Journal of separation science最新文献_第5页

Rapid Screening of 25 Environmental Hormones in Aquatic Products Using QuEChERS-Combined With Dispersive Liquid–Liquid Microextraction Based on Solidification of Floating Organic Droplet Coupled With UHPLC-Q/Orbitrap HRMS 基于悬浮有机液滴固化- UHPLC-Q/Orbitrap HRMS联合quechers -分散液-液微萃取快速筛选水产品中25种环境激素

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2025-07-08 DOI: 10.1002/jssc.70206

Jiwang Tang, Yong Xiao, Hongqing Zhao, Can Li, Xiong Hu, Wenbin He

{"title":"Rapid Screening of 25 Environmental Hormones in Aquatic Products Using QuEChERS-Combined With Dispersive Liquid–Liquid Microextraction Based on Solidification of Floating Organic Droplet Coupled With UHPLC-Q/Orbitrap HRMS","authors":"Jiwang Tang, Yong Xiao, Hongqing Zhao, Can Li, Xiong Hu, Wenbin He","doi":"10.1002/jssc.70206","DOIUrl":"https://doi.org/10.1002/jssc.70206","url":null,"abstract":"<div>\u0000 \u0000 <p>An innovative analytical method integrating QuEChERS with dispersive liquid–liquid microextraction using solidified floating organic droplets (DLLME-SFO) and ultra-high-performance liquid chromatography-quadrupole/orbitrap high-resolution mass spectrometry (UHPLC-Q/Orbitrap HRMS) was developed for the rapid screening of 25 environmental hormones (EHs) in aquatic products. The method systematically optimized key parameters, including extraction solvent selection (1-undecanol), water volume (5 mL), pH (native pH 6.5), adsorbent combination (C18/PSA, 20 mg each), and salt addition (0% NaCl), achieving high sensitivity with detection limits of 0.1–0.4 µg/kg and recoveries of 68.2%–112.8%. The method demonstrated excellent linearity (<i>R</i><sup>2</sup> > 0.995) across a concentration range of 0.4–40 µg/kg, with precision (intra- and inter-day RSDs < 15%) and manageable matrix effects (−19.5% to 10.9%). The environmental impact assessment, conducted using the Analytical GREEnness Metric for Sample Preparation (AGREEprep score: 0.59) and Blue Applicability Grade Index (BAGI score: 80), confirmed that the proposed method satisfies both sustainability and practicality criteria for EHs analysis. Enhanced matrix purification and dual-polarity HRMS detection enabled accurate identification and quantification of structurally diverse EHs, including pesticides and pharmaceuticals. Validated in 60 commercial samples, the method detected prometryn residues in 11.7% of cases, demonstrating its practicality for monitoring EH contamination in complex aquatic matrices. This approach represents a significant advancement in multi-residue analysis, combining efficiency, sensitivity, and environmental compatibility.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144582362","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Progress in Dried Microsampling for MS-Based Protein Analysis 质谱法蛋白质分析的干燥微采样研究进展

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2025-07-08 DOI: 10.1002/jssc.70222

Trine Grønhaug Halvorsen, Léon Reubsaet

{"title":"Progress in Dried Microsampling for MS-Based Protein Analysis","authors":"Trine Grønhaug Halvorsen, Léon Reubsaet","doi":"10.1002/jssc.70222","DOIUrl":"https://doi.org/10.1002/jssc.70222","url":null,"abstract":"<div>\u0000 \u0000 <p>The current review provides an overview of the recent progress (2020–January 2025) in dried microsampling for mass spectrometry (MS) based protein analysis. A systematic search was performed to find the literature. Most of the applications are clinical, primarily focusing on targeted biomarker determination. This includes several multiplex methods, allowing simultaneous biomarker evaluation, offering significant advantages over traditional assays. Microsampling is also described in non-targeted proteomics screenings, aiming to discover new biomarkers across different application areas including disease diagnostics and lifestyle monitoring. Especially for the latter, the noninvasive nature is convenient as it enables more frequent sampling. The review discusses the use of microsampling in analysis of samples from animals, the quality of dried microsamples, as well as alternative sampling matrices and sampling materials. Although microsampling is more widely used, challenges such as long response time and tedious sample preparation remain, prompting innovations in the field. One example of this is smart sampling, where enzymatic or antibody functionalities are integrated directly on sampling media, simplifying sample preparation and enhancing analytical precision. As technology advances, dried microsampling in MS based protein analysis is expected to become increasingly important in clinical and research settings. Future innovations are anticipated to expand the utility and extend the adoption of dried microsamples in MS-based protein analyses.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144582062","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Lightweight Spherical Cellulose Aerogels With High Zr-MOF Loadings for the Facile Extraction of Benzodiazepines From Human Urine and Hair Samples 高Zr-MOF负载的轻质球形纤维素气凝胶用于从人尿和头发样品中快速提取苯二氮卓类药物

