Journal of separation science最新文献

{"title":"From Columns to Clouds: Emerging Interfaces and Ion Sources for Coupling Analytical Separations With Mass Spectrometry.","authors":"Chamarthi Maheswar Raju, Pawel L Urban","doi":"10.1002/jssc.70411","DOIUrl":"https://doi.org/10.1002/jssc.70411","url":null,"abstract":"<p><p>Although mass spectrometry (MS) is a powerful analytical technique, it is vulnerable to matrix interference, and it does not distinguish ions with the same m/z (isobaric interference). Therefore, for the past few decades, numerous efforts have been made to enable coupling separation systems with MS. Apart from a set of mainstream hyphenation approaches (such as those using inductively coupled plasma ionization, electron ionization, and electrospray ionization), a number of less conventional ways to couple separation systems with MS have been devised. Extraordinary methods for coupling gas chromatography, liquid chromatography, capillary electrophoresis, thin-layer chromatography, supercritical fluid chromatography, and other unconventional interfaces and ion sources have been disclosed in the literature. Some of these techniques extend the analyte coverage of traditional hyphenated techniques by enabling the detection of less polar compounds. Others speed up analysis or decrease the cost. Another notable trend is the implementation of the so-called ambient ionization techniques for coupling separations with MS.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 5","pages":"e70411"},"PeriodicalIF":2.8,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147816710","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":"Semi-Quantitative Determination of Volatile Organic Compounds Detected in Air Using Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry.","authors":"Nurbi Karimkyzy, Bauyrzhan Bukenov, Nadezhda V Bakaikina, Tolkyn Kurmanbayeva, Balgyn Dyussenkulova, Bulat Kenessov","doi":"10.1002/jssc.70426","DOIUrl":"https://doi.org/10.1002/jssc.70426","url":null,"abstract":"<p><p>Nontargeted air analysis using methods based on gas chromatography (GC) and mass spectrometry (MS) is very important for the discovery of new potentially dangerous volatile organic compounds (VOCs). Solid-phase microextraction (SPME) is one of the simplest and cost-efficient sampling techniques for screening VOCs in air, but the extraction effectiveness of detected compounds can substantially vary depending on their properties and affinity to the fiber coating. This study was aimed at the development of a novel method for semi-quantitative determination of VOCs identified in air samples using SPME and GC-MS. Extraction effectiveness was estimated from fiber coating-air distribution constants predicted using linear solvation energy relationship and numerical modeling with COMSOL Multiphysics. MS detector response factors were estimated using multiple regression obtained from experimental responses of 111 VOCs and SVOCs, their molecular weights, octanol-water partitioning coefficients, polar surface areas, and fractional ion abundances of base ions. Numerical modeling using COMSOL Multiphysics improved the accuracy for less volatile analytes with greater molecular weight, particularly at lower extraction times. For 12 of 14 tested analytes, recoveries from spiked nitrogen samples were in the range between 39% and 275%. The developed method was successfully applied for determining approximate concentrations of VOCs identified in samples of air, and for determination of approximate time-weighted average concentrations of VOCs. It can be recommended for the quick estimation of approximate concentrations of VOCs detected during nontargeted analysis when calibration standards are not available or when high accuracy is not needed.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 5","pages":"e70426"},"PeriodicalIF":2.8,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147839497","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":"Multistep Plunger Injection Assisted Micellar-to-Solvent Stacking for the Determination of Alkaloids From Medicinal Plants Using Capillary Zone Electrophoresis.","authors":"Kai-Yang Fan, Qi-Zhong Jin, Shi-Qi Niu, Jun Cao, Li-Hong Ye","doi":"10.1002/jssc.70427","DOIUrl":"https://doi.org/10.1002/jssc.70427","url":null,"abstract":"<p><p>A simple, rapid, and efficient multistep plunger injection-assisted micellar to solvent stacking method was developed for the determination of cationic analytes from medicinal plants. In this method, a three-step sequential injection protocol was used, where sodium dodecyl sulfate (SDS), sample, and methanol (MeOH) solutions were introduced in succession to achieve an effective enrichment. The background solution contained 30 mM sodium dihydrogen phosphate and 30 mM citric acid. To achieve optimal enrichment efficiency, we systematically optimized several key parameters: surfactant type, SDS concentration, sodium dihydrogen phosphate concentration in the sample matrix, MeOH concentration, SDS injection time, MeOH injection time, and sample injection time. The optimal stacking conditions were as follows: injection of 10 mM SDS for 30 s, injection of the sample solution for 60 s, and injection of 40% MeOH for 10 s. This method exhibited an excellent linear relationship, as evidenced by the correlation coefficients (R²) ranging from 0.994 to 0.999. The intra-day and inter-day precision of this method was less than 3.701%, and the recovery rates of the analytes ranged from 92.70% to 107.79%, indicating satisfactory accuracy and reliability. Compared with conventional injection techniques, the sensitivity enrichment factors of the four analytes ranged from 42 to 44. The proposed method was validated for its applicability in detecting four alkaloids (fumarine, allocryptopine, tetrahydropalmatine, and corydaline) in Rhizoma corydalis samples.