Liu, Xingya Xue and Jixia Wang
{"title":"Bioactivity-guided isolation of anti-proliferative compounds from Curcuma zedoaria against triple negative breast cancer cells†","authors":"Hongming Tang, Hongjian Kang, Weijia Zhou, Tao Hou, Zhixin Guo, Yanfang Liu, Xingya Xue and Jixia Wang","doi":"10.1039/D5AY00050E","DOIUrl":"10.1039/D5AY00050E","url":null,"abstract":"<p >Triple-negative breast cancer (TNBC) presents limited clinically effective treatment options. <em>Curcuma zedoaria</em> (<em>C. zedoaria</em>), a traditional medicine, has been used in China to treat various cancers including TNBC, although its active components remain unclear. Herein, we applied multidimensional liquid chromatography combined with bioactivity assay to discover anti-proliferative compounds against TNBC cells from <em>C. zedoaria</em>. Initially, 26 fractions were generated through first-dimensional reverse-phase liquid chromatography and profiled using SUM159 cells for its anti-proliferative activity. Two active fractions were identified and separated. Following the third-dimensional separation, we successfully isolated two compounds, diarylheptanoid <strong>a</strong> and diarylheptanoid <strong>b</strong>, and found that both compounds displayed moderate potency in inhibiting SUM159 proliferation with IC<small><sub>50</sub></small> values of 19.82 ± 3.08 μM and 28.16 ± 1.97 μM, respectively. Transcriptome analysis revealed that the differentially expressed genes induced by diarylheptanoid <strong>a</strong> were mainly concentrated with the actin function and involved in motor protein pathways. This study suggests that diarylheptanoids may contribute to the anti-TNBC effects of <em>C. zedoaria</em> and provide potential scaffolds for anti-TNBC drug development.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 13","pages":" 2740-2748"},"PeriodicalIF":2.7,"publicationDate":"2025-03-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143646572","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Hao Du, Yefeng Deng, Lianpeng Lv, Junting Li, Chao Zhang, Yichang Li, Yang Zhou, Zhiqin Peng, Hailiang Yang and Bing Wang
{"title":"On-site rapid detection of ancient leather using a dual recognition strategy","authors":"Hao Du, Yefeng Deng, Lianpeng Lv, Junting Li, Chao Zhang, Yichang Li, Yang Zhou, Zhiqin Peng, Hailiang Yang and Bing Wang","doi":"10.1039/D5AY00004A","DOIUrl":"10.1039/D5AY00004A","url":null,"abstract":"<p >Leather has been widely used since ancient times, and the discovery of ancient leather is of great value for studying the origin and development of costume culture. However, due to contamination and degradation of leather relics in the buried environment, traditional analytical methods face challenges in detecting microtraces of ancient leather. Therefore, an immunosensor based on a dual recognition strategy was proposed in this work for the detection of leather artifacts at archaeological sites. Anti-collagen antibodies type I (Anti-COL I) and type II (Anti-COL II) were prepared through animal immunization. Next, the antibodies on the surfaces of magnetic beads (MBs) and polystyrene microspheres (PMs) underwent a specific binding reaction with the antigens, which were magnetically separated and placed in sucrose solution, further catalyzed by sucrose invertase on functionalized polystyrene microspheres (FPMs). Finally, the collagen concentration was detected using a personal glucose meter (PGM). The prepared immunosensor exhibited excellent sensitivity, specificity, and stability, with a limit of detection (LOD) of 4.92 ng mL<small><sup>−1</sup></small>, a relative standard deviation (RSD) of 8.39% for sensitivity, and a linear detection range of 10 ng mL<small><sup>−1</sup></small> to 100 μg mL<small><sup>−1</sup></small>. The coefficient of variation of specificity was less than 4.34%, and the sensor demonstrated a lifespan of up to three weeks. Moreover, the sensor outperforms enzyme-linked immunosorbent assay (ELISA) in terms of accuracy, specificity, and reproducibility. Therefore, this sensor provides a new strategy for the on-site detection of leather artifacts.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 15","pages":" 2978-2986"},"PeriodicalIF":2.7,"publicationDate":"2025-03-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143750131","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Shili Qin, Jinxin Lei, Dan Wang, Ming Zhao, Hongtao Chu, Lidi Gao and Fenglong Jin