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2025-07-07 DOI: 10.1002/jssc.70221

Suling Zhang, Hengli Liu, Xiaoyang Li, Weixuan Yao, Jianbo Ying, Ting Lü, Dong Zhang, Hongting Zhao, Ying Pan

{"title":"Lightweight Spherical Cellulose Aerogels With High Zr-MOF Loadings for the Facile Extraction of Benzodiazepines From Human Urine and Hair Samples","authors":"Suling Zhang, Hengli Liu, Xiaoyang Li, Weixuan Yao, Jianbo Ying, Ting Lü, Dong Zhang, Hongting Zhao, Ying Pan","doi":"10.1002/jssc.70221","DOIUrl":"https://doi.org/10.1002/jssc.70221","url":null,"abstract":"<div>\u0000 \u0000 <p>A facile dispersive micro-solid phase extraction (D-μ-SPE) method that uses spherical cellulose aerogels is proposed herein for the trace detection of seven benzodiazepines in biological samples. Zirconium metal–organic framework (MOF) particles were dispersed in the cellulose aerogels to improve the extraction efficiency. The prepared lightweight spherical aerogels (diameter of approximately 2 mm) were easily collected from the solution using a disposable dropper, overcoming the difficult recycling of powdered MOFs. The effect of the MOF loading (39, 56, and 66 wt%) and the organic ligand (terephthalic acid, 2-aminoterephthalic acid, and 4,4′-biphenyldicarboxylic acid) in the Zr-MOF on the extraction ability of the hybrid aerogels towards benzodiazepines was studied. The hybrid aerogel with a UiO-67 loading of 66% showed the best extraction performance primarily because of the enhanced surface area, pore volume, and π–π stacking interactions. Moreover, the UiO-67/cellulose aerogel spheres were mechanically stable and showed reusability for at least eight consecutive extraction cycles. The main factors affecting extraction, such as solution pH, extraction time, type and volume of desorption solvent, and desorption time, were also examined. Under the optimal conditions, the limits of detection ranged from 0.01 to 0.03 µg/L, and the limits of quantification ranged from 0.02 to 0.10 µg/L. The recoveries were 81.8%–104.2% for urine samples and 81.5%–99.5% for hair samples. The results suggest that the spherical aerogel-based D-μ-SPE is a simple and effective method for the quantification of benzodiazepines in biological samples.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144573539","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

A Supercritical Fluid Chromatographic Method for the Determination and Separation of Boronic Acids 超临界流体色谱法测定和分离硼酸

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2025-07-07 DOI: 10.1002/jssc.70210

Upputuri Harikrishna, Punniyavel Jeyavel Pandiyan, Kaveesha Srinivas Suryakoppa, Ramesh Appadurai, Vivek Hamse Kameshwar, Shwetha Hosahalli Nanjundappa, Nandeesh Kebbahalli Nagalingaiah