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 5","pages":"e70427"},"PeriodicalIF":2.8,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147839513","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":"Homochiral Metal-organic Framework (+)-diacetyl-L-tartaric-NH-MIL-101(Fe) as Stationary Phase for Enantioseparation in Capillary Electrochromatography.","authors":"Jiatong Yu, Jin Guan, Ke Long, Xinyu Chen, Shuang Shi, Xindong Jiang","doi":"10.1002/jssc.70440","DOIUrl":"https://doi.org/10.1002/jssc.70440","url":null,"abstract":"<p><p>A novel enantioselective open-tubular capillary electrochromatography (CEC) column was fabricated by noncovalently immobilizing (+)-diacetyl-L-tartaric anhydride functionalized NH₂-MIL-101(Fe) onto the capillary inner wall using polydopamine as an adhesive layer. The coating of the modified capillary was comprehensively characterized through Fourier-transform infrared spectroscopy, powder X-ray diffraction, Brunauer-Emmett-Teller analysis, scanning electron microscopy, energy dispersive X-ray spectroscopy, circular dichroism, and electroosmotic flow measurements. The column's chiral separation ability was assessed by analyzing seven model compounds, comprising four proton pump inhibitors (omeprazole, pantoprazole, lansoprazole, and tenatoprazole) and three fluoroquinolones (ofloxacin, sparfloxacin, and gatifloxacin). Under optimized conditions, baseline resolution (9.68-14.56) of all enantiomers was achieved within 7 min. The column demonstrated excellent reproducibility, with inter-day, intra-day, and column-to-column relative standard deviations ranging from 1.22% to 4.98%. Additionally, molecular docking simulations were conducted using AutoDock Tools to investigate interactions between the stationary phase and analyte enantiomers, with computational results corroborating experimental CEC data.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 5","pages":"e70440"},"PeriodicalIF":2.8,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147839489","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":"A Monoclonal Antibody-based Lateral Flow Immunochromatographic Assay for Rapid Detection of Derrisisoflavone A in Derris scandens (Roxb.) Benth.","authors":"Pitragorn Srimongkon, Worapol Sae-Foo, Gorawit Yusakul, Waraporn Putalun","doi":"10.1002/jssc.70428","DOIUrl":"https://doi.org/10.1002/jssc.70428","url":null,"abstract":"<p><p>Derrisisoflavone A is a prenylated isoflavonoid and a chemical marker in the stem of Derris scandens (Roxb.) Benth., it is a suitable chemical marker for this plant. Conventional analytical techniques, such as high-performance liquid chromatography, liquid chromatography-mass spectrometry, and immunoassays, offer high sensitivity but rely on complex analytical equipment and specialized expertise, thereby limiting their applicability for rapid on-site analysis. In this study, a lateral flow immunochromatographic assay (LFIA) employing gold nanoparticle (AuNP)-labeled monoclonal antibodies (mAbs) was developed for qualitative detection of derrisisoflavone A in D. scandens plant materials and herbal products. The LFIA was designed in a competitive format using AuNPs-mAbs conjugates as the detection probe, derrisisoflavone A-cationized ovalbumin conjugates applied on the test zone, and anti-mouse immunoglobulin G antibody on the control zone. Under optimized conditions, the assay was evaluated for sensitivity and specificity and validated by comparison with a well-established indirect competitive enzyme-linked immunosorbent assay (icELISA) using various D. scandens plant parts, commercial products, and representative Fabaceae species. The LFIA exhibited a visual limit of detection of 100 µg/mL, defined by complete inhibition of the test zone signal, and demonstrated high analytical specificity with undetectable cross-reactivity toward structurally related isoflavonoids or prenylated flavonoids. The analytical results showed good agreement with those obtained by icELISA. Although less sensitive than quantitative methods, the developed LFIA provides a rapid, simple, and reliable screening tool for on-site quality control and preliminary assessment of derrisisoflavone A in D. scandens and related products.