Journal of separation science最新文献

{"title":"Interactions of Epinephrine and Norepinephrine with Intralipid Emulsion Studied by Capillary Electrokinetic Chromatography","authors":"Dumidu Perera,&nbsp;Henri K. M. Ravald,&nbsp;Veronika Šolínová,&nbsp;Václav Kašička,&nbsp;Ju-Tae Sohn,&nbsp;Susanne K. Wiedmer","doi":"10.1002/jssc.70188","DOIUrl":"https://doi.org/10.1002/jssc.70188","url":null,"abstract":"<p>Epinephrine and norepinephrine are widely used to treat cardiovascular collapse during resuscitation with lipid emulsions in the treatment of drug toxicity including local or non-local anesthetics. The effect of the lipid emulsion Intralipid on the vasoconstriction induced by epinephrine or norepinephrine is, however, still unknown. In this study, the interaction of epinephrine and norepinephrine with the intravenous Intralipid emulsion was investigated by capillary electromigration techniques. Capillary electrokinetic chromatography was performed to determine the distribution coefficients by running the analytes under different experimental conditions (temperature, ionic strength, and pH) through a capillary filled with the background electrolyte containing Intralipid emulsion. In addition, the binding constants of the epinephrine and norepinephrine complexes with Intralipid emulsion were determined based on the effective electrophoretic mobility data obtained by electrokinetic chromatography at a wide concentration range of Intralipid emulsion. The obtained binding constants, as well as the distribution coefficients determined by electrokinetic chromatography, confirm that epinephrine and norepinephrine are hydrophilic compounds and that they are minimally distributed into the Intralipid emulsion. Therefore, their application as drugs for vasoconstriction upon Intralipid emulsion treatment is well motivated.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 6","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-06-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70188","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144244903","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}

{"title":"Improvement of Pharmacopeial High-Performance Liquid Chromatography Method for Determination of Enantiomeric Purity of Moxifloxacin Drug Substance","authors":"Alma Salkić,&nbsp;Biljana Otašević,&nbsp;Mira Zečević","doi":"10.1002/jssc.70190","DOIUrl":"https://doi.org/10.1002/jssc.70190","url":null,"abstract":"<div>\u0000 \u0000 <p>New chiral isocratic HPLC conditions were proposed for investigation of moxifloxacin hydrochloride and its potential isomeric impurity (R,R)-isomer (impurity G) using the chiral additive copper (II)-sulfate and isoleucine in the mobile phase using an achiral C18 chromatographic column, 150 × 4.6 mm; 3 µm, as a significant improvement of the official European Pharmacopeia method concerning economy and baseline resolution. The mechanism of separation of enantiomers of moxifloxacin using the chiral additive copper (II)-sulfate is also elucidated. In the optimization of the experimental conditions of the chiral HPLC method, the central composite design was used, and for multiobjective optimization the desirability function with its desired value 1.00 was used. After optimization and method validation the best conditions concerning the concentration of chiral agents (0.01 M), organic solvent content in the mobile phase (30%, v/v methanol), pH value of mobile phase (3.5), and column temperature (23°C) with 10 µL injection volume, were defined. Compared to the pharmacopeial HPLC method, the analysis time was shorter and significantly lower amount of chiral agents in mobile phase was required. The optimized method was validated with respect to linearity, accuracy, precision, and robustness. The linearity of the method has been demonstrated in the range of 0.30–2.50 µg/mL (<i>R</i>² &gt; 0.998). Limit of detection and limit of quantification for moxifloxacin chiral impurity G determination were 0.098 and 0.298 µg/mL, respectively. The method was found to be suitable for quantification of moxifloxacin chiral impurity G in moxifloxacin drug substance.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 6","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-06-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144244163","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}