{"title":"Open tubular column coated with a novel zinc-based MOF/imine COF hybrid, for small molecular separation using capillary electrochromatography†","authors":"Shili Qin, Jinxin Lei, Dan Wang, Ming Zhao, Hongtao Chu, Lidi Gao and Fenglong Jin","doi":"10.1039/D5AY00201J","DOIUrl":"10.1039/D5AY00201J","url":null,"abstract":"<p >Metal organic frameworks (MOFs) and covalent organic frameworks (COFs) represent two burgeoning categories of advanced porous materials that have garnered substantial interest within the scientific community in recent years. Notably, the synergistic effect of MOFs and COFs facilitates their integration into MOF/COF hybrid structures, thereby enhancing performance and broadening their applicability across diverse fields. Herein, we report the development of a novel capillary electrochromatographic coated open tubular column, utilizing a MOF/COF hybrid material (ZIF-93/TpBD) as the stationary phase, to achieve high-resolution separation of six groups of analogues. Both ZIF-93/TpBD-coated open tubular (OT) column and the hybrid stationary phase were characterized using a series of analytical techniques. The outstanding separation performance of the as-prepared OT column was evaluated using alkaline amino acids, sulfonamides, acidic antibiotics, vitamin B, purine compounds and β-blocker analyte groups, under optimal separation conditions. The six groups of analytes achieved baseline separation within 9.5 minutes and achieved high resolution (ranging from 1.50 to 9.71). Furthermore, the run to run, day to day, column to column and batch to batch relative standard deviations of retention time and column efficiency were in the range 0.71–3.91% and 0.49–4.19%, respectively. The ZIF-93/TpBD-coated OT column exhibited remarkable stability after 200 consecutive runs. Finally, a rapid, highly efficient, accurate, and reliable method was developed for the qualitative and quantitative analysis of vitamins B1, B2, B6 and nicotinamide in healthcare settings. This novel hybrid stationary phase, composed of MOF/COF, presents a new avenue for the advancement of chromatographic separation.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 15","pages":" 2961-2970"},"PeriodicalIF":2.7,"publicationDate":"2025-03-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143750184","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yanan Zhang, Yimin Wang, Ningjing Huang, Wei Zheng, Hang Guo and Chunyin Li
{"title":"Facile synthesis of water-soluble and pH-stable silicon quantum dots and their application in enzyme-free hydrogen peroxide sensing†","authors":"Yanan Zhang, Yimin Wang, Ningjing Huang, Wei Zheng, Hang Guo and Chunyin Li","doi":"10.1039/D5AY00038F","DOIUrl":"10.1039/D5AY00038F","url":null,"abstract":"<p >A sensor for non-enzymatic hydrogen peroxide (H<small><sub>2</sub></small>O<small><sub>2</sub></small>) detection was developed based on silicon quantum dots (SiQDs). The fluorescent SiQDs were synthesized using a one-pot hydrothermal method. The SiQDs were made water-soluble and pH-stable by covering their surfaces with amino and hydroxyl groups. Additionally, the prepared SiQDs had a large Stokes shift (131 nm), excellent photostability (442 min), and hypotoxicity (<em>e.g.</em>, 99% cell viability was retained after a 24 h-treatment at 8.0 mg mL<small><sup>−1</sup></small> of SiQDs). The dynamic quenching effect induced by H<small><sub>2</sub></small>O<small><sub>2</sub></small> effectively suppresses the blue fluorescence of SiQDs. Under the optimum conditions, the SiQD-based H<small><sub>2</sub></small>O<small><sub>2</sub></small> sensor exhibited a wide linear range (10–1000 μM), high sensitivity and selectivity, and good anti-interference ability. The detection limit and relative standard deviation were 1.7 μM and 4.5% (<em>c</em> = 20 μM, <em>n</em> = 7), respectively. Accordingly, a simple, enzyme-free, and highly efficient method was established for detecting H<small><sub>2</sub></small>O<small><sub>2</sub></small> in aqueous solutions. Moreover, this eco-friendly fluorescent sensor successfully determined the H<small><sub>2</sub></small>O<small><sub>2</sub></small> concentration in human serum samples with 92.0–102.4% recoveries.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 14","pages":" 2894-2901"},"PeriodicalIF":2.7,"publicationDate":"2025-03-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143699137","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Xue Kong, Yi Zhang, Yan Liu, Jinghui Lyu and Zheng-Zhi Yin
