Journal of separation science最新文献

{"title":"Efficient and Sensitive Detection of Organophosphate Pesticides in Orange Juice Using Dispersed Solid-Phase Extraction Based on Amorphous UiO-66.","authors":"Yaqi Yin, Chen Fan, Linru Cheng, Yuwei Shan","doi":"10.1002/jssc.70066","DOIUrl":"https://doi.org/10.1002/jssc.70066","url":null,"abstract":"<p><p>Organophosphate pesticides can cause long-term neurological damage to humans. There is an urgent need to develop a more sensitive and efficient method for detecting trace amounts of organophosphorus pesticides in orange juice, particularly in the presence of interfering substances. This study developed a dispersive solid-phase extraction (DSPE) method using amorphous UiO-66 (aUiO-66) as an adsorbent for the detection of four organophosphate pesticides (fenthion, profenofos, fensulfothion, and chlorpyrifos) in orange juice. The aUiO-66 was synthesized in a green, direct method within a deep eutectic solvent composed of diethanolamine hydrochloride and acetamide. Its amorphous nature was confirmed through x-ray diffraction (XRD) and thermogravimetric analysis (TGA). Parameters influencing extraction efficiency, including adsorbent dosage, extraction time, eluent type, and volume, were optimized by genetic neural network (GNN). The method demonstrated good linearity (R² = 0.9927-0.9981), high recovery (95.35%-110.75%), low limit of detection (0.169-0.214 ng L⁻¹), and precision (intraday RSD = 4.13%-5.44%, interday RSD = 3.28%-4.91%). It was successfully applied to analyze targets in commercially available orange juices, detecting residues within 4.37-36.07 µg L⁻¹. This study's methodological development offers significant guidance for efficient detection of organophosphorus pesticides in food products, potentially facilitating the advancement and application of simpler and more efficient analytical techniques.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 1","pages":"e70066"},"PeriodicalIF":2.8,"publicationDate":"2025-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142909827","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":"An Optimized and Sensitive UHPLC-ESI-Q-TOF/HRMS Demonstrated the Dynamic Profiling of Allantoin, N-trans-Feruloyl-3-Methoxytyramine, and N-p-Coumaroyltyramine from Portulaca oleracea L. In Vivo in Rats.","authors":"Kexian Li, Wei Wang","doi":"10.1002/jssc.70055","DOIUrl":"https://doi.org/10.1002/jssc.70055","url":null,"abstract":"<p><p>This study revealed the dynamic profiling of three main components of Portulaca oleracea L. in vivo in rats, namely allantoin (A), N-trans-feruloyl-3-methoxytyramine (M), and N-p-coumaroyltyramine (C). A sensitive and efficient UHPLC-ESI-Q-TOF/HRMS, including an optimized separation process, was applied to their qualitative and quantitative analysis. The validation of the method presented the correlation coefficients, which were over 0.997. The mean matrix factors were 0.930. Recoveries ranged from 96.6% to 109.2%, and determination accuracy varied from 95% to 109.4%. The biological samples included rat plasma, liver, kidneys, bile, and excreta taken after a single oral administration of the saturated DMSO solution of P. oleracea extract. The contents of A, M, and C were of 2.5, 5.1, and 3.4 g/kg in the dry whole herb, respectively. A was identified in the liver and kidneys from 0 to 6 h. Allantoic acid, as one metabolite of A, was found to be kept in plasma for a short time, but another two successive metabolites of A remained over 6 h. It depicted a pharmacological material basis of the herb, regarded with A. The glucuronidation and/or sulfation of M and C were detected in rat bile from 0 to 12 h. The complicated but interesting metabolic schemes for A, M, and C were illustrated from their HRMS and MS/MS performance.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 1","pages":"e70055"},"PeriodicalIF":2.8,"publicationDate":"2025-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142907210","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Development and Validation of a Stability-Indicating High-Performance Liquid Chromatography Method Coupled With a Diode Array Detector for Quantifying Haloperidol in Oral Solution Using the Analytical Quality-by-Design Approach.","authors":"Allan Michael Junkert, Naomi Gerzvolf Mieres, Karime Zeraik Abdalla Domingues, Luana Mota Ferreira, Roberto Pontarolo","doi":"10.1002/jssc.70067","DOIUrl":"https://doi.org/10.1002/jssc.70067","url":null,"abstract":"<p><p>This study developed a stability-indicating HPLC-DAD method for quantifying haloperidol in oral solution using analytical quality-by-design principles. Haloperidol stability was tested under acidic, alkaline, oxidative, and photolytic stress conditions. The analytical quality-by-design approach began by defining the analytical target profile and identifying critical material attributes and critical method parameters via risk analysis. Factorial and Box-Behnken designs, conducted in Design Expert 13, were used to select critical method parameters and determine the method operable design region. The oral solution degraded significantly under acidic and alkaline