{"title":"Automatic Magnetic Dispersive Solid-Phase Extraction Combined With LC-MS/MS for the Rapid Quantitation of Six Gelsemium elegans Alkaloids in Biological Samples","authors":"Luyao Yang,&nbsp;Chunfang Ni,&nbsp;Chen Liang,&nbsp;Qianya Deng,&nbsp;Siyang He","doi":"10.1002/jssc.70153","DOIUrl":"https://doi.org/10.1002/jssc.70153","url":null,"abstract":"<p>In this study, an innovative, rapid, and automated method for quantifying six <i>Gelsemium elegans</i> alkaloids in biological samples using magnetic dispersive solid-phase extraction (MDSPE) and liquid chromatography tandem mass spectrometry (LC-MS/MS). Magnetic HLB extractant, NaH₂PO₄/Na₂HPO₄ buffer (0.2 M, pH 7) and acetonitrile were used in automatic MDSPE. The average pretreatment time was less than 2 min per sample. Atropine-d3 was employed as the internal standard (IS). The six alkaloids demonstrated a linear response (<i>R</i>² &gt; 0.997) in the concentration range of 1∼100 ng/mL and 2∼200 ng/g. Precision and accuracy were within ± 15%, and the extraction recovery rates for each alkaloid ranged from 60.32% to 105.32%. The samples were found to be stable under various conditions. In summary, we present the first automated MDSPE-LC-MS/MS method for simultaneous quantification of six <i>Gelsemium elegans</i> alkaloids (gelsemine, koumine, humantenmine, humantenine, humantenidine, and humantenirine) in multiple biological matrices (whole blood, urine, liver). Unlike prior studies focused on one to two analytes or single matrices, this method achieves unparalleled specificity for six alkaloids with detection limits up to 0.01 ng/mL (0.02 ng/g), addressing critical gaps in forensic toxicology for complex poisoning cases.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 6","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-06-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144244870","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}

{"title":"Interactions of Epinephrine and Norepinephrine with Intralipid Emulsion Studied by Capillary Electrokinetic Chromatography","authors":"Dumidu Perera,&nbsp;Henri K. M. Ravald,&nbsp;Veronika Šolínová,&nbsp;Václav Kašička,&nbsp;Ju-Tae Sohn,&nbsp;Susanne K. Wiedmer","doi":"10.1002/jssc.70188","DOIUrl":"https://doi.org/10.1002/jssc.70188","url":null,"abstract":"<p>Epinephrine and norepinephrine are widely used to treat cardiovascular collapse during resuscitation with lipid emulsions in the treatment of drug toxicity including local or non-local anesthetics. The effect of the lipid emulsion Intralipid on the vasoconstriction induced by epinephrine or norepinephrine is, however, still unknown. In this study, the interaction of epinephrine and norepinephrine with the intravenous Intralipid emulsion was investigated by capillary electromigration techniques. Capillary electrokinetic chromatography was performed to determine the distribution coefficients by running the analytes under different experimental conditions (temperature, ionic strength, and pH) through a capillary filled with the background electrolyte containing Intralipid emulsion. In addition, the binding constants of the epinephrine and norepinephrine complexes with Intralipid emulsion were determined based on the effective electrophoretic mobility data obtained by electrokinetic chromatography at a wide concentration range of Intralipid emulsion. The obtained binding constants, as well as the distribution coefficients determined by electrokinetic chromatography, confirm that epinephrine and norepinephrine are hydrophilic compounds and that they are minimally distributed into the Intralipid emulsion. Therefore, their application as drugs for vasoconstriction upon Intralipid emulsion treatment is well motivated.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 6","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-06-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70188","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144244161","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}

{"title":"Targeted Separation of Sesquiterpenoids From Dalbergia odorifera T. Chen by High-Speed Countercurrent Chromatography for the Quality Control of Xiangdan Injection","authors":"Yanqi Yang,&nbsp;Yaxuan Bai,&nbsp;Jun Li,&nbsp;Yingfeng Pan,&nbsp;Binbin Shen,&nbsp;Shengqiang Tong,&nbsp;Jizhong Yan,&nbsp;Hui Zhang","doi":"10.1002/jssc.70194","DOIUrl":"https://doi.org/10.1002/jssc.70194","url":null,"abstract":"<div>\u0000 \u0000 <p>This study developed an efficient separation strategy combining high-speed countercurrent chromatography and semi-preparative HPLC for the isolation of sesquiterpenoids from the volatile oil of <i>Dalbergia odorifera</i>, thereby improving the quality control of Xiangdan injection. Initially, the enriched volatile oil was processed using high-speed countercurrent chromatography with a solvent system of <i>n</i>-hexane/ethyl acetate/acetonitrile/water (6:1:6:2, v/v/v/v). Within 350 min, four nerolidol oxides were successfully separated, and a sesquiterpenoid compound was markedly enriched. Then, the enriched compound was further purified using semi-preparative HPLC. HPLC analysis indicated that the strategy successfully separated five sesquiterpenoid compounds from <i>D. odorifera</i> with purities exceeding 91%. Electrospray ionization mass spectrometry and nuclear magnetic resonance spectroscopy were employed to confirm the structures of five isolated compounds. The five isolated compounds were identified as dalberpene (Compound I), nerolidol oxide I (Compound II), nerolidol oxide II (Compound III), nerolidol oxide III (Compound IV), and nerolidol oxide IV (Compound V). Subsequently, based on the HPLC characteristic chromatogram, the isolated compounds, including dalberpene, nerolidol oxide I, nerolidol oxide II, nerolidol oxide IV, and commercially purchased elemicin, were selected as five target analytes for the quality control of <i>D. odorifera</i> components in Xiangdan injection. The previously developed dispersive liquid–liquid microextraction-back extraction method was further optimized and rigorously validated. The results indicated that the average concentrations of five target analytes in Xiangdan injection samples ranged from 0.105 to 4.990 µg/mL. Compared with previous studies, this study significantly improved the specificity and accuracy of quality control for <i>D. odorifera</i> components in Xiangdan injection.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 6","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-06-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144232362","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}

