Journal of separation science最新文献_第10页

An Optimized and Sensitive UHPLC-ESI-Q-TOF/HRMS Demonstrated the Dynamic Profiling of Allantoin, N-trans-Feruloyl-3-Methoxytyramine, and N-p-Coumaroyltyramine from Portulaca oleracea L. In Vivo in Rats 优化且灵敏的 UHPLC-ESI-Q-TOF/HRMS 显示了大鼠体内马齿苋中尿囊素、N-反式-阿魏酰-3-甲氧基酪胺和 N-对香豆酰酪胺的动态轮廓。

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2024-12-31 DOI: 10.1002/jssc.70055

Kexian Li, Wei Wang

{"title":"An Optimized and Sensitive UHPLC-ESI-Q-TOF/HRMS Demonstrated the Dynamic Profiling of Allantoin, N-trans-Feruloyl-3-Methoxytyramine, and N-p-Coumaroyltyramine from Portulaca oleracea L. In Vivo in Rats","authors":"Kexian Li, Wei Wang","doi":"10.1002/jssc.70055","DOIUrl":"10.1002/jssc.70055","url":null,"abstract":"<div>\u0000 \u0000 This study revealed the dynamic profiling of three main components of Portulaca oleracea L. in vivo in rats, namely allantoin (A), N-trans-feruloyl-3-methoxytyramine (M), and N-p-coumaroyltyramine (C). A sensitive and efficient UHPLC-ESI-Q-TOF/HRMS, including an optimized separation process, was applied to their qualitative and quantitative analysis. The validation of the method presented the correlation coefficients, which were over 0.997. The mean matrix factors were 0.930. Recoveries ranged from 96.6% to 109.2%, and determination accuracy varied from 95% to 109.4%. The biological samples included rat plasma, liver, kidneys, bile, and excreta taken after a single oral administration of the saturated DMSO solution of P. oleracea extract. The contents of A, M, and C were of 2.5, 5.1, and 3.4 g/kg in the dry whole herb, respectively. A was identified in the liver and kidneys from 0 to 6 h. Allantoic acid, as one metabolite of A, was found to be kept in plasma for a short time, but another two successive metabolites of A remained over 6 h. It depicted a pharmacological material basis of the herb, regarded with A. The glucuronidation and/or sulfation of M and C were detected in rat bile from 0 to 12 h. The complicated but interesting metabolic schemes for A, M, and C were illustrated from their HRMS and MS/MS performance.\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 1","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-12-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142907210","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

Efficient and Sensitive Detection of Organophosphate Pesticides in Orange Juice Using Dispersed Solid-Phase Extraction Based on Amorphous UiO-66 基于非晶UiO-66的分散固相萃取高效灵敏检测橙汁中有机磷农药

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2024-12-30 DOI: 10.1002/jssc.70066

Yaqi Yin, Chen Fan, Linru Cheng, Yuwei Shan

{"title":"Efficient and Sensitive Detection of Organophosphate Pesticides in Orange Juice Using Dispersed Solid-Phase Extraction Based on Amorphous UiO-66","authors":"Yaqi Yin, Chen Fan, Linru Cheng, Yuwei Shan","doi":"10.1002/jssc.70066","DOIUrl":"10.1002/jssc.70066","url":null,"abstract":"<div>\u0000 \u0000 Organophosphate pesticides can cause long-term neurological damage to humans. There is an urgent need to develop a more sensitive and efficient method for detecting trace amounts of organophosphorus pesticides in orange juice, particularly in the presence of interfering substances. This study developed a dispersive solid-phase extraction (DSPE) method using amorphous UiO-66 (aUiO-66) as an adsorbent for the detection of four organophosphate pesticides (fenthion, profenofos, fensulfothion, and chlorpyrifos) in orange juice. The aUiO-66 was synthesized in a green, direct method within a deep eutectic solvent composed of diethanolamine hydrochloride and acetamide. Its amorphous nature was confirmed through x-ray diffraction (XRD) and thermogravimetric analysis (TGA). Parameters influencing extraction efficiency, including adsorbent dosage, extraction time, eluent type, and volume, were optimized by genetic neural network (GNN). The method demonstrated good linearity (R2 = 0.9927–0.9981), high recovery (95.35%–110.75%), low limit of detection (0.169–0.214 ng L⁻¹), and precision (intraday RSD = 4.13%–5.44%, interday RSD = 3.28%–4.91%). It was successfully applied to analyze targets in commercially available orange juices, detecting residues within 4.37–36.07 µg L⁻¹. This study's methodological development offers significant guidance for efficient detection of organophosphorus pesticides in food products, potentially facilitating the advancement and application of simpler and more efficient analytical techniques.\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 1","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-12-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142909827","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