conditions. Continuous critical method parameters such as mobile phase flow rate, gradient slope, column temperature, and pH were optimized. A quadratic Box-Behnken design with critical method attributes was applied and validated, resulting in robust regression models with significant p-values (> 0.05), absence of lack-of-fit (p-values < 0.05), and R²-adjusted > 0.85. The method proved selective, accurate, and precise within the method operable design range. Normal operating conditions (NOCs) were established using a Waters Symmetry C18 column with a 100-mM formate buffer (pH 3.8) and acetonitrile, with a gradient profile and detection at 246 nm. The operational region included flow rates between 1.2 and 1.35 mL/min (NOC = 1.3 mL/min), temperatures of 8°C-20°C (NOC = 15°C), and mobile phase pH variations from 3.3 to 4.3 (NOC = 3.8). The analytical quality-by-design-based method was robust and effective for stability monitoring, reducing subjectivity while maximizing reliability.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 1","pages":"e70067"},"PeriodicalIF":2.8,"publicationDate":"2025-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142909864","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":"Quasi-Simultaneous and Automated Measurement of Primary Amines and Short-Chain Aldehydes Emission by Dynamic SPME On-Fiber Derivatization Coupled With a Flow-Cell.","authors":"Jian Zou, Shuyu Duan, Bill Winniford, DeGang Zhang","doi":"10.1002/jssc.70070","DOIUrl":"https://doi.org/10.1002/jssc.70070","url":null,"abstract":"<p><p>An automated method was developed to simultaneously measure primary amines and short-chain aldehydes emission from foam and rubber samples in one experiment. The technique involved dynamic solid-phase microextraction (SPME) on-fiber derivatization coupled with a flow-cell unit. The parameters of the dynamic SPME on-fiber derivatization method were optimized, including SPME coating, derivatization agents loading temperature, loading time, and dynamic SPME extraction time. The linearity range for the four primary amines and three aldehydes ranged from 0.5 to 100 µg/m³ and 0.9 to 1050 µg/m³, respectively. The amines and aldehydes' quantitation limits (LOQ) were determined as 0.22-0.27 µg/m³ and 0.10-0.18 µg/m³, respectively. Compared to previous methods, this approach is efficient, labor-saving, and allows researchers to concurrently analyze the emission trends of aldehydes and amines in one experiment.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 1","pages":"e70070"},"PeriodicalIF":2.8,"publicationDate":"2025-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142932097","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":"Identification and Characterization of Chemical Compounds in Compound Shougong Powder by UHPLC-Q-TOF/MS^E Combined With Multiple Data Processing Techniques.","authors":"Rui Yang, Xiaojie Fu, Lanying Li, Ziqi Wei, An Zhou, Huan Wu","doi":"10.1002/jssc.70069","DOIUrl":"https://doi.org/10.1002/jssc.70069","url":null,"abstract":"<p><p>Compound Shougong Powder (CSP) is a traditional Chinese medicine (TCM) preparation recognized for its efficacy in reducing swelling and relieving pain. It is primarily used clinically for the treatment of malignant tumors. However, research on the chemical compounds present in CSP remains limited. In this study, we employed ultra-high-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF/MS^E) combined with multiple data processing techniques to comprehensively characterize the chemical compounds in CSP. This included a multiple-point screening mass defect filtering (MDF), an enhanced method based on conventional MDF and boundary theory that creates a polygonal filtering zone by connecting numerous endpoints (n ≥ 5) to filter target components. Additional techniques utilized were extracted ion chromatogram (EIC), neutral loss filtering (NLF), diagnostic fragment ion filtering (DFIF), and direct identification methods considering retention time, fragmentation behavior, and reference standards. First, UHPLC-Q-TOF/MS^E was applied for comprehensive profiling of CSP's chemical compounds. Then, R language combined with MZmine was used for data preprocessing, enabling the construction of an ion information list to extract valid data. Eventually, through these multiple data processing techniques, a total of 116 chemical compounds in CSP were identified, including 34 flavonoids, 38 saponins, seven stilbenes, six anthraquinones, 12 organic acids, 13 terpenoids, and six others. In summary, this study elucidates the chemical composition of CSP, contributing to the discovery of potential active ingredients for CSP. Additionally, the established strategy provided a powerful guide for the chemical characterization of TCM.