Journal of separation science最新文献

{"title":"Performance of the Reverse Fill/Flush Flow Modulation With Tunable Auxiliary Forward-Pressure Control in the Conditions When the Second Gas Chromatography Column Outlet Pressure Is Different From the Atmospheric Pressure","authors":"Aleksandra Lelevic","doi":"10.1002/jssc.70182","DOIUrl":"https://doi.org/10.1002/jssc.70182","url":null,"abstract":"<div>\u0000 \u0000 <p>Reverse fill/flush flow modulation is an effective approach for peak modulation in comprehensive two-dimensional gas chromatography, and several homemade or commercial solutions have been demonstrated. In terms of configuration, systems with either a fixed bleed capillary or tunable forward or back pressure regulation permit to effectively maintain an optimal modulator channel flow and good modulation performance. In both cases, however, in the up-to-date reported works, the modulator channel flow regulation conditions remain constant during the GC run. In this work it was shown that if the objective is to maintain a constant modulator channel flow, constant pressure–resistance regulation conditions can be an issue when the secondary gas chromatography column outlet pressure is not equal to the outlet pressure of the bleed capillary. When the secondary column outlet is connected to a detector, such as, for example, VUV, or to a purged splitter where an elevated constant pressure is applied, which were both tested in this study, in these cases the temperature changes during the GC run impose having to vary the chosen pressure resistance conditions for maintaining a constant modulator channel flow. It was shown, however, that modulator channel flow variation during the GC run appeared minimal when a fixed bleed capillary was used but increased significantly if a tunable auxiliary flow of carrier gas was rather employed. In addition, it was demonstrated through theoretical calculations and experiments that the temperature dependence of the auxiliary carrier gas flow necessary for maintaining a certain constant modulator channel flow is not linear but rather closer to a second-degree polynomial. While a linear approximation can be sufficient in some cases, in other cases the modulation performance can be impacted more significantly, and thus auxiliary carrier gas flow programming according to a second-degree polynomial model can be preferred.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 6","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-06-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144197050","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":"Purification of Pharmaceuticals via Retention Time Prediction: Leveraging Graph Isomorphism Networks, Limited Data, and Transfer Learning","authors":"Armen G. Beck,&nbsp;Rojan Shrestha,&nbsp;Jun Wang,&nbsp;Jonathan Fine,&nbsp;Erik L. Regalado,&nbsp;Kanaka Hettiarachchi,&nbsp;Katharine B. Williams,&nbsp;Edward C. Sherer,&nbsp;Pankaj Aggarwal","doi":"10.1002/jssc.70178","DOIUrl":"https://doi.org/10.1002/jssc.70178","url":null,"abstract":"<div>\u0000 \u0000 <p>The design-make-test cycle for drug discovery is highly dependent on the purification of synthesized compounds. Prior to evaluation of suitability, ultrahigh-performance liquid chromatography is used for an initial standard analysis, where retention times of analytes are measured with a shorter standard gradient method and used to select the appropriate gradients for a final purification method. To circumvent this preliminary screening experiment for small molecule libraries, retention time prediction had been achieved previously by the use of commercial modeling methods. However, these retention time prediction models can have limited applicability when built from smaller datasets and are less effective when constructed from disparate data collected under differing chromatography conditions. Having thousands of measured retention times from high-throughput physiochemical screening, we sought to leverage these data for the construction of predictive models for a standard preliminary method enabling high-throughput purification of macrocyclic peptide libraries. Utilizing 4549 analytes and their retention times from high-throughput physiochemical screening, a structure-to-retention-time model was built using a graph isomorphism network, a form of artificial neural network architecture. Once fitted to high-throughput screening data, the model was re-trained with standard gradient method data, a technique known as transfer learning. Through transfer learning, a training set of 80 analytes yielded a neural network model that, when evaluated against a test set of 24 analytes, displays high performance metrics with a coefficient of determination (<i>R</i>²) of 0.82 and mean average error of 0.088 min, or 1.26% of the gradient time. Comparatively, the best commercial quantitative structure-retention relationship model poorly performed, with an <i>R</i>² of 0.11 and mean average error of 0.202 min. This model has been deployed internally as a Dash app to help democratize the use of the developed models and is being used for selecting purification methods based on analyte structure.