Development and Validation of a Stability-Indicating High-Performance Liquid Chromatography Method Coupled With a Diode Array Detector for Quantifying Haloperidol in Oral Solution Using the Analytical Quality-by-Design Approach 稳定性指示高效液相色谱耦合二极管阵列检测器定量口服液中氟哌啶醇方法的建立与验证

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2024-12-30 DOI: 10.1002/jssc.70067

Allan Michael Junkert, Naomi Gerzvolf Mieres, Karime Zeraik Abdalla Domingues, Luana Mota Ferreira, Roberto Pontarolo

{"title":"Development and Validation of a Stability-Indicating High-Performance Liquid Chromatography Method Coupled With a Diode Array Detector for Quantifying Haloperidol in Oral Solution Using the Analytical Quality-by-Design Approach","authors":"Allan Michael Junkert, Naomi Gerzvolf Mieres, Karime Zeraik Abdalla Domingues, Luana Mota Ferreira, Roberto Pontarolo","doi":"10.1002/jssc.70067","DOIUrl":"10.1002/jssc.70067","url":null,"abstract":"<div>\u0000 \u0000 This study developed a stability-indicating HPLC-DAD method for quantifying haloperidol in oral solution using analytical quality-by-design principles. Haloperidol stability was tested under acidic, alkaline, oxidative, and photolytic stress conditions. The analytical quality-by-design approach began by defining the analytical target profile and identifying critical material attributes and critical method parameters via risk analysis. Factorial and Box–Behnken designs, conducted in Design Expert 13, were used to select critical method parameters and determine the method operable design region. The oral solution degraded significantly under acidic and alkaline conditions. Continuous critical method parameters such as mobile phase flow rate, gradient slope, column temperature, and pH were optimized. A quadratic Box–Behnken design with critical method attributes was applied and validated, resulting in robust regression models with significant p-values (> 0.05), absence of lack-of-fit (p-values < 0.05), and R2-adjusted > 0.85. The method proved selective, accurate, and precise within the method operable design range. Normal operating conditions (NOCs) were established using a Waters Symmetry C18 column with a 100-mM formate buffer (pH 3.8) and acetonitrile, with a gradient profile and detection at 246 nm. The operational region included flow rates between 1.2 and 1.35 mL/min (NOC = 1.3 mL/min), temperatures of 8°C–20°C (NOC = 15°C), and mobile phase pH variations from 3.3 to 4.3 (NOC = 3.8). The analytical quality-by-design–based method was robust and effective for stability monitoring, reducing subjectivity while maximizing reliability.\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 1","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-12-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142909864","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

Identification and Characterization of Chemical Compounds in Compound Shougong Powder by UHPLC-Q-TOF/MSE Combined With Multiple Data Processing Techniques UHPLC-Q-TOF/MSE结合多种数据处理技术鉴定复方寿公粉中的化合物

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2024-12-30 DOI: 10.1002/jssc.70069