{"title":"Targeted Separation of Sesquiterpenoids From Dalbergia odorifera T. Chen by High-Speed Countercurrent Chromatography for the Quality Control of Xiangdan Injection","authors":"Yanqi Yang,&nbsp;Yaxuan Bai,&nbsp;Jun Li,&nbsp;Yingfeng Pan,&nbsp;Binbin Shen,&nbsp;Shengqiang Tong,&nbsp;Jizhong Yan,&nbsp;Hui Zhang","doi":"10.1002/jssc.70194","DOIUrl":"https://doi.org/10.1002/jssc.70194","url":null,"abstract":"<div>\u0000 \u0000 <p>This study developed an efficient separation strategy combining high-speed countercurrent chromatography and semi-preparative HPLC for the isolation of sesquiterpenoids from the volatile oil of <i>Dalbergia odorifera</i>, thereby improving the quality control of Xiangdan injection. Initially, the enriched volatile oil was processed using high-speed countercurrent chromatography with a solvent system of <i>n</i>-hexane/ethyl acetate/acetonitrile/water (6:1:6:2, v/v/v/v). Within 350 min, four nerolidol oxides were successfully separated, and a sesquiterpenoid compound was markedly enriched. Then, the enriched compound was further purified using semi-preparative HPLC. HPLC analysis indicated that the strategy successfully separated five sesquiterpenoid compounds from <i>D. odorifera</i> with purities exceeding 91%. Electrospray ionization mass spectrometry and nuclear magnetic resonance spectroscopy were employed to confirm the structures of five isolated compounds. The five isolated compounds were identified as dalberpene (Compound I), nerolidol oxide I (Compound II), nerolidol oxide II (Compound III), nerolidol oxide III (Compound IV), and nerolidol oxide IV (Compound V). Subsequently, based on the HPLC characteristic chromatogram, the isolated compounds, including dalberpene, nerolidol oxide I, nerolidol oxide II, nerolidol oxide IV, and commercially purchased elemicin, were selected as five target analytes for the quality control of <i>D. odorifera</i> components in Xiangdan injection. The previously developed dispersive liquid–liquid microextraction-back extraction method was further optimized and rigorously validated. The results indicated that the average concentrations of five target analytes in Xiangdan injection samples ranged from 0.105 to 4.990 µg/mL. Compared with previous studies, this study significantly improved the specificity and accuracy of quality control for <i>D. odorifera</i> components in Xiangdan injection.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 6","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-06-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144232313","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}