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 6","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-06-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144197058","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":"Determination of Hydrogen Cyanide by Gas Chromatography With Post-Column Reaction and Flame Ionization Detection","authors":"Ronda Gras,&nbsp;Jim Luong,&nbsp;Robert A. Shellie","doi":"10.1002/jssc.70176","DOIUrl":"https://doi.org/10.1002/jssc.70176","url":null,"abstract":"<div>\u0000 \u0000 <p>A straightforward and practical 15-min gas chromatographic method utilizing flame ionization detection has been developed to measure hydrogen cyanide in various matrices. This new approach features a catalyzed two-stage post-column reaction that significantly enhances the detection and quantification of hydrogen cyanide. Selecting the right separation column is crucial for accurate analysis. Initial tests with porous layer open tubular columns resulted in significant peak tailing, rendering them unsuitable for trace-level analysis. Modified polyethylene glycol stationary phases also exhibited strong peak tailing in addition to producing artifact peaks. In contrast, a polydimethylsiloxane-based column with a very low phase ratio (<i>β</i> = 10) demonstrated excellent analytical performance, including peak symmetry and inertness. The analytical approach achieved a minimum detection limit of 50 parts per billion (ppb, v/v) without preconcentration and a linear range from 0.05 to 200 parts per million (ppm, v/v). At a concentration level of 20 ppm (v/v), the RSD at the 95% confidence level was less than 1% (<i>n</i> = 10), and at a concentration level of 1 ppm (v/v), the RSD at the 95% confidence level was less than 3% (<i>n</i> = 10) under the established conditions. The method's effectiveness has been validated through real-life applications, including analyzing hydrogen cyanide in fruit seeds and the headspace of untreated water samples.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144140470","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":"Effective Separation of Granaticins From Streptomyces Vilmorinianum YP1 Using High-Speed Countercurrent Chromatography and Their Characteristic Evaluation","authors":"Xuechen Si,&nbsp;Huilin Li,&nbsp;Jiarong Yang,&nbsp;Yunping Zhu,&nbsp;Xueli Cao","doi":"10.1002/jssc.70184","DOIUrl":"https://doi.org/10.1002/jssc.70184","url":null,"abstract":"<div>\u0000 \u0000 <p>Granaticins and their derivatives are a series of benzoisochromanequinones (BIQs) compounds with remarkable biological activities, but their practical applications have been restricted due to the low separation efficiency of traditional methods. In this work, a high-speed countercurrent chromatography (HSCCC) method was developed for the first time to separate granaticins from the fermentation broth of <i>Streptomyces vilmorinianum</i> YP1. Considering the similar structures, polarities, and dissociation constants of granaticins, an appropriate solvent system for their complete separation by HSCCC was determined. This system consisted of <i>n</i>-hexane: ethyl acetate: methanol: water in volume ratios of 2: 5: 3: 4 and 1: 4: 1: 4. Five granaticins with high purity were obtained: a granaticin analogue (29.5 mg); granaticin acid (111.3 mg; purity: 99.2%), MM44785 (49.4 mg; purity: 99.1%), granaticin (0.8 mg; purity: 98.7 %), and granaticin B (73.3 mg; purity: 99.4%) from 2.7 g of crude granaticins extract. The antibacterial activity and stability characteristics of the two main compounds were further evaluated. Granaticin B exhibited excellent antibacterial effects on Gram-positive bacteria, while granaticin acid showed better thermal stability. This is the first time to develop a general separation strategy for granaticins that are potentially applicable in industry production.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144140525","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":"Recent Trends in the Development of Green Analytical Sample Preparation Methods Using Advanced Materials","authors":"Eduardo Carasek,&nbsp;Amanda Vitória Santos,&nbsp;Francielle Crocetta Turazzi,&nbsp;Lucas Morés,&nbsp;Luciane Effting,&nbsp;Guilherme Mariz de Oliveira Barra","doi":"10.1002/jssc.70177","DOIUrl":"https://doi.org/10.1002/jssc.70177","url":null,"abstract":"<p>Recent concern about the impact of environmental preservation and the health of living beings has opened new avenues for scientific research. In this context, contemporary analytical chemistry has been marked by the development of green analytical methodologies, which aim to reduce the use of toxic reagents and minimize the environmental impact of analytical processes. Progress in this area involves the optimization of sample preparation techniques and the use of new functional materials, which contribute to a more sustainable and efficient