Journal of Chromatography A最新文献_第5页

Amino-β-cyclodextrin derivatives with different chain lengths as chiral selectors for separation of dansyl amino acid enantiomers by capillary electrophoresis

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-02-14 DOI: 10.1016/j.chroma.2025.465781

Yuanyuan Fu , Min Jiang , Zilin Chen

To date, cyclodextrins (CDs) and their derivatives are recognized as highly effective chiral selectors in electrophoresis for enantiomer separation due to their numerous advantages. In this study, three amino-β-CD derivatives, including NH₂-β-CD-5 (Mono-(6-(tetraethylenepentamine)-6-deoxy)-beta-Cyclodextrin), NH₂-β-CD-3 (mono-(6-(diethylenetriamine)-6-deoxy)-β-Cyclodextrin), and NH₂-β-CD-1 (6-Monodeoxy-6-monoamino-beta-cyclodextrine) with varying amino substituent chain lengths were employed as chiral selectors in capillary electrophoresis (CE) to examine their chiral selectivity in the separation of five dansylated amino acid enantiomers, namely Dns-DL-Val, Dns-DL-Leu, Dns-DL-Thr, Dns-DL-Phe, and Dns-DL-Ser, as the chain length of the substituent group significantly impacts separation performance. Among the three amino-β-CD derivatives, NH₂-β-CD-5 exhibited superior performance by separating four dansylated amino acid enantiomers, whereas NH₂-β-CD-3 and NH₂-β-CD-1 separated only two and one enantiomers, respectively. Additionally, the effects of pH values, buffer concentrations, and concentrations of the chiral selectors on the separation of dansylated amino acid enantiomers were also investigated. Furthermore, the stability and reproducibility of the three amino-β-CD derivatives were evaluated, with the relative standard deviations (RSDs) of resolution all below 8.2 %.

{"title":"Amino-β-cyclodextrin derivatives with different chain lengths as chiral selectors for separation of dansyl amino acid enantiomers by capillary electrophoresis","authors":"Yuanyuan Fu , Min Jiang , Zilin Chen","doi":"10.1016/j.chroma.2025.465781","DOIUrl":"10.1016/j.chroma.2025.465781","url":null,"abstract":"<div><div>To date, cyclodextrins (CDs) and their derivatives are recognized as highly effective chiral selectors in electrophoresis for enantiomer separation due to their numerous advantages. In this study, three amino-β-CD derivatives, including NH<sub>2</sub>-β-CD-5 (Mono-(6-(tetraethylenepentamine)-6-deoxy)-beta-Cyclodextrin), NH<sub>2</sub>-β-CD-3 (mono-(6-(diethylenetriamine)-6-deoxy)-β-Cyclodextrin), and NH<sub>2</sub>-β-CD-1 (6-Monodeoxy-6-monoamino-beta-cyclodextrine) with varying amino substituent chain lengths were employed as chiral selectors in capillary electrophoresis (CE) to examine their chiral selectivity in the separation of five dansylated amino acid enantiomers, namely Dns-DL-Val, Dns-DL-Leu, Dns-DL-Thr, Dns-DL-Phe, and Dns-DL-Ser, as the chain length of the substituent group significantly impacts separation performance. Among the three amino-β-CD derivatives, NH<sub>2</sub>-β-CD-5 exhibited superior performance by separating four dansylated amino acid enantiomers, whereas NH<sub>2</sub>-β-CD-3 and NH<sub>2</sub>-β-CD-1 separated only two and one enantiomers, respectively. Additionally, the effects of pH values, buffer concentrations, and concentrations of the chiral selectors on the separation of dansylated amino acid enantiomers were also investigated. Furthermore, the stability and reproducibility of the three amino-β-CD derivatives were evaluated, with the relative standard deviations (RSDs) of resolution all below 8.2 %.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1746 ","pages":"Article 465781"},"PeriodicalIF":3.8,"publicationDate":"2025-02-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143437830","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Suberin as a green surfactant additive for peptide analysis using capillary electrophoresis

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-02-13 DOI: 10.1016/j.chroma.2025.465774

Isabella Kwan , Parisa Askarisarvestani , Anton Wiberg , Peter Skagerlind , Monica Ek , Åsa Emmer

Capillary electrophoresis is a powerful separation technique for analysis of proteins and peptides, with benefits like low consumption of reagents, solvents and sample. The separation efficiency and resolution can be deteriorated by adsorption of analytes to the inner capillary wall, though. Many methods to circumvent this obstacle have been reported, including background electrolyte addition of surfactants that aggregate as protective coatings at the wall. In this work, anionic suberin surfactant was used together with the cationic surfactant cetyltrimethylammonium bromide (CTAB) for analysis of trypsin digested lysozyme as a model sample. Suberin fatty acids were extracted from birch bark, which is a side-stream product originating from pulp and paper waste streams.