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 1","pages":"e70069"},"PeriodicalIF":2.8,"publicationDate":"2025-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142909829","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":"Integrating Ultra-High-Performance Liquid Chromatography and Orbitrap High-Resolution Mass Spectrometry, Feature-Based Molecular Networking, and Network Medicine to Unlock Harvesting Strategies for Endangered Sinocalycanthus Chinensis.","authors":"Yingpeng Tong, Xin Li, Jiang Wan, Qi Zhou, Chunxiao Jiang, Na Li, Zexin Jin, Junjie Gu, Fan Li, Junmin Li","doi":"10.1002/jssc.70072","DOIUrl":"https://doi.org/10.1002/jssc.70072","url":null,"abstract":"<p><p>Evaluating the practical utility of endangered plant species is crucial for their conservation. Nevertheless, numerous endangered plants, including Sinocalycanthus chinensis, lack historical usage data, leading to a paucity of guidance in traditional pharmacological research. This gap impedes their development and potential utilization. Ultra-high-performance liquid chromatography and Orbitrap high-resolution mass spectrometry were employed to analyze the S. chinensis leaves collected at different harvesting times. Then, the metabolites were automatically annotated by a self-built R script in conjunction with characteristic fragment ions, neutral loss filtering, and feature-based molecular networking. By integrating metabolomics with network medicine analysis, the potential usage and optimal harvest times for S. chinensis were unlocked. A total of 305 metabolites were identified, with 66.8% annotated by self-built R script. A progressive increase in metabolite disparities was observed from May to August, followed by a relatively minor distinction from August to October. Notably diverse metabolites were detected in S. chinensis harvested during different periods, implying potential variations in efficacy. Network medicine analysis indicated possible therapeutic implications of S. chinensis for lung cancer, diabetes, bladder cancer, and Alzheimer's disease. Samples collected in May and September demonstrated exceptional efficacy. Harvesting was strategically conducted during these months based on variations in sample characteristics and metabolite content, tailored to their intended applications for dietary or medicinal purposes. This study developed an efficient methodology for investigating metabolites and exploring the potential applications of S. chinensis in food and herbal medicine. Consequently, it provides technical support for the sustainable conservation of endangered plants with limited clinical application experience.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 1","pages":"e70072"},"PeriodicalIF":2.8,"publicationDate":"2025-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142932095","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":"An Imaged Capillary Isoelectric Focusing Separation of the Linear and Cyclic Variants of a Mimotope of the Cancer-Related CD20 Antigen-Validation and Statistical Evaluation.","authors":"Georg Bloderer, Luigi Grassi, Chiara Cabrele, Hanno Stutz","doi":"10.1002/jssc.70054","DOIUrl":"10.1002/jssc.70054","url":null,"abstract":"<p><p>Imaged capillary isoelectric focusing was successfully applied for separating an in-house synthesized closely related peptide pair, that is, a linear 12-mer (Rp5-L) and its cyclic 15-mer variant (Rp5-C). Rp5-L represents a mimotope, that is, an epitope mimicking peptide, of the CD20 antigen, which is over-expressed in B-cell-related tumors. Peptide identity-including the successful disulfide bond formation in Rp5-C-was confirmed with matrix-assisted laser desorption ionization-time of flight mass spectrometry. The purity of synthesized products was determined by a reversed-phase high-performance liquid chromatographic method with ultraviolet detection. The apparent isoelectric point (pI) of cyclic Rp5-C and Rp5-L was 5.99 and 6.47, respectively. An appropriate combination of carrier ampholytes allowed for their baseline separation with an analysis time of <20 min. Method validation was done for the synthesized peptides and three flanking pI markers covering, for example, repeatability and intermediate precision. Calibrations on different days resulted in identical slopes for Rp5-L and Rp5-C, respectively, as statistically confirmed by Welch's t-test and pooled t-test over 8 days. The calibration data of mimotopes and pI markers were evaluated for outliers, normality, homoscedasticity, and autocorrelation with complementary statistical procedures, which identified an otherwise unnoticed outlier for a pI marker. The linearity of calibration for Rp5-L, Rp5-C, and the pI markers was tested with Mandel's fitting test and lack-of-fit test. For Rp5-L and Rp5-C, the calculated limits of detection and limits of quantification were ≤0.31 and ≤0.96 µmol/L, respectively.