{"title":"Enhanced Lipidomics Analysis of Breast Cancer Cells Using Three-phase Liquid Extraction and Ultra High-performance Liquid Chromatography Coupled With Quadrupole Time-of-Flight Tandem Mass Spectrometry","authors":"Binhong He, Fengying Ye, Jieqing Feng, Ting Zhou","doi":"10.1002/jssc.70014","DOIUrl":"10.1002/jssc.70014","url":null,"abstract":"<div>\u0000 \u0000 <p>Lipid extraction of complex biological samples is essential for high-quality data in liquid chromatography-mass spectrometry (LC-MS)-based lipidomics. This study introduces a three-phase liquid extraction (3PLE)-ultra-high-performance LC coupled with quadrupole time-of-flight tandem MS method. This method was successfully applied to lipidomics analysis of breast cancer cells, including highly metastatic MDA-MB-231 and slightly metastatic MCF7 cells. The 3PLE method employed an <i>n</i>-hexane/methyl tert-butyl ether/acetonitrile/water solvent system that formed one aqueous and two organic phases. Neutral and polar lipids were enriched in the upper and middle organic phases, respectively, and combined for detection, thereby reducing analysis time. Compared with the Bligh and Dyer method, 3PLE achieved higher sensitivity and detected more features, with over a 50% increase in the relative abundance of nearly 50% of the differential lipids. In total, 21 differential lipids were identified in the MDA-MB-231 group and 22 in the MCF7 group compared to normal breast epithelial cells (MCF10A). Pathway analysis suggested that lipid changes in breast cancer cells were associated with glycerophospholipid metabolism, arachidonic acid metabolism, sphingolipid metabolism, and linoleic acid metabolism. The study presents a highly efficient lipidomics method, providing a scientific foundation for understanding breast cancer pathogenesis and aiding in diagnosis.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":null,"pages":null},"PeriodicalIF":2.8,"publicationDate":"2024-11-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142568857","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":"Preparation and Application of Weak Cation Exchange Resin Based on Thiol Click Reaction","authors":"Zhongping Huang, Qingqing Zhu, Yu Han, Ying Mo, Junhao Zhang, Huijun Liu","doi":"10.1002/jssc.70012","DOIUrl":"10.1002/jssc.70012","url":null,"abstract":"<div>\u0000 \u0000 <p>Using poly(styrene-divinylbenzene) microspheres as stationary phase matrix and mercaptosuccinic acid as a modifier, a new weak cation exchange resin was synthesized by thiol click reaction. The conditions for thiol-chlorine click reaction and thiol-alkene click reaction were optimized. The surface morphology and chemical composition of the modified microspheres were characterized by scanning electron microscopy, Fourier-transform infrared spectroscopy, and an elemental analyzer. The stationary phase can achieve the separation of six common cations within 25 min. A homemade weak cation chromatographic column was used to determine the impurities of Na<sup>+</sup> and K<sup>+</sup> and the content of tetramethylammonium ions in tetramethylammonium hydroxide samples. The method showed a good linear correlation in the range of 0.1–500.0 mg/L with correlation coefficients of 0.9998–0.9999, and the limits of detection (signal-to-noise ratio ≥ 3) were 0.01–0.20 mg/L. The intra-day relative standard deviations (RSDs) were in the range of 1.1%–4.4%, and the inter-day RSDs were in the range of 0.8%–14.8%. The spiked recoveries were in the range of 91.92%–119.86%. The results showed that the prepared stationary phase exhibited effective separation ability and good reproducibility, which was suitable for the analysis of the impurities of Na<sup>+</sup>, K<sup>+</sup>, and the content of tetramethylammonium in the tetramethylammonium reagents.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":null,"pages":null},"PeriodicalIF":2.8,"publicationDate":"2024-11-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142568868","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 Determination of Galantamine in Human Plasma by Microchip Electrophoresis With a Highly Integrated Contactless Conductivity Detector","authors":"Zhilei Li, Gangyuan Lin, Xiujuan Yang","doi":"10.1002/jssc.70013","DOIUrl":"10.1002/jssc.70013","url":null,"abstract":"<div>\u0000 \u0000 <p>A novel and rapid method was developed for the determination of galantamine in human plasma by microchip electrophoresis with a highly integrated contactless conductivity detector (CCD). The instrumental parameters affecting the response of the detector, such as excitation frequency and excitation voltage, were examined and optimized. The electrophoresis conditions that influenced the separation and detection of galantamine, including the composition of buffer solution, buffer pH, buffer concentration, additives, injection time, and separation voltage were systematically investigated. Under the optimal conditions, the peak height had a good linear relationship with the concentration of galantamine in human plasma from 10 to 160 µg/L, and the correlation coefficient was 0.9992, the limit of detection reached 1.1 µg/L. The recoveries were between 98.6% and 102.1%. This sensitive, rapid, and convenient method is a good alternative to existing methods for galantamine determination. Also, this highly integrated CCD holds great promise in clinical biochemical analysis.