{"title":"An electrochemical microsensor for osteopontin based on a molecularly imprinted layer and a built-in probe-functionalized acupuncture needle†","authors":"Xue Kong, Yi Zhang, Yan Liu, Jinghui Lyu and Zheng-Zhi Yin","doi":"10.1039/D5AY00114E","DOIUrl":"10.1039/D5AY00114E","url":null,"abstract":"<p >Osteopontin (OPN) is an important biomarker for reflecting osteoarthritic inflammation and endochondral ossification. In the field of electroanalysis, OPN is a non-electroactive protein, which is usually detected by means of an outer probe or biolabel. Here, a novel microsensor that can directly electroanalyze OPN was constructed by coordinating a surface molecularly imprinted polymer (SMIP) with a built-in electroactive probe of poly(methylene blue) (pMB) on an acupuncture needle microelectrode (ANME). The OPN template can be reversibly anchored using 4-mercaptophenylboronic acid (4-MBPA) <em>via</em> a borate bond between phenylboronic acid and the external <em>cis</em>-diol of the glycoprotein. Methylene blue (MB) and dopamine (DA) were sequentially electropolymerized and grown around templates, which played pivotal roles in the detection signal from the built-in pMB through the imprinted nanocavities. After the recombination of OPN molecules with imprinted nanocavities, the current strength of built-in pMB could be impeded, producing a highly sensitive response. This microsensor shows a linear relationship with the concentration of OPN from 0.01 to 1000 ng mL<small><sup>−1</sup></small> with a detection limit of 3 pg mL<small><sup>−1</sup></small>. The microsensor also exhibits high selectivity and stability, which is attributed to the recognizing ability of the imprinted nanocavities and the hindrance and anti-interference function of coated polydopamine (pDA). This strategy of preparing a sensor shows practical and scientific significance for functionalizing microelectrodes and constructing microsensors for non-electroactive glycoproteins. In the future, it will be fascinating to integrate this microsensor with the acupuncture technique.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 14","pages":" 2902-2910"},"PeriodicalIF":2.7,"publicationDate":"2025-03-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143699134","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
André L. Ferreira, Mayra V. Paschoarelli, William R. de Araujo and Lucas F. de Lima
{"title":"From colors to currents: a hybrid electrochemical and colorimetric sensor for real-time detection of emerging pollutants and pH monitoring†","authors":"André L. Ferreira, Mayra V. Paschoarelli, William R. de Araujo and Lucas F. de Lima","doi":"10.1039/D5AY00054H","DOIUrl":"10.1039/D5AY00054H","url":null,"abstract":"<p >The development of new tools for detecting and monitoring emerging pollutants is highly desired in the environmental field. Here, we report a hybrid multiplexed sensor for colorimetric detection of nitrite (NO<small><sub>2</sub></small><small><sup>−</sup></small>) and pH, along with simultaneous electrochemical detection of methylparaben (MP) and bisphenol A (BPA) in tap, lake and natural water. Through a portable potentiostat and a smartphone, our device provides relevant environmental parameters within two minutes. The colorimetric sensors were fabricated through spot tests, detecting NO<small><sub>2</sub></small><small><sup>−</sup></small> at a concentration ranging from 1 to 200 μmol L<small><sup>−1</sup></small>, with a limit of detection (LOD) of 3.0 μmol L<small><sup>−1</sup></small>. The electrochemical sensors for MP and BPA were fabricated using the laser-scribed graphene (LSG) technique on a polyamide (PI) substrate. We achieved LODs of 0.22 μmol L<small><sup>−1</sup></small> (MP) and 0.057 μmol L<small><sup>−1</sup></small> (BPA), ranging from 1 to 100 μmol L<small><sup>−1</sup></small> for both, and reproducibility with relative standard deviations (RSDs) of 2.5% (MP) and 4.8% (BPA). As a proof-of-concept, our device was tested using real samples of lake, tap and natural water, achieving recoveries from 93% to 120%, demonstrating its suitability for in-field applications for environmental analyses.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 13","pages":" 2697-2707"},"PeriodicalIF":2.7,"publicationDate":"2025-03-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143622803","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Mo Chen, Lidi Gao, Huiying Liu, Jiawen Yu, Fuquan Zhao, Liming Bai, Hongtao Chu, Ming Zhao and Shili Qin