analysis. Among these methodologies, miniaturized sample preparation techniques stand out, as they use smaller volumes of solvents and offer high sensitivity and selectivity. The use of advanced materials, such as molecularly imprinted polymers, MOFs, and conductive polymers, has driven innovation in analytical procedures regarding complex matrices, including environmental, food, and biological samples. These materials offer high selectivity and stability, improving efficiency in the extraction and detection of specific analytes. This review explores the integration of sustainable and green methodologies. It critically highlights applications and evaluates them using the Analytical Greenness Metric for Sample Preparation, based on publications from the past 6 years.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70177","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144140475","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":"Innovative Off-line Two-dimensional Supercritical Fluid Chromatography, Separation, and Purification of Structurally Similar Polyphenols From Gentiana szechenyii Using Propyl Urea and Phenyl/Tetrazole Stationary Phases","authors":"Jingwen Hu,&nbsp;Haihua Zhang,&nbsp;Zonghao Zhang,&nbsp;Xueru Fan,&nbsp;Ting Li,&nbsp;Li Tong,&nbsp;Fang Yang","doi":"10.1002/jssc.70180","DOIUrl":"https://doi.org/10.1002/jssc.70180","url":null,"abstract":"<div>\u0000 \u0000 <p>Although traditional Tibetan medicine is a valuable source for the discovery of novel lead compounds, the isolation of structural analogs from natural sources remains a challenge in the field of separation science. The Tibetan medicine <i>Gentiana szechenyii</i> (GC) is widely to treat various types of inflammation and upper respiratory tract infections. Despite its strong medicinal value, a complex purification process has limited investigations into its chemical composition. Therefore, in this study, a novel off-line two-dimensional supercritical fluid chromatographic (2D-SFC) method was developed and successfully applied to the efficient separation and purification of complex compounds and structural analogs from GS. Initially, the crude GS sample was pretreated using a binary medium-pressure liquid chromatography system to obtain the target fraction (Fr16, 1.0 g). A novel propyl urea and phenyl/tetrazole stationary phases off-line 2D-SFC system was then developed and applied for the separation and purification of Fr16. Consequently, five polyphenolic compounds were successfully isolated with purities of &gt;95%. The obtained results demonstrate the potential of off-line 2D-SFC for maximizing the discovery of novel structural analogs and isomers, thereby providing a theoretical basis for the further exploitation of natural products.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144140526","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 of a Capsule Phase Microextraction Protocol for the Determination of Monomers Released from Dental Resins in Cola Drinks Analyzed by High-Pressure Liquid Chromatography Coupled to UV","authors":"Magdalini Vladitsi,&nbsp;Natasa P. Kalogiouri,&nbsp;Petros Mourouzis,&nbsp;Abuzar Kabir,&nbsp;Kenneth Furton,&nbsp;Victoria F. Samanidou","doi":"10.1002/jssc.70183","DOIUrl":"https://doi.org/10.1002/jssc.70183","url":null,"abstract":"<p>A novel, simple capsule phase microextraction combined with high-pressure liquid chromatography coupled with ultraviolet detection analytical method was developed for the simultaneous determination of organic monomers that can be released from dental resins [bisphenol-A (BPA), bisphenol A glycerolatedimethacrylate (Bis-GMA), triethylene glycol dimethacrylate (TEGDMA), and urethane dimethacrylate (UDMA)] in cola drinks. The critical parameters that affect the extraction, such as the selection of the capsule type and size, extraction time, type, and volume of elution solvent, stirring rate during the extraction, and desorption time, were optimized. The method was subsequently validated in terms of selectivity, linearity, accuracy, precision, and robustness and showed satisfactory results. The limits of detection and quantitation were equal to 0.06 and 0.2 ng/µL, respectively, and the recoveries ranged between 93.3% and 106.9%. The method was employed in the determination of monomers released from cola drinks. For this purpose, cola refreshments were incubated with dental resins for 24 h and 7 days, and the proposed method was successfully used for monitoring the release in cola samples.