Rui Yang, Xiaojie Fu, Lanying Li, Ziqi Wei, An Zhou, Huan Wu

{"title":"Identification and Characterization of Chemical Compounds in Compound Shougong Powder by UHPLC-Q-TOF/MSE Combined With Multiple Data Processing Techniques","authors":"Rui Yang, Xiaojie Fu, Lanying Li, Ziqi Wei, An Zhou, Huan Wu","doi":"10.1002/jssc.70069","DOIUrl":"10.1002/jssc.70069","url":null,"abstract":"<div>\u0000 \u0000 Compound Shougong Powder (CSP) is a traditional Chinese medicine (TCM) preparation recognized for its efficacy in reducing swelling and relieving pain. It is primarily used clinically for the treatment of malignant tumors. However, research on the chemical compounds present in CSP remains limited. In this study, we employed ultra-high-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF/MSE) combined with multiple data processing techniques to comprehensively characterize the chemical compounds in CSP. This included a multiple-point screening mass defect filtering (MDF), an enhanced method based on conventional MDF and boundary theory that creates a polygonal filtering zone by connecting numerous endpoints (n ≥ 5) to filter target components. Additional techniques utilized were extracted ion chromatogram (EIC), neutral loss filtering (NLF), diagnostic fragment ion filtering (DFIF), and direct identification methods considering retention time, fragmentation behavior, and reference standards. First, UHPLC-Q-TOF/MSE was applied for comprehensive profiling of CSP's chemical compounds. Then, R language combined with MZmine was used for data preprocessing, enabling the construction of an ion information list to extract valid data. Eventually, through these multiple data processing techniques, a total of 116 chemical compounds in CSP were identified, including 34 flavonoids, 38 saponins, seven stilbenes, six anthraquinones, 12 organic acids, 13 terpenoids, and six others. In summary, this study elucidates the chemical composition of CSP, contributing to the discovery of potential active ingredients for CSP. Additionally, the established strategy provided a powerful guide for the chemical characterization of TCM.\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 1","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-12-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142909829","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

An Imaged Capillary Isoelectric Focusing Separation of the Linear and Cyclic Variants of a Mimotope of the Cancer-Related CD20 Antigen–Validation and Statistical Evaluation 肿瘤相关CD20抗原的线性和循环变异的毛细等电聚焦成像-验证和统计评估。

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2024-12-30 DOI: 10.1002/jssc.70054

Georg Bloderer, Luigi Grassi, Chiara Cabrele, Hanno Stutz

{"title":"An Imaged Capillary Isoelectric Focusing Separation of the Linear and Cyclic Variants of a Mimotope of the Cancer-Related CD20 Antigen–Validation and Statistical Evaluation","authors":"Georg Bloderer, Luigi Grassi, Chiara Cabrele, Hanno Stutz","doi":"10.1002/jssc.70054","DOIUrl":"10.1002/jssc.70054","url":null,"abstract":"Imaged capillary isoelectric focusing was successfully applied for separating an in-house synthesized closely related peptide pair, that is, a linear 12-mer (Rp5-L) and its cyclic 15-mer variant (Rp5-C). Rp5-L represents a mimotope, that is, an epitope mimicking peptide, of the CD20 antigen, which is over-expressed in B-cell-related tumors. Peptide identity—including the successful disulfide bond formation in Rp5-C—was confirmed with matrix-assisted laser desorption ionization-time of flight mass spectrometry. The purity of synthesized products was determined by a reversed-phase high-performance liquid chromatographic method with ultraviolet detection. The apparent isoelectric point (pI) of cyclic Rp5-C and Rp5-L was 5.99 and 6.47, respectively. An appropriate combination of carrier ampholytes allowed for their baseline separation with an analysis time of <20 min. Method validation was done for the synthesized peptides and three flanking pI markers covering, for example, repeatability and intermediate precision. Calibrations on different days resulted in identical slopes for Rp5-L and Rp5-C, respectively, as statistically confirmed by Welch's t-test and pooled t-test over 8 days. The calibration data of mimotopes and pI markers were evaluated for outliers, normality, homoscedasticity, and autocorrelation with complementary statistical procedures, which identified an otherwise unnoticed outlier for a pI marker. The linearity of calibration for Rp5-L, Rp5-C, and the pI markers was tested with Mandel's fitting test and lack-of-fit test. For Rp5-L and Rp5-C, the calculated limits of detection and limits of quantification were ≤0.31 and ≤0.96 µmol/L, respectively.","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 1","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-12-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11685353/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142909860","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