{"title":"A Supercritical Fluid Chromatographic Method for the Determination and Separation of Boronic Acids","authors":"Upputuri Harikrishna, Punniyavel Jeyavel Pandiyan, Kaveesha Srinivas Suryakoppa, Ramesh Appadurai, Vivek Hamse Kameshwar, Shwetha Hosahalli Nanjundappa, Nandeesh Kebbahalli Nagalingaiah","doi":"10.1002/jssc.70210","DOIUrl":"https://doi.org/10.1002/jssc.70210","url":null,"abstract":"<div>\u0000 \u0000 <p>A green and high-throughput chromatography method was developed for the separation and quantification of boronic acids using an environmentally friendly supercritical fluid chromatography (SFC). The developed method was successfully applied for the separation of a mixture of five boronic acid compounds having different functional groups and also used for the quantification of over 15 wide ranges of boronic acid and boronic ester compounds. Expanding this method, reaction monitoring studies were performed to analyze the boronic acids present in the organic reaction mixtures obtained from the Suzuki coupling reaction, Arylation of amine, and Arylation of phenol reactions. The mobile phase used for this analysis was supercritical carbon dioxide modified by 8%–40% of methanol, which contained 20 mM aqueous ammonia (25%) as an additive, and the stationary phase used was 2-ethylpyridine-bonded silica. Overall runtime of the optimized method was 7 min with back pressure of 100 bar at a column temperature of 40°C. An extensive study was performed to optimize the various method parameters, such as columns, mobile phase modifier, additives, back pressure, and temperature. The validated SFC method was found to give a relative standard deviation of interday and intraday peak average area precision of each compound (A–E). The precision of the analytical method was evaluated based on the %RSD of the peak areas for each compound under both intraday and interday conditions. Despite slight variations, all intraday %RSD values were well within the acceptable range of analytical precision (<2%). The LOD and LOQ were in the range from 0.02 to 20 µg/mL and from 0.2 to 100 µg/mL respectively, for the five boronic acids compounds studied.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144573536","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Lightweight Spherical Cellulose Aerogels With High Zr-MOF Loadings for the Facile Extraction of Benzodiazepines From Human Urine and Hair Samples 高Zr-MOF负载的轻质球形纤维素气凝胶用于从人尿和头发样品中快速提取苯二氮卓类药物

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2025-07-07 DOI: 10.1002/jssc.70221

Suling Zhang, Hengli Liu, Xiaoyang Li, Weixuan Yao, Jianbo Ying, Ting Lü, Dong Zhang, Hongting Zhao, Ying Pan

{"title":"Lightweight Spherical Cellulose Aerogels With High Zr-MOF Loadings for the Facile Extraction of Benzodiazepines From Human Urine and Hair Samples","authors":"Suling Zhang, Hengli Liu, Xiaoyang Li, Weixuan Yao, Jianbo Ying, Ting Lü, Dong Zhang, Hongting Zhao, Ying Pan","doi":"10.1002/jssc.70221","DOIUrl":"https://doi.org/10.1002/jssc.70221","url":null,"abstract":"<div>\u0000 \u0000 <p>A facile dispersive micro-solid phase extraction (D-μ-SPE) method that uses spherical cellulose aerogels is proposed herein for the trace detection of seven benzodiazepines in biological samples. Zirconium metal–organic framework (MOF) particles were dispersed in the cellulose aerogels to improve the extraction efficiency. The prepared lightweight spherical aerogels (diameter of approximately 2 mm) were easily collected from the solution using a disposable dropper, overcoming the difficult recycling of powdered MOFs. The effect of the MOF loading (39, 56, and 66 wt%) and the organic ligand (terephthalic acid, 2-aminoterephthalic acid, and 4,4′-biphenyldicarboxylic acid) in the Zr-MOF on the extraction ability of the hybrid aerogels towards benzodiazepines was studied. The hybrid aerogel with a UiO-67 loading of 66% showed the best extraction performance primarily because of the enhanced surface area, pore volume, and π–π stacking interactions. Moreover, the UiO-67/cellulose aerogel spheres were mechanically stable and showed reusability for at least eight consecutive extraction cycles. The main factors affecting extraction, such as solution pH, extraction time, type and volume of desorption solvent, and desorption time, were also examined. Under the optimal conditions, the limits of detection ranged from 0.01 to 0.03 µg/L, and the limits of quantification ranged from 0.02 to 0.10 µg/L. The recoveries were 81.8%–104.2% for urine samples and 81.5%–99.5% for hair samples. The results suggest that the spherical aerogel-based D-μ-SPE is a simple and effective method for the quantification of benzodiazepines in biological samples.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144573537","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

A Supercritical Fluid Chromatographic Method for the Determination and Separation of Boronic Acids 超临界流体色谱法测定和分离硼酸

