Journal of separation science最新文献

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Identification, Isolation and Structural Elucidation of New Inner Salt Impurity in Vildagliptin and Metformin Tablet by Using Supercritical Fluid Chromatography, NMR, HRMS 维格列汀二甲双胍片剂中新的内盐杂质的超临界液相色谱、核磁共振、质谱鉴定、分离及结构解析
IF 2.8 3区 工程技术
Journal of separation science Pub Date : 2025-07-12 DOI: 10.1002/jssc.70218
Saravana Kumar Meganathan, Bijaya Ketan Sahoo, Y. Rajender Reddy, K. Rajani, Peedi Rajasekhara Reddy
{"title":"Identification, Isolation and Structural Elucidation of New Inner Salt Impurity in Vildagliptin and Metformin Tablet by Using Supercritical Fluid Chromatography, NMR, HRMS","authors":"Saravana Kumar Meganathan,&nbsp;Bijaya Ketan Sahoo,&nbsp;Y. Rajender Reddy,&nbsp;K. Rajani,&nbsp;Peedi Rajasekhara Reddy","doi":"10.1002/jssc.70218","DOIUrl":"https://doi.org/10.1002/jssc.70218","url":null,"abstract":"<p>Vildagliptin is an orally active antihyperglycemic agent used for the treatment of type 2 diabetes mellitus in adults as monotherapy either alone or in combination with metformin. The presence of impurities in drug substances or drug products could be toxic and unsafe (injurious) to the user, and it should be ensured that drugs must be free of or controlled from any impurities to the specified level as per International Council for Harmonization guidelines before that reaches the user. That is the reason why work on identification, isolation, and characterization of impurities in drug substances and drug products is very important towards ensuring drug safety and efficacy. Further, product-related impurity isolation and characterization is an important aspect of pharmaceutical processes. The aim of the work is to identify a new impurity which was detected in vildagliptin and metformin tablets under stability storage conditions by using high-performance liquid chromatography (HPLC). The new impurity was isolated and characterized by using comprehensive analysis of HPLC, flash chromatography, supercritical fluid chromatography, Fourier transform infrared spectroscopy, high-resolution mass spectrometry, 1D-NMR [<sup>1</sup>H and <sup>13</sup>C], and 2D-NMR (<sup>1</sup>H-<sup>1</sup>H correlated spectroscopy, total correlated spectroscopy, <sup>1</sup>H-<sup>13</sup>C heteronuclear single quantum coherence spectroscopy, <sup>1</sup>H-<sup>13</sup>C and <sup>1</sup>H-<sup>15</sup>N heteronuclear multiple bond coherence spectroscopy) spectroscopic data.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70218","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144606500","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
UiO-66-NH2 Dispersed Solid-Phase Extraction Combined With Liquid Chromatography-Tandem Mass Spectrometry for Metabolomics Analysis in Cancer Patients and Healthy Individuals UiO-66-NH2分散固相萃取联合液相色谱-串联质谱法用于癌症患者和健康个体的代谢组学分析
IF 2.8 3区 工程技术
Journal of separation science Pub Date : 2025-07-12 DOI: 10.1002/jssc.70217
Piao Liu, Changhong Li, Minqi Ou, Chang Yin, Xinyue Kang, Jun Chen, Ran Liu, Jialang Zhuang
{"title":"UiO-66-NH2 Dispersed Solid-Phase Extraction Combined With Liquid Chromatography-Tandem Mass Spectrometry for Metabolomics Analysis in Cancer Patients and Healthy Individuals","authors":"Piao Liu,&nbsp;Changhong Li,&nbsp;Minqi Ou,&nbsp;Chang Yin,&nbsp;Xinyue Kang,&nbsp;Jun Chen,&nbsp;Ran Liu,&nbsp;Jialang Zhuang","doi":"10.1002/jssc.70217","DOIUrl":"https://doi.org/10.1002/jssc.70217","url":null,"abstract":"<div>\u0000 \u0000 <p>A dispersive solid-phase extraction process was established using UiO-66-NH<sub>2</sub> as an adsorbent, in combination with ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) technology, and the performance of this combination for the metabolomic analysis of biological specimens was assessed. Differential metabolites in plasma samples from oral squamous cell carcinoma and hepatocellular carcinoma patients and healthy volunteers were screened, and