Column Screening and Development of HILIC and RPLC Methods Coupled to Tandem Mass Spectrometry for the Monitoring of Albumin on Cysteine 34 Exposed to Mustard Agents 柱筛选及HILIC和RPLC耦合串联质谱法监测芥菜制剂暴露的半胱氨酸34白蛋白的建立

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2024-12-30 DOI: 10.1002/jssc.70065

Lorenzo Avigo, Audrey Combès, Charlotte Desoubries, Christine Albaret, Anne Bossée, Emmanuel Joubert, Valérie Pichon

{"title":"Column Screening and Development of HILIC and RPLC Methods Coupled to Tandem Mass Spectrometry for the Monitoring of Albumin on Cysteine 34 Exposed to Mustard Agents","authors":"Lorenzo Avigo, Audrey Combès, Charlotte Desoubries, Christine Albaret, Anne Bossée, Emmanuel Joubert, Valérie Pichon","doi":"10.1002/jssc.70065","DOIUrl":"10.1002/jssc.70065","url":null,"abstract":"<div>\u0000 \u0000 Adduction on protein nucleophile sites by mustard agents can be monitored to assess detection of retrospective exposure to these agents. Cysteine 34 (Cys34) on human serum albumin was selected as the target of choice. This work targets di- and tripeptides adducted on Cys34 by sulfur mustard, sesquimustard, and nitrogen mustards separated in hydrophilic liquid chromatography (HILIC) and Reversed–Phase (RP) mode. The effect of several mobile phase additives on the mass spectrometry (MS) and MS/MS signal and on LC retention profile was studied. A mix of ammonium acetate and acetic acid offered satisfactory results in terms of MS sensitivity. Screening of HILIC columns was performed, and ZIC-HILIC stationary phase was selected for HILIC mode, and C18 stationary phase was used for RP analysis. Negative ionization mode leads to a higher S/N ratio compared to positive ionization mode. Adducted tripeptides were selected for the monitoring of mustard agents’ exposure, allowing better sensitivity than their dipeptide homologues. The two developed chromatographic methods have similar sensitivities with LOQs ranging from 1.9 to 20.5 ng/mL for the reversed-phase liquid chromatography (RPLC)–ESI–(−)–MS/MS method and from 1.7 to 43.3 ng/mL for the HILIC–ESI–(−)–MS/MS method. The monitoring method should be selected based on the targeted mustard agent, and the remaining method can be a confirmation tool.\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 1","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-12-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142909861","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

Preparation of a 1,1'-Binaphthyl-based Chiral Polyimine Macrocycle Bonded Chiral Stationary Phase by Thiol-ene Click Reaction and Its Enantioseparation Performance in High-Performance Liquid Chromatography 巯基点击反应制备1,1′-联萘基手性聚亚胺大环键合手性固定相及其在高效液相色谱中的对映分离性能

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2024-12-25 DOI: 10.1002/jssc.70064

Jia-Lei Wu, Li-Qin Yu, Hua-Can Zhang, Bang-Jin Wang, Sheng-Ming Xie, Jun-Hui Zhang, Li-Ming Yuan