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2025-07-07 DOI: 10.1002/jssc.70210

Upputuri Harikrishna, Punniyavel Jeyavel Pandiyan, Kaveesha Srinivas Suryakoppa, Ramesh Appadurai, Vivek Hamse Kameshwar, Shwetha Hosahalli Nanjundappa, Nandeesh Kebbahalli Nagalingaiah

{"title":"A Supercritical Fluid Chromatographic Method for the Determination and Separation of Boronic Acids","authors":"Upputuri Harikrishna, Punniyavel Jeyavel Pandiyan, Kaveesha Srinivas Suryakoppa, Ramesh Appadurai, Vivek Hamse Kameshwar, Shwetha Hosahalli Nanjundappa, Nandeesh Kebbahalli Nagalingaiah","doi":"10.1002/jssc.70210","DOIUrl":"https://doi.org/10.1002/jssc.70210","url":null,"abstract":"<div>\u0000 \u0000 <p>A green and high-throughput chromatography method was developed for the separation and quantification of boronic acids using an environmentally friendly supercritical fluid chromatography (SFC). The developed method was successfully applied for the separation of a mixture of five boronic acid compounds having different functional groups and also used for the quantification of over 15 wide ranges of boronic acid and boronic ester compounds. Expanding this method, reaction monitoring studies were performed to analyze the boronic acids present in the organic reaction mixtures obtained from the Suzuki coupling reaction, Arylation of amine, and Arylation of phenol reactions. The mobile phase used for this analysis was supercritical carbon dioxide modified by 8%–40% of methanol, which contained 20 mM aqueous ammonia (25%) as an additive, and the stationary phase used was 2-ethylpyridine-bonded silica. Overall runtime of the optimized method was 7 min with back pressure of 100 bar at a column temperature of 40°C. An extensive study was performed to optimize the various method parameters, such as columns, mobile phase modifier, additives, back pressure, and temperature. The validated SFC method was found to give a relative standard deviation of interday and intraday peak average area precision of each compound (A–E). The precision of the analytical method was evaluated based on the %RSD of the peak areas for each compound under both intraday and interday conditions. Despite slight variations, all intraday %RSD values were well within the acceptable range of analytical precision (<2%). The LOD and LOQ were in the range from 0.02 to 20 µg/mL and from 0.2 to 100 µg/mL respectively, for the five boronic acids compounds studied.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144573538","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

The Quality Control Markers Study of Artificial Tiger Bone Powder Based on Peptidomic by NanoLC-HRMS and UHPLC-QQQ-MS 基于肽组学的人工虎骨粉质量控制标记的纳米高效液相色谱-质谱联用和高效液相色谱-质谱联用研究

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2025-07-04 DOI: 10.1002/jssc.70208

Shaowei Hu, Jing Xu, Liying Tang, Fangbo Zhang, Ye Zhao, Jing Li, Hongwei Wu, Rui Zhai, Hongjun Yang

{"title":"The Quality Control Markers Study of Artificial Tiger Bone Powder Based on Peptidomic by NanoLC-HRMS and UHPLC-QQQ-MS","authors":"Shaowei Hu, Jing Xu, Liying Tang, Fangbo Zhang, Ye Zhao, Jing Li, Hongwei Wu, Rui Zhai, Hongjun Yang","doi":"10.1002/jssc.70208","DOIUrl":"https://doi.org/10.1002/jssc.70208","url":null,"abstract":"<div>\u0000 \u0000 <p>Artificial tiger bone powder (ATBP) is an animal-derived traditional Chinese medicine for treating osteoporosis. The combination of NanoLC-HRMS and UHPLC-QQQ-MS was used to identify and quantify the quality control markers of ATBP. Peptidomics by NanoLC-HRMS was used to characterize the native peptides in ATBP and four individual bone extracts. Five signature peptides from the deer bone extracts were identified in ATBP and validated by comparison with synthetic peptides. These signature peptides were used as quality marker peptides to establish an analytical method using UHPLC-QQQ-MS, which was found to have good specificity, stability, and accuracy. The bioactivity of peptides was determined using in vitro osteoblast proliferation and anti-inflammatory assays. GPQGIAGQRGVV and AFAQLSELH could promote the proliferation and mineralization of MC3T3E1 cells. VDVVGAEALGR and FAVEGPKLVA exhibited anti-inflammatory effects in lipopolysaccharide-treated RAW 264.7 cells. This strategy for screening signature peptides in ATBP exhibits significant translational potential and can be systematically applied to the identification and characterization of quality marker peptides in various animal-derived pharmaceuticals.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144558226","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Screening and Identification of Anti-Gout Components From Herb Pair Combining Ultrafiltration-HPLC-MS, On-Line HPLC-2,2′-Azinobis(3-Ethylbenzothiazoline-6-Sulfonic Acid)-MS and In Silico Analysis: Case Study by Smilacis Glabrae Rhizoma–Dioscoreae Spongiosae Rhizoma 超滤-高效液相色谱-质谱联用、在线高效液相色谱-2,2′-偶氮唑（3-乙基苯并噻唑-6-磺酸）-质谱联用和硅质谱联用筛选鉴定中药对抗痛风成分：以山参-山药为例