metabolic pathway enrichment analysis was performed via pseudo-targeted metabolomics. Based on the significantly enriched metabolic pathways and related literature, 20 amino acids were selected and targeted for quantitative analysis. The key parameters for extraction recovery, including the type of liquid in the adsorption system, pH of the eluent, amount of UiO-66-NH<sub>2</sub>, and time of extraction and elution, were optimized based on the selected amino acids. The optimized method demonstrated a remarkable performance: correlation coefficients &gt; 0.99, limits of detection ranging from 0.002 to 0.080 µg/mL (signal-to-noise ratio = 10), and recoveries of 63.9%–110.8% in plasma samples. Thus, via targeted metabolomics analysis, 10 amino acids (including lysine and 3-iodo-L-tyrosine) and 10 amino acids (including arginine and histidine) were determined as potential biomarkers for oral squamous cell carcinoma and hepatocellular carcinoma, respectively. Based on the above potential amino acid markers, discriminant equations for oral squamous cell carcinoma and hepatocellular carcinoma were established, respectively. Two biomarker combinations were successfully screened: lysine and 3-iodo-L-tyrosine (AUC = 0.998, sensitivity = 0.967, specificity = 1.0) for oral squamous cell carcinoma, and histidine and arginine (AUC = 0.944, sensitivity = 0.833, specificity = 0.933) for hepatocellular carcinoma. Our findings will provide new directions for cancer diagnosis.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144606633","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Vortex-Assisted Magnetic Nanofluid-Based Liquid Phase Microextraction of Methylene Blue and Crystal Violet 涡流辅助磁纳米流体液相微萃取亚甲基蓝和结晶紫
IF 2.8 3区 工程技术
Journal of separation science Pub Date : 2025-07-12 DOI: 10.1002/jssc.70225
Xiaochun Chen, Wenxu Hu, Yang Yu, Dandan Ge, Zhehui Weng, Yao Huang, Ren Li
{"title":"Vortex-Assisted Magnetic Nanofluid-Based Liquid Phase Microextraction of Methylene Blue and Crystal Violet","authors":"Xiaochun Chen,&nbsp;Wenxu Hu,&nbsp;Yang Yu,&nbsp;Dandan Ge,&nbsp;Zhehui Weng,&nbsp;Yao Huang,&nbsp;Ren Li","doi":"10.1002/jssc.70225","DOIUrl":"https://doi.org/10.1002/jssc.70225","url":null,"abstract":"<div>\u0000 \u0000 <p>In the present study, a new vortex-assisted magnetic solid phase extraction method was developed based on magnetic ZIF-67 (MZIF-67) nanofluid and supramolecular solvents (SUPRASs) for the extraction and preconcentration of synthetic dyes, followed by high performance liquid chromatography-diode array detector detection. MZIF-67 functionalized with sodium dodecyl sulfate and titanium dioxide (MZIF-67/SDS-TiO<sub>2</sub>) were synthesized and used as magnetic materials. SUPRAS prepared from hexafluorobutanol and nerol was employed as the carrier liquid. Finally, FFs were prepared by adding MZIF-67/SDS-TiO<sub>2</sub> to SUPRAS for the first time. The prepared adsorbents were characterized by scanning electron microscopy, x-ray diffraction, and Fourier transform infrared spectroscopy. The extraction efficiency of the developed method was enhanced by optimization of the influencing parameters. Under the optimized conditions, the linearity was in the range of 9–1000 ng mL<sup>−1</sup> with regression coefficients higher than 0.9961. The limits of detection and limits of quantification were in the range of 2.5–2.7–8.4–9.1 ng mL<sup>−1</sup>, respectively. Finally, the developed method was applied to determine synthetic dyes in river water and beverage samples. Extraction recoveries ranged from 91.0% to 105.8% with relative standard deviations between 0.9% and 7.9%. The green character of the developed method was assessed using the AGREEprep tool. The obtained results indicate that the established method has low environmental impact. The developed method is a simple, cheap, green, and fast and can be applied to determine synthetic dyes in sample solutions.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144606746","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Synthesis of Perfluorooctyl-Functionalized Halloysite Nanotubes for Dispersive Solid-Phase Extraction of Antimalarial Inhibitors in Whole Blood 全血抗疟抑制剂分散固相萃取用全氟辛基功能化高岭土纳米管的合成