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 1","pages":"e70054"},"PeriodicalIF":2.8,"publicationDate":"2025-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11685353/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142909860","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":"Column Screening and Development of HILIC and RPLC Methods Coupled to Tandem Mass Spectrometry for the Monitoring of Albumin on Cysteine 34 Exposed to Mustard Agents.","authors":"Lorenzo Avigo, Audrey Combès, Charlotte Desoubries, Christine Albaret, Anne Bossée, Emmanuel Joubert, Valérie Pichon","doi":"10.1002/jssc.70065","DOIUrl":"https://doi.org/10.1002/jssc.70065","url":null,"abstract":"<p><p>Adduction on protein nucleophile sites by mustard agents can be monitored to assess detection of retrospective exposure to these agents. Cysteine 34 (Cys34) on human serum albumin was selected as the target of choice. This work targets di- and tripeptides adducted on Cys34 by sulfur mustard, sesquimustard, and nitrogen mustards separated in hydrophilic liquid chromatography (HILIC) and Reversed-Phase (RP) mode. The effect of several mobile phase additives on the mass spectrometry (MS) and MS/MS signal and on LC retention profile was studied. A mix of ammonium acetate and acetic acid offered satisfactory results in terms of MS sensitivity. Screening of HILIC columns was performed, and ZIC-HILIC stationary phase was selected for HILIC mode, and C₁₈ stationary phase was used for RP analysis. Negative ionization mode leads to a higher S/N ratio compared to positive ionization mode. Adducted tripeptides were selected for the monitoring of mustard agents' exposure, allowing better sensitivity than their dipeptide homologues. The two developed chromatographic methods have similar sensitivities with LOQs ranging from 1.9 to 20.5 ng/mL for the reversed-phase liquid chromatography (RPLC)-ESI-(-)-MS/MS method and from 1.7 to 43.3 ng/mL for the HILIC-ESI-(-)-MS/MS method. The monitoring method should be selected based on the targeted mustard agent, and the remaining method can be a confirmation tool.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 1","pages":"e70065"},"PeriodicalIF":2.8,"publicationDate":"2025-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142909861","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 Advances in Screening and Separating Active Components From Natural Products Based on High-Speed Countercurrent Chromatography","authors":"Xing-Cui Wang,&nbsp;Xin-Yi Huang,&nbsp;Fu-Xin Zhang,&nbsp;Jules Muhire,&nbsp;Duo-Long Di,&nbsp;Jun Hai,&nbsp;Dong Pei","doi":"10.1002/jssc.70051","DOIUrl":"10.1002/jssc.70051","url":null,"abstract":"<div>\u0000 \u0000 <p>Natural products play a vital role in human health because people find that they can reduce the incidence of many diseases, such as cancer and cardiovascular diseases. Therefore, researchers have developed many effective techniques for screening and separating active compounds from natural products. High-speed countercurrent chromatography is a unique unsupported liquid–liquid chromatography technology that has been widely used in the separation of natural products. In this paper, the research progress of screening and separating active components from natural products by combining high-speed countercurrent chromatography technology with other technologies is reviewed from two aspects: pre-column activity assay and post-column activity assay. The purpose of this paper is to provide some theoretical support for the screening and separation of natural active compounds by high-speed countercurrent chromatography. I hope that the contents summarized in this paper can provide more basis for the development of screening and separation of natural active compounds to realize large-scale preparation.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"47 24","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-12-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142836988","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":"Research on the Selective Extraction of Oxibendazole Residues in Animal-Derived Food Using Molecularly Imprinted Polymers","authors":"Yue Qiu,&nbsp;Yue Wang,&nbsp;Chengli Xie,&nbsp;Yike Huang,&nbsp;Genrong Li,&nbsp;Zhining Xia","doi":"10.1002/jssc.70052","DOIUrl":"10.1002/jssc.70052","url":null,"abstract":"<div>\u0000 \u0000 <p>To achieve specific adsorption-based sample preparation for the poorly soluble veterinary drug oxibendazole, this study employed 4-vinylpyridine as the functional monomer and conducted radical polymerization on the surface of functionalized silica nanoparticles to synthesize a surface molecularly imprinted polymer (OBZMIP). This OBZMIP exhibited good adsorption capacity for oxibendazole within 30 min, with its adsorption behavior conforming to the pseudo–second-order kinetic and Langmuir models, predicting a maximum adsorption capacity of 4.93 mg/g. After five adsorption–desorption cycles, the adsorption capacity remained unchanged, demonstrating excellent reusability. In a mixed system containing eight similar compounds, the selectivity coefficients ranged from 1.3 to 16.9, indicating outstanding specific recognition ability. Utilized as an adsorbent packing material for solid-phase extraction, the prepared OBZMIP demonstrated significantly high recovery rates in the extraction of oxibendazole from four distinct meat samples. Therefore, OBZMIP holds promising applications in the selective extraction of veterinary drug oxibendazole residues during the pretreatment of meat samples.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"47 24","pages":""},"PeriodicalIF":2.8,"publicationDate":"2024-12-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142837176","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}