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":null,"pages":null},"PeriodicalIF":2.8,"publicationDate":"2024-11-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142568892","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}
Miao Liu, Xiangyu Jia, Rongfei Peng, Zhijun Bai, Jun Yuan, Lei Tan
{"title":"Human Biomonitoring of Serum Polybrominated Diphenyl Ethers by Supported Liquid Extraction and Gas Chromatography Coupled With Tandem Mass Spectrometry","authors":"Miao Liu, Xiangyu Jia, Rongfei Peng, Zhijun Bai, Jun Yuan, Lei Tan","doi":"10.1002/jssc.70010","DOIUrl":"10.1002/jssc.70010","url":null,"abstract":"<div>\u0000 \u0000 <p>This study aims to develop and validate a robust analytical method for the quantification of polybrominated diphenyl ethers (PBDEs) in human serum using gas chromatography–tandem mass spectrometry. We compared procedural blanks, recoveries, and operational convenience of liquid–liquid extraction and supported liquid extraction for the determination of serum PBDEs. We evaluated different extraction solvents for their effect on PBDE recoveries. Supported liquid extraction was selected for method validation due to its operational convenience. The method demonstrated satisfactory linearity, sensitivity, and reproducibility, with the range of 0.10–5.00 µg/L for most PBDE congeners and 0.20–10.0 µg/L for PBDE-154 and PBDE-183, with limits of detection ranging from 2 to 48 ng/L, and with matrix effects ranging from 94% to 113%. Quality control assessments indicated that recoveries ranged from 85% to 110% and relative standard deviations of less than 11%. The proposed method was applied to biomonitoring of 111 healthy adults, revealing detectable levels of PBDEs in over 90% of the samples. BDE-47 and BDE-183 were the most prevalent, with mean concentrations of 4.13 and 22.1 ng/L, respectively. Detection frequencies ranged from 0.90% for BDE-17 and BDE-85 to 25.2% for BDE-47. Males had higher mean concentrations of BDE-183 than females.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":null,"pages":null},"PeriodicalIF":2.8,"publicationDate":"2024-11-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142568863","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 Dual Column pH Switchable Water Stationary Phase System for Separation Control in Supercritical Fluid Chromatography","authors":"Emmanuel A. Nai, Kevin B. Thurbide","doi":"10.1002/jssc.70008","DOIUrl":"10.1002/jssc.70008","url":null,"abstract":"<div>\u0000 \u0000 <p>A dual column system comprised of a pH switchable water stationary phase column and a conventional non-polar capillary column is introduced for use in Supercritical Fluid Chromatography (SFC). By removing or adding NH<sub>4</sub>OH to the system hydration source, the water stationary phase pH can be rapidly switched between acidic (measured at pH∼3) and basic (measured at pH∼9) in seconds, while the operating character of the conventional column is unchanged. This switch modulates the velocity of ionizable analytes about 20-fold in the system, whereas non-ionizable analytes are not affected. In this way, the retention time of acids and/or bases can be reproducibly altered (<1% RSD; n = 3) in SFC separations. As a result, analyte selectivity and resolution can be readily controlled during analyses. For example, a selectivity reversal (alpha from 0.4 to 1.6) and a resolution increase (from 0 to 13) are demonstrated. Rapid stationary phase pH switching also allows multiple acids, bases, and/or neutral analytes to be determined simultaneously. Applications demonstrate that this method can greatly simplify complex mixture analysis in SFC by helping to separate target analytes from interfering matrix components.