{"title":"Covalent/Metal–Organic Skeleton Composites for Solid-Phase Extraction of Ultraviolet Absorbers in Environmental Samples","authors":"Mengxi Li,&nbsp;Xinrui Tian,&nbsp;Jiayi Song,&nbsp;Ping Su,&nbsp;Yi Yang","doi":"10.1002/jssc.70186","DOIUrl":"https://doi.org/10.1002/jssc.70186","url":null,"abstract":"<div>\u0000 \u0000 <p>In this study, novel covalent/metal–organic skeleton composites (TpBD@MIL-68; 2,4,6-triformylphloroglucinol (Tp) and benzidine (BD)) were combined with high-performance liquid chromatography (HPLC) and used to develop a method for detecting ultraviolet absorbers, including 4-(4,6-diphenyl-1,3,5-triazin-2-yl)benzene-1,3-diol (Appolo-116), 3-benzenediol, 4-[4,6-bis(2,4-dimethylphenyl)-1,3,5-triazin-2-yl]-1 (DBDT), 2,4,6-triphenyl-s-triazine (TPTZ), 2,4,6-trip-tolyl-1.3.5-triazine, 2-(4,6-diphenyl-1,3,5-triazin-2-yl)-5-((hexyl)oxy)phenol (UV-1577), and 2-(4,6-bis-(2,4-dimethylphenyl)-1,3,5-triazin-2-yl)-5-(octyloxy)-phenol (UV-1164) is present in greenhouse films and soils. TpBD@MIL-68 has the unique characteristics of a covalent organic framework and a metal–organic framework. TpBD@MIL-68 exhibited a higher extraction efficiency because of π–π and electrostatic interactions between the benzene ring structure of the TpBD, MIL-68, and the ultraviolet absorber molecules. The extraction conditions, including the adsorbent dosage, eluent type and dosage, elution time, and the pH of the sample solution, were fully optimized. The extraction efficiency of TpBD@MIL-68 exceeded 80%. The detection results showed good linearity over a wide range of concentrations (5–5000 µg/L) and low detection limits (0.61–0.94 ng/mL) for target molecules. The practicability of this solid-phase extraction (SPE)–HPLC method was further evaluated by analyzing greenhouse films and soils, with target recoveries of 80.9%–109.9% and relative standard deviations of less than 8.9%. The as-synthesized TpBD@MIL-68 adsorbent exhibited great potential in ultraviolet absorber analysis.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 6","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-06-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144220068","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}

{"title":"Comprehensive Quality Evaluation of Viticis Fructus Based on Simultaneous Quantification of Nine Flavones and One Iridoid Glycoside by Ultra-High Performance Liquid Chromatography Electrospray Ionization Tandem Mass Spectrometry and Chemometric Analysis","authors":"Wen-Jing Ren,&nbsp;Yi-Zhe Liu,&nbsp;Rezeye Aili,&nbsp;Zhao-Xia Li,&nbsp;Feng Qiu","doi":"10.1002/jssc.70174","DOIUrl":"https://doi.org/10.1002/jssc.70174","url":null,"abstract":"<div>\u0000 \u0000 <p>Viticis fructus is the dry fruit of <i>Vitex trifolia</i> L. var. <i>simplicifolia</i> Cham. or <i>Vitex trifolia</i> L., both belonging to the family Verbenaceae. Viticis fructus can grow well in saline alkali lands, and is currently an important industrial raw material for extracting flavones and iridoid glycosides for medicinal use. However, the significance of differences in the chemical components of Viticis fructus from different production areas is not yet clear. Therefore, a sensitive, selective, and accurate UHPLC–ESI–MS/MS method with high selectivity and efficiency was established and validated for simultaneous quantification of nine flavones and one iridoid glycoside in Viticis fructus. A comprehensive quality evaluation of 36 batches of Viticis fructus samples collected from 10 main production areas in China was performed using this method and chemometric analysis. The contents of vitexicarpin in 36 batches of samples were all higher than 0.030% (300 µg/g), which met the requirements of <i>Chinese Pharmacopoeia</i> (2020 edition). However, the contents of the 10 active ingredients from different production areas were quite different. The contents of nine flavones and one iridoid glycoside in Viticis fructus were greatly affected by the growth environment. Humid climatic conditions were relatively favorable for the accumulation of active components in Viticis fructus. The flavone and iridoid glycoside contents were higher in the samples from Shandong, Jiangxi, Guangxi, and Guizhou. Chemometric analysis also showed that vitexicarpin, chrysosplenol D, and agnuside could well represent the total flavones and iridoid glycoside of Viticis fructus for the classification and evaluation of the overall quality of Viticis fructus from different regions. These three representative components can be used as markers to evaluate the quality of Viticis fructus, providing a reliable theoretical and experimental basis for improving the quality standards of Viticis fructus.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 6","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-06-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144220069","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}

