{"title":"Determination of Hydrogen Cyanide by Gas Chromatography With Post-Column Reaction and Flame Ionization Detection","authors":"Ronda Gras, Jim Luong, 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}
Xuechen Si, Huilin Li, Jiarong Yang, Yunping Zhu, Xueli Cao
{"title":"Effective Separation of Granaticins From Streptomyces Vilmorinianum YP1 Using High-Speed Countercurrent Chromatography and Their Characteristic Evaluation","authors":"Xuechen Si, Huilin Li, Jiarong Yang, Yunping Zhu, 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}
Eduardo Carasek, Amanda Vitória Santos, Francielle Crocetta Turazzi, Lucas Morés, Luciane Effting, Guilherme Mariz de Oliveira Barra
{"title":"Recent Trends in the Development of Green Analytical Sample Preparation Methods Using Advanced Materials","authors":"Eduardo Carasek, Amanda Vitória Santos, Francielle Crocetta Turazzi, Lucas Morés, Luciane Effting, 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}
Jingwen Hu, Haihua Zhang, Zonghao Zhang, Xueru Fan, Ting Li, Li Tong, Fang Yang
{"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, Haihua Zhang, Zonghao Zhang, Xueru Fan, Ting Li, Li Tong, 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 >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}
Magdalini Vladitsi, Natasa P. Kalogiouri, Petros Mourouzis, Abuzar Kabir, Kenneth Furton, Victoria F. Samanidou
{"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, Natasa P. Kalogiouri, Petros Mourouzis, Abuzar Kabir, Kenneth Furton, 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}
Hechen Liu, Chongzhi Wang, Na Li, Baokun Tang, Tao Zhu
{"title":"Study on Adsorption of Two Functionalized Conjugated Microporous Polymers: Extraction of Carbendazim and Thiabendazole in Ophiopogon japonicus","authors":"Hechen Liu, Chongzhi Wang, Na Li, Baokun Tang, 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, Jiahui Wang, Lulu Yu, Miao Xu, Siyue Chen, Yajie Dou, Guangzhi Cui, Yuming Wang, Yanyan Xu, 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 MS<sup>2</sup> 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, 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><sup>2</sup> > 0.999), the RSD for the precision was < 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}
Greta Compagnin, Chiara De Luca, Chiara Nosengo, Giorgia Greco, Martina Catani, Alberto Cavazzini, Yannick Krauke, Simona Felletti
{"title":"Continuous Depletion of Tetrahydrocannabinol From Cannabis Extract Through Simulated Moving Bed Chromatography Using Green Mobile Phase","authors":"Greta Compagnin, Chiara De Luca, Chiara Nosengo, Giorgia Greco, Martina Catani, Alberto Cavazzini, Yannick Krauke, Simona Felletti","doi":"10.1002/jssc.70175","DOIUrl":"https://doi.org/10.1002/jssc.70175","url":null,"abstract":"<p>The interest toward greener and more sustainable chemical processes is constantly growing, especially in chemical industries, where there is an urgent need to reduce the waste on one hand, and to replace not environmentally friendly organic solvents, on the other.</p><p>One of the current challenges in industrial processes is the depletion of the psychoactive cannabinoid tetrahydrocannabinol (THC) from hemp extracts. Indeed, current legislations impose that THC in hemp products must meet defined concentration limits or, in some cases, it must be completely removed. In the present study, the continuous depletion of THC has been performed through simulated moving bed chromatography operated with a fully green mobile phase, made of water and ethanol. This process permits to overcome the limits and drawbacks of available purification methods, based on toxic solvents and traditional single column chromatography.</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.70175","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144108719","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}
Tao Bao, Jiao Long, Jina Wang, Meng Sun, Xinglong Zheng, Sicen Wang
{"title":"Materials Institute Lavoisier-68(Al)-coated Frosted Glass Rods for Enhanced Detection of Tetracyclines in Food Samples by Suspended Bar Sorptive Extraction","authors":"Tao Bao, Jiao Long, Jina Wang, Meng Sun, Xinglong Zheng, Sicen Wang","doi":"10.1002/jssc.70141","DOIUrl":"https://doi.org/10.1002/jssc.70141","url":null,"abstract":"<div>\u0000 \u0000 <p>Herein, we present a sensitive analytical method utilizing Materials Institute Lavoisier (MIL)-68(Al)-coated frosted glass rods (MIL-68(Al)@FGR) coupled with ultra-high-performance liquid chromatography for detecting trace tetracycline (TC) antibiotics in food matrices. The synthesized coating was thoroughly characterized through field-emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, X-ray diffraction, and Fourier-transform infrared spectroscopy analyses. Systematic optimization of critical parameters, including extraction time, sample pH, formic acid concentration, and desorption time achieved optimal extraction efficiency. The developed method exhibited a wide linear range (3–70 ng/mL) with low detection limits (0.1–0.3 ng/mL) for target analytes. Practical application to spiked food samples demonstrated satisfactory recoveries of 75.2%–115.1% across milk, chicken, and egg matrices, accompanied by precise relative standard deviations of ≤8.4%. The MIL-68(Al)@FGR-based approach shows exceptional resistance to matrix interference and detection sensitivity, establishing an effective strategy for monitoring TC residues in complex food samples.</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":"144108720","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}