IF 2.8 3区 工程技术
Journal of separation science Pub Date : 2025-07-12 DOI: 10.1002/jssc.70226
Kejie Wang, Bingye Shi, Yihui Chen, Chunyan Hou, Xie Li, Xiaoqiang Qiao, Tingting Wang
{"title":"Synthesis of Perfluorooctyl-Functionalized Halloysite Nanotubes for Dispersive Solid-Phase Extraction of Antimalarial Inhibitors in Whole Blood","authors":"Kejie Wang,&nbsp;Bingye Shi,&nbsp;Yihui Chen,&nbsp;Chunyan Hou,&nbsp;Xie Li,&nbsp;Xiaoqiang Qiao,&nbsp;Tingting Wang","doi":"10.1002/jssc.70226","DOIUrl":"https://doi.org/10.1002/jssc.70226","url":null,"abstract":"<div>\u0000 \u0000 <p>Quinine, chloroquine, and hydroxychloroquine are effective antimalarial drugs that have shown antiviral activity against SARS-CoV-2 in initial in vitro studies. However, their excessive use can lead to adverse effects in humans. Therefore, rapid and accurate analysis of these inhibitors in whole blood samples is crucial for public health, although this presents significant challenges. In this study, perfluorooctyl-functionalized halloysite nanotubes were synthesized and used as sorbents for dispersive solid-phase extraction. The developed sorbents interacted with inhibitors through various mechanisms, including hydrophobic interactions, electrostatic interactions, F–π interactions, and hydrogen bonding. Notably, their adsorption capacity was twice that of unmodified halloysite nanotubes. By combining the perfluorooctyl-functionalized halloysite nanotubes-based dispersive solid-phase extraction method with liquid chromatography-tandem mass spectrometry, an analytical method was developed to determine concentrations of the three inhibitors in whole blood samples. Under optimized conditions, the limits of detection ranged from 1.2 to 2.1 ng/mL. The recoveries achieved 91.9%–101.5% for intra-day and 92.8%–101.2% for inter-day. The inter- and intra-day relative standard deviations were in the range of 0.6%–3.8% and 2.3%–8.1%, respectively. This study introduces a novel approach for developing sorbents to target drugs and presents an innovative analytical method for therapeutic monitoring. These advancements will facilitate the evaluation of the pharmacokinetics of these inhibitors in patients and support ongoing clinical trials.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144606748","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Determination of Carbazole Derivatives Associated With Photoelectric Materials in Sediments Using QuEChERS Pretreatment Coupled With Ultra-High Performance Liquid Chromatography-High Resolution Mass Spectrometry QuEChERS预处理-超高效液相色谱-高分辨质谱法测定沉积物中与光电材料相关的咔唑衍生物
IF 2.8 3区 工程技术
Journal of separation science Pub Date : 2025-07-12 DOI: 10.1002/jssc.70214
Qiang Fu, Dunfan Yao, Shuqing He, Yun Fang, Guowei Wang, Jianhua Li, Chunqiao Xiao
{"title":"Determination of Carbazole Derivatives Associated With Photoelectric Materials in Sediments Using QuEChERS Pretreatment Coupled With Ultra-High Performance Liquid Chromatography-High Resolution Mass Spectrometry","authors":"Qiang Fu,&nbsp;Dunfan Yao,&nbsp;Shuqing He,&nbsp;Yun Fang,&nbsp;Guowei Wang,&nbsp;Jianhua Li,&nbsp;Chunqiao Xiao","doi":"10.1002/jssc.70214","DOIUrl":"https://doi.org/10.1002/jssc.70214","url":null,"abstract":"<div>\u0000 \u0000 <p>Carbazole derivatives (CZDs) are an important class of nitrogen-containing heterocyclic compounds which have been widely used in photoelectric materials, dyes, medicine, supramolecules and other fields. The ecological risks of CZDs released into environment during the production and product utilization have gradually attracted people's attention. However, for the lack of analytical methods of CZDs in environment, the levels of CZDs entering the environment remain