{"title":"Comprehensive Quality Evaluation of Viticis Fructus Based on Simultaneous Quantification of Nine Flavones and One Iridoid Glycoside by Ultra-High Performance Liquid Chromatography Electrospray Ionization Tandem Mass Spectrometry and Chemometric Analysis","authors":"Wen-Jing Ren,&nbsp;Yi-Zhe Liu,&nbsp;Rezeye Aili,&nbsp;Zhao-Xia Li,&nbsp;Feng Qiu","doi":"10.1002/jssc.70174","DOIUrl":"https://doi.org/10.1002/jssc.70174","url":null,"abstract":"<div>\u0000 \u0000 <p>Viticis fructus is the dry fruit of <i>Vitex trifolia</i> L. var. <i>simplicifolia</i> Cham. or <i>Vitex trifolia</i> L., both belonging to the family Verbenaceae. Viticis fructus can grow well in saline alkali lands, and is currently an important industrial raw material for extracting flavones and iridoid glycosides for medicinal use. However, the significance of differences in the chemical components of Viticis fructus from different production areas is not yet clear. Therefore, a sensitive, selective, and accurate UHPLC–ESI–MS/MS method with high selectivity and efficiency was established and validated for simultaneous quantification of nine flavones and one iridoid glycoside in Viticis fructus. A comprehensive quality evaluation of 36 batches of Viticis fructus samples collected from 10 main production areas in China was performed using this method and chemometric analysis. The contents of vitexicarpin in 36 batches of samples were all higher than 0.030% (300 µg/g), which met the requirements of <i>Chinese Pharmacopoeia</i> (2020 edition). However, the contents of the 10 active ingredients from different production areas were quite different. The contents of nine flavones and one iridoid glycoside in Viticis fructus were greatly affected by the growth environment. Humid climatic conditions were relatively favorable for the accumulation of active components in Viticis fructus. The flavone and iridoid glycoside contents were higher in the samples from Shandong, Jiangxi, Guangxi, and Guizhou. Chemometric analysis also showed that vitexicarpin, chrysosplenol D, and agnuside could well represent the total flavones and iridoid glycoside of Viticis fructus for the classification and evaluation of the overall quality of Viticis fructus from different regions. These three representative components can be used as markers to evaluate the quality of Viticis fructus, providing a reliable theoretical and experimental basis for improving the quality standards of Viticis fructus.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 6","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-06-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144220067","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}

{"title":"Covalent/Metal–Organic Skeleton Composites for Solid-Phase Extraction of Ultraviolet Absorbers in Environmental Samples","authors":"Mengxi Li,&nbsp;Xinrui Tian,&nbsp;Jiayi Song,&nbsp;Ping Su,&nbsp;Yi Yang","doi":"10.1002/jssc.70186","DOIUrl":"https://doi.org/10.1002/jssc.70186","url":null,"abstract":"<div>\u0000 \u0000 <p>In this study, novel covalent/metal–organic skeleton composites (TpBD@MIL-68; 2,4,6-triformylphloroglucinol (Tp) and benzidine (BD)) were combined with high-performance liquid chromatography (HPLC) and used to develop a method for detecting ultraviolet absorbers, including 4-(4,6-diphenyl-1,3,5-triazin-2-yl)benzene-1,3-diol (Appolo-116), 3-benzenediol, 4-[4,6-bis(2,4-dimethylphenyl)-1,3,5-triazin-2-yl]-1 (DBDT), 2,4,6-triphenyl-s-triazine (TPTZ), 2,4,6-trip-tolyl-1.3.5-triazine, 2-(4,6-diphenyl-1,3,5-triazin-2-yl)-5-((hexyl)oxy)phenol (UV-1577), and 2-(4,6-bis-(2,4-dimethylphenyl)-1,3,5-triazin-2-yl)-5-(octyloxy)-phenol (UV-1164) is present in greenhouse films and soils. TpBD@MIL-68 has the unique characteristics of a covalent organic framework and a metal–organic framework. TpBD@MIL-68 exhibited a higher extraction efficiency because of π–π and electrostatic interactions between the benzene ring structure of the TpBD, MIL-68, and the ultraviolet absorber molecules. The extraction conditions, including the adsorbent dosage, eluent type and dosage, elution time, and the pH of the sample solution, were fully optimized. The extraction efficiency of TpBD@MIL-68 exceeded 80%. The detection results showed good linearity over a wide range of concentrations (5–5000 µg/L) and low detection limits (0.61–0.94 ng/mL) for target molecules. The practicability of this solid-phase extraction (SPE)–HPLC method was further evaluated by analyzing greenhouse films and soils, with target recoveries of 80.9%–109.9% and relative standard deviations of less than 8.9%. The as-synthesized TpBD@MIL-68 adsorbent exhibited great potential in ultraviolet absorber analysis.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 6","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-06-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144220070","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}