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70183","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144140476","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":"Study on Adsorption of Two Functionalized Conjugated Microporous Polymers: Extraction of Carbendazim and Thiabendazole in Ophiopogon japonicus","authors":"Hechen Liu,&nbsp;Chongzhi Wang,&nbsp;Na Li,&nbsp;Baokun Tang,&nbsp;Tao Zhu","doi":"10.1002/jssc.70185","DOIUrl":"https://doi.org/10.1002/jssc.70185","url":null,"abstract":"<div>\u0000 \u0000 <p>In this study, two novel conjugated microporous polymers modified with functional groups were synthesized. Meanwhile, static and dynamic adsorption tests were conducted on the obtained materials. To achieve the best extraction efficiency, the parameters of the pipette-tip solid-phase extraction procedure were optimized, including the amount of adsorbent, the type and amount of washing solvent, and the elution solvent. The results demonstrate that the adsorption performance of the sulfonated conjugated microporous polymer is remarkably superior to that of the aminated conjugated microporous polymer. Under the optimal conditions, the linear range for targets was 0.05–10.00 µg/g using this method, the limits of detection were 0.009 µg/g for carbendazim and 0.004 µg/g for thiabendazole, and the recoveries were in the range of 80.7%–108.3% for carbendazim and 87.4%–119.2% for thiabendazole, which was successfully applied to the analysis of target residues in actual samples. In addition, the adsorption capacity of material prepared in this study was superior to that of several commercially available adsorbents. Therefore, a method for the determination of target residues in <i>Ophiopogon japonicus</i> by pipette-tip solid-phase extraction coupled with high-performance liquid chromatography using the material adsorbent was established. This method is important for detecting target residues.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144140467","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":"Rapid Identification of Chemical Constituents in Qubai Babuqi Tablets by Ultra-High-Performance Liquid Chromatography Quadrupole-Orbitrap-Mass Spectrometry","authors":"Xuebin Qin,&nbsp;Jiahui Wang,&nbsp;Lulu Yu,&nbsp;Miao Xu,&nbsp;Siyue Chen,&nbsp;Yajie Dou,&nbsp;Guangzhi Cui,&nbsp;Yuming Wang,&nbsp;Yanyan Xu,&nbsp;Yubo Li","doi":"10.1002/jssc.70117","DOIUrl":"https://doi.org/10.1002/jssc.70117","url":null,"abstract":"<div>\u0000 \u0000 <p>Qubai Babuqi Tablets (QBBBQT) is a traditional Chinese medicine compound preparation. It is mainly used in treating vitiligo, with the effect of activating pulse-beat and regulating blood condition. However, the chemical composition of QBBBQT has not been reported, and it was difficult to determine its active and toxic components. In this study, a simple and efficient method was established to characterize the chemical constituents of the alcohol extract of QBBBQT. Which used ultra-high-performance liquid chromatography quadrupole-orbitrap-mass spectrometry to match experimental MS² with characteristic ions and neutral losses for rapid analysis and identification of its chemical composition. Finally, a total of 106 chemical components were identified, including 47 flavonoids, 13 coumarins, 21 organic acids, 11 diarylheptanes, four saccharides, and 10 others. This method can be used for the systematic and rapid analysis of the chemical components in QBBBQT, which is of great significance for the study of its pharmacodynamic material basis and quality control.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144108721","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":"Simultaneous Determination of 10 Fat-Soluble Vitamins by Ultra-Performance Liquid Chromatography in Multivitamins With Minerals Capsules","authors":"Salika Jeelani,&nbsp;Zarema Kassymbek","doi":"10.1002/jssc.70167","DOIUrl":"https://doi.org/10.1002/jssc.70167","url":null,"abstract":"<p>A novel and accurate ultra-high performance liquid chromatography (UHPLC) method combined with UV detector was developed for the simultaneous determination of 10 fat-soluble vitamins (retinyl acetate, retinyl palmitate, beta carotene, alpha tocopherol, alpha tocopheryl acetate, alpha tocopheryl acid succinate, ergocalciferol, cholecalciferol, phytonadione, and menaquinone-7) in multivitamin with mineral capsules. The chromatographic separation was achieved on a Waters XBridge Sheild C18 (100 × 2.1 mm, 1.7 µm) column. The mobile phase comprised of 0.1% formic acid (v/v) in water and 0.1% formic acid in acetonitrile (v/v) delivered in a gradient mode. An enhanced and simple sample preparation procedure involving enzyme digestion of the gel coating of the capsules and ultra-sonication was developed compared to the complex and time-consuming saponification methods. The method was validated to fulfill International Conference on Harmonization (ICH) requirements and included specificity, linearity, accuracy, precision, and robustness. The linearity of the method was excellent (<i>R</i>² &gt; 0.999), the RSD for the precision was &lt; 5% and the recovery of the vitamins was in the range of 99.2%–101.9%, demonstrating that the method is suitable for analysis of fate-soluble vitamins in multivitamin capsules. The developed method could be incorporated into the USP-NF Multivitamin with minerals capsules monograph.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70167","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144108722","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}