{"title":"Preparation of a 1,1'-Binaphthyl-based Chiral Polyimine Macrocycle Bonded Chiral Stationary Phase by Thiol-ene Click Reaction and Its Enantioseparation Performance in High-Performance Liquid Chromatography","authors":"Jia-Lei Wu, Li-Qin Yu, Hua-Can Zhang, Bang-Jin Wang, Sheng-Ming Xie, Jun-Hui Zhang, Li-Ming Yuan","doi":"10.1002/jssc.70064","DOIUrl":"10.1002/jssc.70064","url":null,"abstract":"<div>\u0000 \u0000 Chiral macrocycles have emerged as attractive media for chromatographic enantioseparation due to their excellent host-guest recognition properties. In this study, a new chiral stationary phase (CSP) based on 1,1'-binaphthyl chiral polyimine macrocycle (CPM) was reported. The CPM was synthesized by one-step aldehyde-amine condensation of (S)-2,2'-dihydroxy-[1,1'-binaphthalene]-3,3'-dicarboxaldehyde with 1,2-phenylenediamine and bonded on thiolated silica via the thiol-ene click reaction to afford the CSP. The enantioseparation performance of the CSP was evaluated by separating different types of racemates including alcohols, esters, ketones, amides, organic acids, and ethers in both normal-phase (NP) and reversed-phase (RP) elution modes. As a result, enantioseparations of 10 and 15 racemates were achieved in the two elution modes, respectively. Meanwhile, the effects of chromatographic conditions on separation, such as mobile phase composition and injection mass, were studied in detail. Moreover, a comparison of the proposed CSP for the separation of the tested racemates with commercial Chiralcel OD-H and Chiralpak AD-H columns was also conducted, and results revealed that the proposed CSP can achieve some enantioseparations that cannot be achieved by the two commercial columns. This study indicates that the chiral macrocycle is a promising chiral selector for high-performance liquid chromatography.\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"47 24","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-12-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142895667","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

Leveraging Green Chromatography in Quality-by-Design-Driven Study for the Simultaneous Analysis of Essential Single-Pill Antidiabetic Drug Combinations 利用绿色色谱法在质量设计驱动研究中同时分析单片抗糖尿病药物组合。

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2024-12-25 DOI: 10.1002/jssc.70063

Adel Ehab Ibrahim, Samy G. Alamir, Khaled Maged, Galal Magdy, Baher I. Salman, Ahmed Al-Harrasi

{"title":"Leveraging Green Chromatography in Quality-by-Design-Driven Study for the Simultaneous Analysis of Essential Single-Pill Antidiabetic Drug Combinations","authors":"Adel Ehab Ibrahim, Samy G. Alamir, Khaled Maged, Galal Magdy, Baher I. Salman, Ahmed Al-Harrasi","doi":"10.1002/jssc.70063","DOIUrl":"10.1002/jssc.70063","url":null,"abstract":"<div>\u0000 \u0000 Micellar liquid chromatography (MLC) has proven beneficial efficiency and ecological impact for routine quality control activities. In the proposed study, cyrene was investigated for the first time, together with other green additives, as a novel safe organic solvent in reversed-phase MLC. Quality-by-design (QbD) approach screened their effect on the separation performance. Six antidiabetic drugs from different classes, namely, metformin (MTF), empagliflozin (EMP), ertugliflozin (ERT), linagliptin (LNT), sitagliptin (SIT), and gliclazide (GCZ) were utilized to assess some newly approved antidiabetic drugs and combinations. An organic solvent-free mobile phase consisting of (0.01 M Brij-35, 0.09 M sodium dodecyl sulfate, and 0.01 M ammonium acetate, pH 5.0) separated the studied drugs using an RP-C18 core–shell column. The flow rate was set at 1.2 mL/min, and analytes were detected using a photodiode array detector at 245, 270, and 225 nm. System suitability parameters demonstrated MLC capability to eliminate organic solvents without compromising separation efficiency. The method was validated across a concentration range of 2.0–30.0 µg/mL for EMP, ERT, and LNT, 20.0–120.0 µg/mL for GCZ and SIT, and 100.0–600.0 µg/mL for MTF. The method successfully determined analytes in different single and multicomponent tablets. Greenness assessment was performed using MoGAPI and AGREE metrics.\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"47 24","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-12-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142895605","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

In Situ Column Modification of Silica Monoliths With Pentafluorophenyl Ligands for the HPLC Separation of Eight Tocochromanols 五氟苯基配体原位修饰硅胶整体柱用于HPLC分离八种tocochromanol。

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2024-12-23 DOI: 10.1002/jssc.70056