{"title":"Separation of dithiothreitol and dithioerythritol by an open tubular capillary electrochromatographic column with an MOF modified by histidine as the stationary phase†","authors":"Mo Chen, Lidi Gao, Huiying Liu, Jiawen Yu, Fuquan Zhao, Liming Bai, Hongtao Chu, Ming Zhao and Shili Qin","doi":"10.1039/D5AY00097A","DOIUrl":"10.1039/D5AY00097A","url":null,"abstract":"<p >A separation and determination method for dithiothreitol (DTT), as an important small molecule reducing agent, and dithioerythritol (DTE), as a C3-epimer of DTT, was developed <em>via</em> capillary electrochromatography. A functional MOF (His-ZIF-93) was first prepared using ZIF-93 (synthesized <em>via</em> coordination between 4-methylimidazole-5-carbaldehyde and Zn<small><sup>2+</sup></small>) as the framework and <small>D</small>-histidine (<small>D</small>-His) as the modifier, and then it was bonded to the inner wall of the capillary column to obtain a His-ZIF-93 column <em>via</em> the Schiff base reaction. Results showed that the baseline separation of DTT and DTE was easily achieved under wide experimental conditions with an extremely short analysis time of less than 3 min. The success of the separation mechanism was proved through binding constant experiments. There was a good linearity between the concentration (0.10–5.0 mg mL<small><sup>−1</sup></small>) and peak area of DTT and DTE (<em>R</em><small><sup>2</sup></small> ≥ 0.996), and the relative standard deviations for the peak area and retention time were less than 0.93%. The average impurity content of DTE in 5.0 mg per mL DTT was 0.79%. Thus, the method was able to realize simple and fast separation of DTT and DTE and their precise quantification.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 14","pages":" 2887-2893"},"PeriodicalIF":2.7,"publicationDate":"2025-03-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143699138","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Xunjie Zhang, Ke Li, Ruiqing Xian, Pengfei You, Chaochao Liang, Feng Shi, Baojian Hang and Liping Gong
{"title":"Quantification of glucose in the plasma of healthy Chinese volunteers and a bioequivalence study using a surrogate matrix approach combined with UHPLC-MS/MS","authors":"Xunjie Zhang, Ke Li, Ruiqing Xian, Pengfei You, Chaochao Liang, Feng Shi, Baojian Hang and Liping Gong","doi":"10.1039/D4AY02120G","DOIUrl":"10.1039/D4AY02120G","url":null,"abstract":"<p >Acarbose works by competitively inhibiting α-glucosidase, delaying the breakdown of starch into glucose. Thus, it plays an important role in treating type 2 diabetes. Acarbose exhibits unique pharmacokinetic characteristics, and the United States of America (USA) Food and Drug Administration (FDA) has focused on pharmacodynamic parameters rather than pharmacokinetic ones in acarbose bioequivalence studies since issuing its 2009 draft guidance, which was formalized in 2017. A literature review on glucose measurement shows that glucose concentration data are primarily derived from serum matrices. In the 2022 draft guidance, the FDA reaffirmed that plasma glucose concentration is the most suitable pharmacodynamic endpoint for acarbose. This study employed a surrogate matrix method combined with ultra-high performance liquid chromatography-MS/MS (UHPLC-MS/MS) to measure plasma glucose levels. Because glucose is an endogenous substance, directly measuring its concentration in biological matrices does not effectively reflect the impact of acarbose on blood glucose levels. This study used Phosphate Buffered Saline (PBS) as the surrogate matrix to determine glucose concentrations and accurately achieve precise glucose quantification. Moreover, glucose and fructose are structural isomers that are difficult to quickly separate chromatographically, which can affect detection efficiency and introduce interference. Therefore, we aim to develop a rapid, simple, and accurate method for quantifying glucose concentration in human plasma using a surrogate matrix approach combined with UHPLC-MS/MS. Plasma samples were processed using protein precipitation, with glucose-[U-13C6] as the internal standard. Chromatographic separation was performed using a Waters ACQUITY UPLC BEH amide column (100 × 2.1 mm, 1.7 μm), and gradient elution was carried out at a flow rate of 0.4 mL min<small><sup>−1</sup></small> with a mobile phase of 0.05% aqueous ammonia and 0.05% ammonia in acetonitrile. Electrospray ionization (ESI) in negative ion multiple reaction monitoring (MRM) mode was used for detection, with a total analysis time of 6 min. Glucose exhibited good linearity in the concentration range of 2.00 to 20.00 mmol L<small><sup>−1</sup></small> (<em>r</em><small><sup>2</sup></small> = 0.9980), with a precision and accuracy within and between batches of less than 10%. The method was fully validated to ensure data accuracy. This method was successfully applied to a bioequivalence study of acarbose tablets in healthy Chinese subjects in the fasting state, providing valuable data for evaluating the consistency of acarbose formulations.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 13","pages":" 2708-2717"},"PeriodicalIF":2.7,"publicationDate":"2025-03-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://pubs.rsc.org/en/content/articlepdf/2025/ay/d4ay02120g?page=search","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143622805","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}