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2025-07-04 DOI: 10.1002/jssc.70209

Simeng Hu, Huanying Guo, Ran Miao, Jinqian Yu, Xiao Wang, Hengqiang Zhao

{"title":"Screening and Identification of Anti-Gout Components From Herb Pair Combining Ultrafiltration-HPLC-MS, On-Line HPLC-2,2′-Azinobis(3-Ethylbenzothiazoline-6-Sulfonic Acid)-MS and In Silico Analysis: Case Study by Smilacis Glabrae Rhizoma–Dioscoreae Spongiosae Rhizoma","authors":"Simeng Hu, Huanying Guo, Ran Miao, Jinqian Yu, Xiao Wang, Hengqiang Zhao","doi":"10.1002/jssc.70209","DOIUrl":"https://doi.org/10.1002/jssc.70209","url":null,"abstract":"<div>\u0000 \u0000 <p><i>Smilacis Glabrae Rhizoma–Dioscoreae Spongiosae Rhizoma</i> (SGR-DSR), a herb pair used in traditional Chinese medicine (TCM), has definite curative effect on the clinical treatment of gout. To screen and identify the anti-gout ingredients from SGR-DSR. In this study, an integration strategy combining ultrafiltration-high performance liquid chromatography-mass spectrometry (UF-HPLC-MS) and on-line HPLC-2,2′-azinobis(3-ethylbenzothiazoline-6-sulfonic acid) diammonium salt (ABTS)-MS were proposed and applied for the rapid screening and identification of anti-gout components (xanthine oxidase [XOD] inhibitors and free radical scavengers) from SGR-DSR. As a result, 35 compounds with both potential XOD inhibitor activity and free radical scavenging activity were screened from the herbal pair. Among them, 18 active components were verified by in vitro activity assays. Astilbin showed better XOD inhibition activity and ABTS<sup>•+</sup> scavenging ability with the inhibition rates of 73.76% and 81.56% at 80 µM, respectively. In addition, the molecular docking simulation calculation results showed that all the 18 components had good binding ability with XOD. This study indicated that herb pair with clear clinical efficacy of TCM was a promising source for anti-gout ingredients, and the integration screening strategy provides rapid and effective identification method of anti-gout ingredients from complex herb pairs.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144558123","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Screening and Identification of Anti-Gout Components From Herb Pair Combining Ultrafiltration-HPLC-MS, On-Line HPLC-2,2′-Azinobis(3-Ethylbenzothiazoline-6-Sulfonic Acid)-MS and In Silico Analysis: Case Study by Smilacis Glabrae Rhizoma–Dioscoreae Spongiosae Rhizoma 超滤-高效液相色谱-质谱联用、在线高效液相色谱-2,2′-偶氮唑（3-乙基苯并噻唑-6-磺酸）-质谱联用和硅质谱联用筛选鉴定中药对抗痛风成分：以山参-山药为例

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2025-07-04 DOI: 10.1002/jssc.70209