unclear. Herein, an analytical methodology for simultaneous measuring 13 CZDs associated with photoelectric materials in sediment samples has been established by using ultra-high performance liquid chromatography-high resolution mass spectrometry (UHPLC-HRMS) in combination with a QuEChERS pretreatment technique. The parameters of the sample pretreatment and UHPLC-HRMS analysis were optimized. The established method was validated by evaluating its recovery, accuracy, matrix effect, limits of method detection (LODs), and so on. The instrument detection exhibits a linear response within concentration range of 1 to 1000 µg/L, and the LODs were ranged from 0.005 to 0.165 µg/kg. The average recoveries for the majority of CZDs were in the ranges of 82.9% ∼ 107.0% (spiked level 25 µg/kg), 74.1% ∼ 114.5% (spiked level 10 µg/kg) and 53.3% ∼ 123.7% (spiked level 2 µg/kg), respectively, and the relative standard deviations of all spiked levels were between 0.47% and 11.30%. The developed methodology was applied to the analysis of twenty sediment samples. A CZD of 2-methoxycarbazole (2-MOCZ) has been firstly detected in the sediments with the concentration up to1.4 µg/kg, indicating the environmental occurrence of CZDs and alerting to their potentially ecological risks in the environment.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144606747","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Sustainable Microextraction Using Switchable Solubility Solvent for the Liquid Chromatographic Determination of Three Profenoid Drugs in Urine Samples 可调溶解度溶剂可持续微萃取液相色谱法测定尿液样品中3种类丙烯类药物
IF 2.8 3区 工程技术
Journal of separation science Pub Date : 2025-07-12 DOI: 10.1002/jssc.70223
Christina Patakidou, Marianna Ntorkou, Constantinos K. Zacharis
{"title":"Sustainable Microextraction Using Switchable Solubility Solvent for the Liquid Chromatographic Determination of Three Profenoid Drugs in Urine Samples","authors":"Christina Patakidou,&nbsp;Marianna Ntorkou,&nbsp;Constantinos K. Zacharis","doi":"10.1002/jssc.70223","DOIUrl":"https://doi.org/10.1002/jssc.70223","url":null,"abstract":"<p>Herein, a switchable solubility solvent (sodium salicylate) was employed for the microextraction of “profenoid” drugs (i.e., ketoprofen, fenoprofen, and flurbiprofen) from human urine samples. This approach utilizes the phase transition of salicylic acid (0.75 mol/L) by altering the sample's pH (addition of 10 µL of H<sub>3</sub>PO<sub>4</sub> 10 M), facilitating efficient dispersion and phase separation in a single step. The solidified salicylic acid was easily collected using a syringe filter (nylon). In addition, the extensive contact area between the solidified solvent and the sample solution ensured effective extraction of the target analyte. The critical experimental parameters affecting the extraction performance of the analytes were examined. The separation of the drugs was carried out on a C<sub>18</sub> analytical column using gradient elution. Excellent linearity was observed in the dynamic range of 50–3000 ng/mL while the precision (%RSD) was less than 14.3% in all cases. The intraday and interday trueness were satisfactory, being in the range of 82.3%–110.1%. The green potential of the proposed analytical scheme was examined based on AGREEprep, ComplexMoGAPI, CACI, and AGREE metric tools. The developed method was utilized for the analysis of authentic urine samples after oral administration of a ketoprofen-containing formulation.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70223","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144606502","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Determination of Carbazole Derivatives Associated With Photoelectric Materials in Sediments Using QuEChERS Pretreatment Coupled With Ultra-High Performance Liquid Chromatography-High Resolution Mass Spectrometry QuEChERS预处理-超高效液相色谱-高分辨质谱法测定沉积物中与光电材料相关的咔唑衍生物
IF 2.8 3区 工程技术
Journal of separation science Pub Date : 2025-07-12 DOI: 10.1002/jssc.70214