Georgijs Baškirovs, Arianne Soliven, Paweł Górnaś

{"title":"In Situ Column Modification of Silica Monoliths With Pentafluorophenyl Ligands for the HPLC Separation of Eight Tocochromanols","authors":"Georgijs Baškirovs, Arianne Soliven, Paweł Górnaś","doi":"10.1002/jssc.70056","DOIUrl":"10.1002/jssc.70056","url":null,"abstract":"<div>\u0000 \u0000 Silica-based monoliths offer higher separation efficiency per unit pressure drop compared to particle-packed columns. Their application is limited by the commercial availability of different column chemistries. Pentafluorophenyl ligands enable hydrogen bonding, dipole–dipole, π–π, and hydrophobic interactions, facilitating the separation of various compounds. This study employs an in situ modification procedure, namely, the silylation reaction to bond these specific ligands to silica-based monoliths. Three chromolith silica monoliths were modified with three different PFP-moieties. The silica monolith was successfully modified in situ with 3-(pentafluorophenyl)propylmethyldichlorosilane and the separation behavior was compared to a particle-packed pentafluorophenyl column and a C18 monolith for the separation of tocochromanols (Vitamin E-related compounds). The C18 monolith failed to resolve all the tocochromanols, while the PFP particle-packed column and monolith were comparable under their optimized conditions. The PFP monoliths conditions are as follows: isocratic water-methanol (22:78, v/v) mobile phase, with a flow rate of 1.45 mL/min, at 15°C. Further chromatographic comparisons between the PFP particle-packed column to the PFP monolith included selectivity studies under isocratic conditions via the linear solvent strength model, which also showed comparable selectivity behavior. Differences in selectivity was demonstrated for a gradient separation of eight compounds to represent a relatively more complex separation. In addition, backpressure and Van Deemter comparisons were performed, and it was demonstrated that the main PFP monolith advantages were obtained near the pressure maximum of the PFP particle-packed column at 3.5 mL/min, comparable efficiencies were obtained, and the PFP monolith decreased the backpressure by one-third.\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"47 24","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-12-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142882395","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

Triphenyl-Modified Mixed-Mode Stationary Phases With and Without Embedded Ion-Exchange Sites for High-Performance Liquid Chromatography 高效液相色谱中有或没有嵌入离子交换位点的三苯基修饰混合模式固定相。

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2024-12-23 DOI: 10.1002/jssc.70058

Marc Wolter, Mirna Maalouf, Mateusz Janek, Cornelius Knappe, Markus Kramer, Michael Lämmerhofer

{"title":"Triphenyl-Modified Mixed-Mode Stationary Phases With and Without Embedded Ion-Exchange Sites for High-Performance Liquid Chromatography","authors":"Marc Wolter, Mirna Maalouf, Mateusz Janek, Cornelius Knappe, Markus Kramer, Michael Lämmerhofer","doi":"10.1002/jssc.70058","DOIUrl":"10.1002/jssc.70058","url":null,"abstract":"The present work reports on the preparation, characterization, and evaluation of a set of novel triphenyl-modified silica-based stationary phases without and with embedded ion-exchange sites for mixed-mode liquid chromatography. The three synthesized triphenyl phases differed in additionally incorporated ion-exchange sites. In one embodiment, allyltriphenylsilane was bonded to thiol-modified silica by thiol-ene click reaction, leading to particles with no ion-exchange sites. A second stationary phase was obtained by thiol-yne click reaction of thiol silica with 2-propinyl-triphenylphosphonium bromide, yielding a strong anion-exchanger (SAX). A third stationary phase was obtained from this SAX phase by the oxidation of residual thiols to sulfonic acid moieties, leading to a zwitterionic surface. All synthesized materials were subjected to elemental analysis, 13C and 29Si solid-state cross-polarization/magic angle spinning nuclear magnetic resonance (CP/MAS NMR) spectroscopy analysis, and pH-dependent ζ-potential determinations via electrophoretic light scattering. The prepared stationary phases were chromatographically evaluated under classical reversed-phase, ion-exchange, and hydrophilic interaction chromatography conditions and classified within a set of commercially available columns by principal component analysis of retention factors. Finally, the obtained stationary phases were applied for biomolecule separations (e.g., teicoplanin and siRNA patisiran). These LC tests proved the orthogonality of the three prepared stationary phases and indicated possible fields of application.","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"47 24","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-12-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11667146/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142882412","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}

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