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 5","pages":"e70428"},"PeriodicalIF":2.8,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147816524","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":"Hydrophobic Menthol-Based Deep Eutectic Solvent for Ultrasound-Assisted Dispersive Liquid‒Liquid Microextraction of Amide Herbicides in Food and Environmental Samples Before Determination by HPLC.","authors":"Menghong Xie, Guxi Huang, Hao Wang, Jiazhen Wei, Junliang Lin, Yipeng Huang, Guihua Ruan","doi":"10.1002/jssc.70433","DOIUrl":"https://doi.org/10.1002/jssc.70433","url":null,"abstract":"<p><p>Toxic amide herbicide residues pose significant risks to food safety and environmental health. In this study, an ultrasound-assisted dispersive liquid‒liquid extraction method utilizing a hydrophobic menthol-based deep eutectic solvent (DES) was developed for the efficient separation and determination of four amide herbicides in complex matrices, including vegetables, soil, and water. DES composed of decanoic acid (hydrogen bond acceptor) and menthol (hydrogen bond donor) at a molar ratio of 2:3 demonstrated superior extraction performance compared to those using lauric or oleic acid as a hydrogen bond acceptor. The extraction was equilibrated within 2 min under neutral pH conditions. Molecular docking simulations revealed that the N─H groups in the amide moieties served as the primary active sites for hydrogen bonding interactions with the DES. By integrating this green extraction technique with high-performance liquid chromatography, a robust analytical method was established, exhibiting excellent linearity (R² > 0.9991) over a wide range (1-200 ng mL^-1), with low limits of detection (0.3-0.5 ng mL^-1) and high precision (intraday RSDs ≤ 3.6%, inter-day RSDs ≤ 8.2%). The method achieved high recoveries (89.8%-116%) across various samples. Greenness assessments using the GAREEprep and Analytical Ecological Scale showed scores of 0.57 and 85, respectively, underscoring the sustainability of the method. This study presents a rapid, sensitive, and sustainable alternative for monitoring amide herbicide residues, contributing to food safety and environmental protection.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 5","pages":"e70433"},"PeriodicalIF":2.8,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147839508","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":"Development and Validation of a Sensitive UHPLC-MS/MS Method for the Simultaneous Determination of 19 Bile Acids in Liver and Feces: Application to Metabolic Dysfunction-Associated Steatotic Liver Disease Mice.","authors":"Meng Xiao, Wenwen Zhao, Yinying Ba, Miao Xia, Kui Luo, Longtai You, Xiao Li, Ke Zan, Xiaoqing Chen","doi":"10.1002/jssc.70430","DOIUrl":"https://doi.org/10.1002/jssc.70430","url":null,"abstract":"<p><p>Recently, bile acids (BAs) have garnered significant attention due to their crucial roles in various metabolic diseases. However, the simultaneous quantification of BAs in biological samples is challenging due to the structural similarities, complex biological matrix, and tissue-specific distribution. We developed a sensitive UHPLC-MS/MS method for quantitation of 19 BAs in mouse liver (mainly conjugated BAs) and feces (mainly unconjugated BAs). We compared protein precipitation, liquid-liquid extraction, and solid-phase extraction (SPE) methods for sample preparation, and SPE was chosen due to the low background noise and high extraction efficiency for both conjugated and unconjugated BAs. The method was extensively validated by evaluating the linearity (R² ≥ 0.991), extraction recovery (82%-112%), limits of detection (1-2 ng/mL) and low limits of quantification (2-5 ng/mL). Then, the method was applied to the detection of BAs in liver and feces of metabolic dysfunction-associated steatotic liver disease mice, and the correlations between BA levels and the mRNA expression levels of BA metabolic enzymes, transporters, and receptors were analyzed. This study provides a direct and reliable determination method for the in-depth investigation of the enterohepatic circulation of BAs.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 5","pages":"e70430"},"PeriodicalIF":2.8,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147816707","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":"Replacing Ecologically Risky Trifluoroacetic Acid and Acetonitrile With Methanesulfonic Acid and Dimethyl Carbonate in High-Performance Liquid Chromatography Analyses of Small Molecule Drugs.","authors":"Franziska Pögel Neé Steinicke, Taha B El-Jourani, Jana Haegner, Matthias Schiedel, Hermann Wätzig","doi":"10.1002/jssc.70425","DOIUrl":"10.1002/jssc.70425","url":null,"abstract":"<p><p>It has long been recognised that, in the long term, hazardous acetonitrile (ACN) as a mobile-phase component and the environmentally critical trifluoroacetic acid (TFA) as an ion-pairing reagent should be replaced in high-performance liquid chromatography (HPLC). Nevertheless, methods relying on precisely these reagents are still widely used. Herein, we show that alternative approaches for the analysis of small molecule drugs are readily applicable, using examples from pharmaceutical quality control and medicinal chemistry. First, the principles of green analytical chemistry were implemented in an alternative HPLC method for the theophylline monohydrate monograph of the European Pharmacopoeia, without altering the core methodology. Among the various conditions tested, the use of 2% dimethyl carbonate (DMC) provided equivalent separation and an even slightly improved