Qiang Fu, Dunfan Yao, Shuqing He, Yun Fang, Guowei Wang, Jianhua Li, Chunqiao Xiao
{"title":"Determination of Carbazole Derivatives Associated With Photoelectric Materials in Sediments Using QuEChERS Pretreatment Coupled With Ultra-High Performance Liquid Chromatography-High Resolution Mass Spectrometry","authors":"Qiang Fu,&nbsp;Dunfan Yao,&nbsp;Shuqing He,&nbsp;Yun Fang,&nbsp;Guowei Wang,&nbsp;Jianhua Li,&nbsp;Chunqiao Xiao","doi":"10.1002/jssc.70214","DOIUrl":"https://doi.org/10.1002/jssc.70214","url":null,"abstract":"<div>\u0000 \u0000 <p>Carbazole derivatives (CZDs) are an important class of nitrogen-containing heterocyclic compounds which have been widely used in photoelectric materials, dyes, medicine, supramolecules and other fields. The ecological risks of CZDs released into environment during the production and product utilization have gradually attracted people's attention. However, for the lack of analytical methods of CZDs in environment, the levels of CZDs entering the environment remain unclear. Herein, an analytical methodology for simultaneous measuring 13 CZDs associated with photoelectric materials in sediment samples has been established by using ultra-high performance liquid chromatography-high resolution mass spectrometry (UHPLC-HRMS) in combination with a QuEChERS pretreatment technique. The parameters of the sample pretreatment and UHPLC-HRMS analysis were optimized. The established method was validated by evaluating its recovery, accuracy, matrix effect, limits of method detection (LODs), and so on. The instrument detection exhibits a linear response within concentration range of 1 to 1000 µg/L, and the LODs were ranged from 0.005 to 0.165 µg/kg. The average recoveries for the majority of CZDs were in the ranges of 82.9% ∼ 107.0% (spiked level 25 µg/kg), 74.1% ∼ 114.5% (spiked level 10 µg/kg) and 53.3% ∼ 123.7% (spiked level 2 µg/kg), respectively, and the relative standard deviations of all spiked levels were between 0.47% and 11.30%. The developed methodology was applied to the analysis of twenty sediment samples. A CZD of 2-methoxycarbazole (2-MOCZ) has been firstly detected in the sediments with the concentration up to1.4 µg/kg, indicating the environmental occurrence of CZDs and alerting to their potentially ecological risks in the environment.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144606498","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
UiO-66-NH2 Dispersed Solid-Phase Extraction Combined With Liquid Chromatography-Tandem Mass Spectrometry for Metabolomics Analysis in Cancer Patients and Healthy Individuals UiO-66-NH2分散固相萃取联合液相色谱-串联质谱法用于癌症患者和健康个体的代谢组学分析
IF 2.8 3区 工程技术
Journal of separation science Pub Date : 2025-07-12 DOI: 10.1002/jssc.70217
Piao Liu, Changhong Li, Minqi Ou, Chang Yin, Xinyue Kang, Jun Chen, Ran Liu, Jialang Zhuang
{"title":"UiO-66-NH2 Dispersed Solid-Phase Extraction Combined With Liquid Chromatography-Tandem Mass Spectrometry for Metabolomics Analysis in Cancer Patients and Healthy Individuals","authors":"Piao Liu,&nbsp;Changhong Li,&nbsp;Minqi Ou,&nbsp;Chang Yin,&nbsp;Xinyue Kang,&nbsp;Jun Chen,&nbsp;Ran Liu,&nbsp;Jialang Zhuang","doi":"10.1002/jssc.70217","DOIUrl":"https://doi.org/10.1002/jssc.70217","url":null,"abstract":"<div>\u0000 \u0000 <p>A dispersive solid-phase extraction process was established using UiO-66-NH<sub>2</sub> as an adsorbent, in combination with ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) technology, and the performance of this combination for the metabolomic analysis of biological specimens was assessed. Differential metabolites in plasma samples from oral squamous cell carcinoma and hepatocellular carcinoma patients and healthy volunteers were screened, and metabolic pathway enrichment analysis was performed via pseudo-targeted metabolomics. Based on the significantly enriched metabolic pathways and related literature, 20 amino acids were selected and targeted