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":null,"pages":null},"PeriodicalIF":2.8,"publicationDate":"2024-11-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142568779","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":"Ready-to-use Models Built Using a Diverse Set of 266 Aroma Compounds for the Estimation of Gas Chromatographic Retention Indices for the 50%-Cyanopropylphenyl-50%-Dimethylpolysiloxane Stationary Phase","authors":"Anastasia Yu. Sholokhova, Dmitriy D. Matyushin","doi":"10.1002/jssc.70016","DOIUrl":"10.1002/jssc.70016","url":null,"abstract":"<div>\u0000 \u0000 <p>Retention index prediction based on the molecule structure is not often used in practice due to low accuracy, the need to use paid software to calculate molecular descriptors (MD), and the narrow applicability domain of many models. In recent years, relatively accurate and versatile deep learning (DL)-based models have emerged. These models are now used in practice as an additional criterion in gas chromatography-mass spectrometry identification. The DB-225ms stationary phase (usually described as 50%-cyanopropylphenyl-50%-dimethylpolysiloxane in available sources) is widely used, but ready-to-use retention index estimation models are not available for it. This study presents such models. The models are linear and use simple constitutional MD and retention indices predicted by DL for the DB-WAX and DB-624 stationary phases as MD (we show that it is their use that allows us to achieve satisfactory accuracy). The accuracy obtained for a completely unseen hold-out test set: root mean square error 73.2; mean absolute error 45.7; median absolute error 22.0. The models were trained using a retention data set of 266 volatile compounds. All calculations can be performed using the convenient open-source software CHERESHNYA. The final equations are implemented as a spreadsheet and a code snippet and are available online: https://doi.org/10.6084/m9.figshare.26800789.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":null,"pages":null},"PeriodicalIF":2.8,"publicationDate":"2024-11-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142568897","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":"Supercritical Fluid Chromatography in Bioanalysis–A Review","authors":"Laura Toribio, María Teresa Martín, José Bernal","doi":"10.1002/jssc.70003","DOIUrl":"10.1002/jssc.70003","url":null,"abstract":"<p>In the last decade, the instrumentation improvements in supercritical fluid chromatography (SFC) and the hyphenation to mass spectrometry (MS), have increased the SFC acceptance between scientists, becoming today a valuable tool in analytical chemistry. The unique selectivity, short analysis times, low consumption of organic solvents, and the greener mobile phase, have contributed to expanding its applicability which has led to an increase in the number of publications especially in the bioanalysis area. This work reviews the advantages and main applications of SFC in bioanalysis during the last 5 years. Fundamental aspects concerning mobile phase composition, stationary phase, hyphenation to MS as well as matrix effect have been discussed. Finally, the most relevant applications have been summarized.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":null,"pages":null},"PeriodicalIF":2.8,"publicationDate":"2024-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70003","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142564266","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}
Jiaqi Liang, Yuchi Zhang, Chunming Liu, Sainan Li, Ruizhe Li, Yutong Zhang, Ming Chen, Ruijun Sun
{"title":"High-Speed Countercurrent Chromatography Isolation of Active Components from Evodia Rutaecarpa and Affinity Ultrafiltration Screening for Their Acetylcholinesterase Inhibitor Activity","authors":"Jiaqi Liang, Yuchi Zhang, Chunming Liu, Sainan Li, Ruizhe Li, Yutong Zhang, Ming Chen, Ruijun Sun","doi":"10.1002/jssc.70002","DOIUrl":"10.1002/jssc.70002","url":null,"abstract":"<div>\u0000 \u0000 <p>Acetylcholinesterase inhibitors from <i>Evodia rutaecarpa</i> were screened, prepared, and evaluated. To screen the lipophilic alkaloid active constituents in <i>E. rutaecarpa</i>, we improved and optimized an ultrafiltration system. Three acetylcholinesterase (AChE) inhibitors, dehydroevodiamine, evodiamine, and rutecarpine, were screened. Addressing the limitations of the traditional response surface methodology (RSM) for multiobjective screening, we integrated RSM with the Non-dominated Sorting Genetic Algorithm III to achieve the optimal extraction of these active ingredients. High-speed countercurrent chromatography was used to isolate the active components using a two-phase solvent system: <i>n-</i>hexane/ethyl acetate/methanol/water (3.0:2.5:3.5:2.0, v/v/v/v) and ethyl acetate/methanol/water (3.0:1.0:4.0, v/v/v). The nuclear magnetic resonance spectroscopy confirmed the structures of the compounds, and molecular docking and dynamics simulations assessed the inhibitory effects of the chemical components on AChE, which were consistent with the findings of the ultrafiltration experiments. We also confirmed the neuroprotective properties of these compounds against glutamate-induced apoptosis in PC12 cells. Overall, we achieved the systematic optimization of multitarget compound extraction and lipophilic alkaloid ultrafiltration screening, as well as preparation and activity validation, laying the groundwork for the development of AChE inhibitors from lipophilic alkaloids.