Different adjustments of the solvent extraction protocol, and the method to neutralize the suberin fatty acids to obtain surface active sodium salts were evaluated regarding number of peaks observed, separation repeatability, and analysis time. The influence of background electrolyte pH was also studied.

The potential of the surface-active sodium salts of suberin fatty acids as an additive enhancer in combination with CTAB is illustrated by excellent repeatability, especially at lower pH values. The number of peaks observed was also higher at lower pH, while the analysis time was shorter.

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引用次数: 0

Comparative analysis of impurity profiles in rifampicin capsules with different crystal forms using LC-MS/MS

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-02-13 DOI: 10.1016/j.chroma.2025.465769

Yun Shen , Jinlin Zhang , Qian Zhang , Wen-Qian Liu , Si-Tong Zheng , Sheng Tang , Yaozuo Yuan , Hian Kee Lee , Hai-Wei Shi

Rifampicin (RIF) is a kind of semi-synthetic antibiotic with broad-spectrum antibacterial action, which has remarkable antibacterial activity against many pathogenic microorganisms. The World Health Organization classifies RIF as critically important for human medicine, especially for tuberculosis treatment. The polymorphic nature of RIF contributes to the complexity of the impurities of the drug. Lack of systematic and comparative studies on its impurities in different crystal forms may affect the efficiency of this drug and increase the incidence of adverse reactions. Current methods in pharmacopoeias and literature can only separate a limited number of known impurities, and the process of preparing the mobile phase is highly cumbersome. In this work, response surface methodology was employed to optimize the conditions of one-dimensional liquid chromatography (LC) as an alternative approach to pharmacopoeia methods. This method demonstrated high accuracy and sensitivity, enabling the quantification of impurities as low as 0.25 μg/mL. The proposed method provided satisfactory linearity, percentage of recovery from 88 to 101 % with relative standard, deviations (RSD) lower than 5 %, indicating good precision. Additionally, the parallel determination of 6 sample solutions showed that the content changes of the relevant components were within an acceptable range, demonstrating method repeatability. A detection method based on high-resolution two-dimensional LC-mass spectrometry (2D-LC-MS/MS) was developed to analyze. A total of 25 impurities were identified and the impurity profiles were systematically investigated for the first time, providing experimental basis for the quality control of the drug.

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引用次数: 0

Cell-free synthesis of membrane receptors for preparation of NKG2A monolithic micro-affinity chromatography

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-02-13 DOI: 10.1016/j.chroma.2025.465775

Chun Chen , Xinyi Chai , Yanqiu Gu , Chengliang Wang , Yongfang Yuan , Yifeng Chai , Zhengjin Jiang , Xiaofei Chen

Membrane receptor affinity chromatography is a practical strategy for screening compounds targeting membrane receptors and determining their binding affinity. The key of these methods is to create a biomimetic cell membrane environment for the immobilization of specific receptors on chromatographic stationary phase. However, its large-scale applications are limited by the labor-intensive and time-consuming procedures including cell culture, recombinant protein expression and column packing. Furthermore, traditional affinity chromatography columns are prone to drawbacks such as heterogeneous composition of the stationary phase and low permeability. In this study, a novel membrane receptor biological affinity chromatographic method based on cell-free protein synthesis (CFPS) and Bis(sulfosuccinimidyl)suberate modified monolithic stationary phase was developed for fast preparation of monolithic micro-affinity column in batches, which realized efficient synthesis and immobilization of immune checkpoint natural killer group 2 family of receptor A (NKG2A) with controlled orientation. Coupling the prepared NKG2A micro-affinity column with an offline-2D-UPLC-QTOF/MS system, two new NKG2A inhibitors, baicalin and wogonoside, were screened out with the K_D values of 30.23 and 13.01 μM respectively, significantly upregulating the gene expression of granzyme B, tumor necrosis factor-α and interferon-γ and the protein expression of CD107a in natural killer (NK) cells. Moreover, the cytotoxic activity of NK cells against tumor cells was enhanced by these two compounds. The proposed CFPS-based monolithic micro-affinity chromatography realizes rapid synthesis and immobilization of transmembrane receptors within one day, achieving homogeneity, good permeability and orientation-controlled high expression. This approach could be extended to any interested transmembrane receptors for rapid drug screening and affinity determination.