Simeng Hu, Huanying Guo, Ran Miao, Jinqian Yu, Xiao Wang, Hengqiang Zhao

{"title":"Screening and Identification of Anti-Gout Components From Herb Pair Combining Ultrafiltration-HPLC-MS, On-Line HPLC-2,2′-Azinobis(3-Ethylbenzothiazoline-6-Sulfonic Acid)-MS and In Silico Analysis: Case Study by Smilacis Glabrae Rhizoma–Dioscoreae Spongiosae Rhizoma","authors":"Simeng Hu, Huanying Guo, Ran Miao, Jinqian Yu, Xiao Wang, Hengqiang Zhao","doi":"10.1002/jssc.70209","DOIUrl":"https://doi.org/10.1002/jssc.70209","url":null,"abstract":"<div>\u0000 \u0000 <p><i>Smilacis Glabrae Rhizoma–Dioscoreae Spongiosae Rhizoma</i> (SGR-DSR), a herb pair used in traditional Chinese medicine (TCM), has definite curative effect on the clinical treatment of gout. To screen and identify the anti-gout ingredients from SGR-DSR. In this study, an integration strategy combining ultrafiltration-high performance liquid chromatography-mass spectrometry (UF-HPLC-MS) and on-line HPLC-2,2′-azinobis(3-ethylbenzothiazoline-6-sulfonic acid) diammonium salt (ABTS)-MS were proposed and applied for the rapid screening and identification of anti-gout components (xanthine oxidase [XOD] inhibitors and free radical scavengers) from SGR-DSR. As a result, 35 compounds with both potential XOD inhibitor activity and free radical scavenging activity were screened from the herbal pair. Among them, 18 active components were verified by in vitro activity assays. Astilbin showed better XOD inhibition activity and ABTS<sup>•+</sup> scavenging ability with the inhibition rates of 73.76% and 81.56% at 80 µM, respectively. In addition, the molecular docking simulation calculation results showed that all the 18 components had good binding ability with XOD. This study indicated that herb pair with clear clinical efficacy of TCM was a promising source for anti-gout ingredients, and the integration screening strategy provides rapid and effective identification method of anti-gout ingredients from complex herb pairs.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144558124","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Chemical Derivatization-Based Liquid Chromatography-Mass Spectrometry Method for Fatty Acid Profiling in Biological Samples 基于化学衍生的液相色谱-质谱法分析生物样品中的脂肪酸

IF 2.8 3区工程技术

Journal of separation science Pub Date : 2025-07-04 DOI: 10.1002/jssc.70211

Jingxuan Yang, Yi Wu, Liang Zhao, Meng Li, Wenjun Guo, Yajuan Xu, Yang Wang

{"title":"Chemical Derivatization-Based Liquid Chromatography-Mass Spectrometry Method for Fatty Acid Profiling in Biological Samples","authors":"Jingxuan Yang, Yi Wu, Liang Zhao, Meng Li, Wenjun Guo, Yajuan Xu, Yang Wang","doi":"10.1002/jssc.70211","DOIUrl":"https://doi.org/10.1002/jssc.70211","url":null,"abstract":"<div>\u0000 \u0000 <p>Fatty acids (FAs) are important metabolites for various biochemical functions in living organisms, including energy storage, cell structure, and cell signaling. Changes in FAs composition were significantly related to abnormal metabolic levels and body status. In this study, the derivatization-based liquid chromatography-quadrupole-orbitrap mass spectrometry method was established for FA analysis under parallel reaction monitoring mode. The 4-amino-1-benzylpiperidine (4A1BP) was used as a derivatization reagent to amide with FAs. The results showed that protonated molecules of FA+4A1BP–H<sub>2</sub>O were observed, and characteristic fragment ions at <i>m</i>/<i>z</i> 174.1280 and 91.0548 were detected in the tandem mass spectrum. The derivatization method was optimized in terms of sample preparation, chromatographic separation, and mass spectrometric conditions. The linearity, stability, and repeatability of the method were also investigated with good results. Finally, we applied the established method to analyze the serum and liver tissue samples, successfully evaluating the efficacy of Qizha Shuangye granules in the treatment of hyperlipidemia rats. The established method has broad utility and great potential in the detection of FAs, which can provide technical support for disease mechanism research, biomarker discovery, as well as food quality assurance, and nutritional value evaluation.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 7","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144558121","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}

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