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":null,"pages":null},"PeriodicalIF":2.8,"publicationDate":"2024-10-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142502752","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}
Mansoor Ahmad, Amir Badshah, Hongji Li, Muhammad Asad, Mohamed A. Ibrahim, Essam A. Ali, Abdelaaty A. Shahat, Umar Nishan, Mansoor Khan, Wei Sun
{"title":"Vortex-Assisted Magnetic Solid-Phase Extraction of Heavy Metals in Water and Food Samples Using Iron Oxide Nanoparticle-Impregnated Carboxymethyl-β-Cyclodextrin","authors":"Mansoor Ahmad, Amir Badshah, Hongji Li, Muhammad Asad, Mohamed A. Ibrahim, Essam A. Ali, Abdelaaty A. Shahat, Umar Nishan, Mansoor Khan, Wei Sun","doi":"10.1002/jssc.70004","DOIUrl":"10.1002/jssc.70004","url":null,"abstract":"<div>\u0000 \u0000 <p>The excessive accumulation of heavy metals has adverse effects on the human body. Here, magnetic iron oxide-impregnated carboxymethyl-β-cyclodextrin was synthesized. The synthesized material was employed as a magnetic solid-phase extracting adsorbent for specific heavy metals like lead (Pb), nickel (Ni), copper (Cu), and cobalt (Co). Characterization was performed by X-ray diffraction, energy dispersive X-ray spectroscopy, scanning electron microscopy, Brunauer–Emmett–Teller, and Fourier-transform infrared spectroscopy. The analytical merits, like detection limits (Pb: 1.38 ng/mL, Ni: 0.5 ng/mL, Co: 0.14 ng/mL, and Cu: 0.55 ng/mL) and quantification limits (Pb: 4.14 ng/mL, Ni: 1.62 ng/mL, Co: 1.85 ng/mL, and Cu: 1.82 ng/mL) were calculated. Similarly, the preconcentration and enhancement factors (15) and relative standard deviation (Pb: 3.5, Ni: 0.92, Co: 2.7, and Cu: 1.5) were also calculated. The interfering study shows that the method is highly selective. For validation, it was applied to certified reference materials such as the Institute of Nuclear Chemistry and Technology ornamental Basma tobacco leaves and trace metal double addition 63.4 environmental water with good percent recovery values (92%–99%). Real water and food samples were also used with satisfactory (90%–99%) recovery results.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":null,"pages":null},"PeriodicalIF":2.8,"publicationDate":"2024-10-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142502754","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}
Denis V. Ovchinnikov, Sergey A. Vakhrameev, Ilya S. Voronov, Marina P. Semushina, Nikolay V. Ul'yanovskii, Dmitry S. Kosyakov
{"title":"Determination of Macrolides in Water Using Solid-Phase Extraction and Supercritical Fluid Chromatography-Tandem Mass Spectrometry","authors":"Denis V. Ovchinnikov, Sergey A. Vakhrameev, Ilya S. Voronov, Marina P. Semushina, Nikolay V. Ul'yanovskii, Dmitry S. Kosyakov","doi":"10.1002/jssc.70000","DOIUrl":"10.1002/jssc.70000","url":null,"abstract":"<div>\u0000 \u0000 <p>Macrolides are a group of compounds used to treat bacterial infections in humans and animals. Their widespread use results in the contamination of the water environment, which, on the one hand, has a detrimental effect on aquatic organisms and, on the other hand, can lead to the emergence of resistant strains of microorganisms. All of the above determines the need for monitoring of these compounds in the environment, particularly, in water objects. Usually, the high-performance liquid chromatography combined with tandem mass spectrometry method is used to solve this problem, however, this work shows the possibility of using the supercritical fluid chromatography-tandem mass spectrometry method. An approach for the determination of four common macrolides, namely erythromycin, clarithromycin, midecamycin, and josamycin, was developed. The use of solid-phase extraction allowed to achieve limits of quantification at 0.57–6.8 ng/L. The presented approach was validated and tested on a real object—a sample of municipal wastewater.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":null,"pages":null},"PeriodicalIF":2.8,"publicationDate":"2024-10-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142502751","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}