resolution compared with the original ACN-based pharmacopoeial method. In a second approach, we present a highly sustainable gradient HPLC method for routine purity analysis of synthesis products by replacing TFA with safe, biodegradable, and environmentally benign methanesulfonic acid (MSA). Furthermore, in the case of this gradient method, ACN could be replaced by the biodegradable and environmentally friendly DMC. An eluent composition consisting of 42 parts DMC, 23 parts EtOH, 35 parts H₂O and 0.1 parts MSA was found to be equivalent to ACN containing 0.1% TFA. By employing a reproducible protocol using EtOH as a co-solvent, we were able to overcome current challenges associated with the use of organic carbonates in HPLC, which primarily arise from their limited miscibility with water. Given the continued widespread use of gradient HPLC methods employing ACN as an eluent and TFA as an acidic modifier, the methods presented herein offer significant potential to advance the implementation of sustainability in pharmaceutical quality control and medicinal chemistry.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 5","pages":"e70425"},"PeriodicalIF":2.8,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13146114/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147839483","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":"Sample Preparation and Separation of Lignans by Liquid Chromatography.","authors":"Miikka Paloluoto, Susanne K Wiedmer","doi":"10.1002/jssc.70432","DOIUrl":"10.1002/jssc.70432","url":null,"abstract":"<p><p>Lignans are important phytochemicals found mostly in the resins of coniferous trees, but are also introduced into human diets through foods such as sesame seeds and extra-virgin olive oil. They are pharmacologically interesting mainly because of their antioxidant activities, and they have also been shown to have cytotoxic and antimicrobial effects. Lignans are typically analyzed using liquid chromatography, although the complexity of the common matrices from which lignans are studied requires extensive sample preparation methodologies beforehand. While the simplest samples, such as wines and olive oils, can be analyzed without complicated procedures, most samples will require purification through liquid‒liquid extraction or silica gel column chromatography. Lignans are most often detected using mass spectrometry or ultraviolet‒visible spectrophotometry, but other methods, such as fluorescence and coulometric electrode array detectors, have also been proven useful. In this review, we will describe the typical characteristics of lignans with focus on their main pharmaceutical benefits, as well as typical sample preparation methodologies and liquid chromatographic analyses.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 5","pages":"e70432"},"PeriodicalIF":2.8,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13146148/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147839479","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":"Design of Experiments-assisted Micellar Electrokinetic Chromatography Separation of Phosphodiesterase-5 Inhibitors: Application to Sildenafil and Tadalafil.","authors":"Cristina Niculaș, Gabriel Hancu, Zoltán István Szabó, Anca Gabriela Cârje, Valentin Ion, Daniela Lucia Muntean","doi":"10.1002/jssc.70429","DOIUrl":"https://doi.org/10.1002/jssc.70429","url":null,"abstract":"<p><p>A micellar electrokinetic chromatography method was developed for the simultaneous separation of the phosphodiesterase-5 inhibitors sildenafil and tadalafil, two therapeutic agents used in the treatment of erectile dysfunction that are frequently identified as illicit adulterants in dietary supplements marketed for sexual enhancement. Method development was supported by a design of experiments strategy. An initial fractional factorial screening design was used to evaluate the influence of selected experimental parameters on resolution (R_s) and migration time. Pareto analysis of standardized effects indicated that cyclodextrin (CD) concentration, methanol (MeOH) content, and separation voltage significantly affected the separation, whereas pH, sodium dodecyl sulfate (SDS) concentration, and temperature did not show a statistically significant impact within the studied range. Based on the screening results, a Box-Behnken response surface design was employed to optimize the significant factors. Optimized separation conditions consisted of a 50 mM phosphate buffer (pH 2.5) containing 50 mM SDS, 10% MeOH, and 5 mM hydroxypropyl-β-CD, with a separation voltage of -20 kV and a capillary temperature of 20°C. Under these conditions, baseline separation was achieved with a R_s of 4.75 and migration times below 6 min. The method was validated in terms of precision, linearity, accuracy, and robustness, showing satisfactory analytical performance. Application to pharmaceutical formulations and dietary supplement samples confirmed the suitability of the proposed method for routine screening and quality control purposes.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"49 5","pages":"e70429"},"PeriodicalIF":2.8,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147816554","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}