for quantitative analysis. The key parameters for extraction recovery, including the type of liquid in the adsorption system, pH of the eluent, amount of UiO-66-NH<sub>2</sub>, and time of extraction and elution, were optimized based on the selected amino acids. The optimized method demonstrated a remarkable performance: correlation coefficients &gt; 0.99, limits of detection ranging from 0.002 to 0.080 µg/mL (signal-to-noise ratio = 10), and recoveries of 63.9%–110.8% in plasma samples. Thus, via targeted metabolomics analysis, 10 amino acids (including lysine and 3-iodo-L-tyrosine) and 10 amino acids (including arginine and histidine) were determined as potential biomarkers for oral squamous cell carcinoma and hepatocellular carcinoma, respectively. Based on the above potential amino acid markers, discriminant equations for oral squamous cell carcinoma and hepatocellular carcinoma were established, respectively. Two biomarker combinations were successfully screened: lysine and 3-iodo-L-tyrosine (AUC = 0.998, sensitivity = 0.967, specificity = 1.0) for oral squamous cell carcinoma, and histidine and arginine (AUC = 0.944, sensitivity = 0.833, specificity = 0.933) for hepatocellular carcinoma. Our findings will provide new directions for cancer diagnosis.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144606752","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Sustainable Microextraction Using Switchable Solubility Solvent for the Liquid Chromatographic Determination of Three Profenoid Drugs in Urine Samples 可调溶解度溶剂可持续微萃取液相色谱法测定尿液样品中3种类丙烯类药物
IF 2.8 3区 工程技术
Journal of separation science Pub Date : 2025-07-12 DOI: 10.1002/jssc.70223
Christina Patakidou, Marianna Ntorkou, Constantinos K. Zacharis
{"title":"Sustainable Microextraction Using Switchable Solubility Solvent for the Liquid Chromatographic Determination of Three Profenoid Drugs in Urine Samples","authors":"Christina Patakidou,&nbsp;Marianna Ntorkou,&nbsp;Constantinos K. Zacharis","doi":"10.1002/jssc.70223","DOIUrl":"https://doi.org/10.1002/jssc.70223","url":null,"abstract":"<p>Herein, a switchable solubility solvent (sodium salicylate) was employed for the microextraction of “profenoid” drugs (i.e., ketoprofen, fenoprofen, and flurbiprofen) from human urine samples. This approach utilizes the phase transition of salicylic acid (0.75 mol/L) by altering the sample's pH (addition of 10 µL of H<sub>3</sub>PO<sub>4</sub> 10 M), facilitating efficient dispersion and phase separation in a single step. The solidified salicylic acid was easily collected using a syringe filter (nylon). In addition, the extensive contact area between the solidified solvent and the sample solution ensured effective extraction of the target analyte. The critical experimental parameters affecting the extraction performance of the analytes were examined. The separation of the drugs was carried out on a C<sub>18</sub> analytical column using gradient elution. Excellent linearity was observed in the dynamic range of 50–3000 ng/mL while the precision (%RSD) was less than 14.3% in all cases. The intraday and interday trueness were satisfactory, being in the range of 82.3%–110.1%. The green potential of the proposed analytical scheme was examined based on AGREEprep, ComplexMoGAPI, CACI, and AGREE metric tools. The developed method was utilized for the analysis of authentic urine samples after oral administration of a ketoprofen-containing formulation.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70223","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144606750","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
A Facile Hydrophilic Coating to Construct Immobilized Metal Affinity Chromatography for Protein Adsorption 构建固定化金属亲和层析用于蛋白质吸附的易溶亲水涂层
IF 2.8 3区 工程技术
Journal of separation science Pub Date : 2025-07-12 DOI: 10.1002/jssc.70219
Xiao-Bei Huang, Yong-Ming Wei, Lin Yu, Zhen-Liang Xu, Hu Yang
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