{"title":"Cell-free synthesis of membrane receptors for preparation of NKG2A monolithic micro-affinity chromatography","authors":"Chun Chen , Xinyi Chai , Yanqiu Gu , Chengliang Wang , Yongfang Yuan , Yifeng Chai , Zhengjin Jiang , Xiaofei Chen","doi":"10.1016/j.chroma.2025.465775","DOIUrl":"10.1016/j.chroma.2025.465775","url":null,"abstract":"<div><div>Membrane receptor affinity chromatography is a practical strategy for screening compounds targeting membrane receptors and determining their binding affinity. The key of these methods is to create a biomimetic cell membrane environment for the immobilization of specific receptors on chromatographic stationary phase. However, its large-scale applications are limited by the labor-intensive and time-consuming procedures including cell culture, recombinant protein expression and column packing. Furthermore, traditional affinity chromatography columns are prone to drawbacks such as heterogeneous composition of the stationary phase and low permeability. In this study, a novel membrane receptor biological affinity chromatographic method based on cell-free protein synthesis (CFPS) and Bis(sulfosuccinimidyl)suberate modified monolithic stationary phase was developed for fast preparation of monolithic micro-affinity column in batches, which realized efficient synthesis and immobilization of immune checkpoint natural killer group 2 family of receptor A (NKG2A) with controlled orientation. Coupling the prepared NKG2A micro-affinity column with an offline-2D-UPLC-QTOF/MS system, two new NKG2A inhibitors, baicalin and wogonoside, were screened out with the <em>K<sub>D</sub></em> values of 30.23 and 13.01 μM respectively, significantly upregulating the gene expression of granzyme B, tumor necrosis factor-<em>α</em> and interferon-<em>γ</em> and the protein expression of CD107a in natural killer (NK) cells. Moreover, the cytotoxic activity of NK cells against tumor cells was enhanced by these two compounds. The proposed CFPS-based monolithic micro-affinity chromatography realizes rapid synthesis and immobilization of transmembrane receptors within one day, achieving homogeneity, good permeability and orientation-controlled high expression. This approach could be extended to any interested transmembrane receptors for rapid drug screening and affinity determination.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1746 ","pages":"Article 465775"},"PeriodicalIF":3.8,"publicationDate":"2025-02-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143437831","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Recent advances in lipid analysis by capillary electromigration methods, 2019–2024

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-02-12 DOI: 10.1016/j.chroma.2025.465756

Pierre Gavard , Amélie Gavard , Lucie Perquis , Fabrice Collin , François Couderc

Following a long period during which Capillary Electrophoresis (CE) was little used for lipid analysis (see Poinsot et al., Electrophoresis, 40, 2019, 190–211), the last five years have seen an increase in publications on this subject. Micellar Electrokinetic Chromatography (MEKC) can now compete with Gas Chromatography (GC) for the analysis of fatty acids, while non-aqueous capillary electrophoresis (NACE) now allows the study of fatty acids as well as phospholipids or glycolipids. As NACE also allows easy coupling to Mass Spectrometry (MS) in both positive and negative Electrospray Ionization (ESI), the technique has now become sufficiently robust, and for laboratories equipped with GC or Liquid Chromatography (LC) to consider using CE, particularly as it presents the advantage of much faster sample preparation than with GC for fatty acids and a resolution identical to LC for phospholipids and glycolipids. In this article, we will therefore describe the advances made in this area over the last five years.

引用次数: 0

Synthesis of sulfonamide-functionalized magnetic microporous organic network for magnetic solid-phase extraction of polar aromatic amines from tea beverages

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-02-12 DOI: 10.1016/j.chroma.2025.465773

Yi-Xin Zhong , Chun-Ying Xu , Yi-Fan Cao , Hong-Liang Li , Cheng-Xiong Yang

Aromatic amines (AAs) are a typical class of carcinogenic contaminants frequently present in food packaging materials. Considering the huge consumption of tea beverages in our daily life and the frequently usage of packaging materials in tea beverages, establishment of sensitive and selective method to detect polar and trace AAs in tea beverages is urgently needed. Herein, a sulfonamide-functionalized magnetic microporous organic network (MMON-SO₂NH₂) was synthesized for the efficient magnetic solid-phase extraction (MSPE) of AAs from tea beverages through the pre-designed electrostatic attraction, π-π, hydrophobic, and hydrogen bonding interactions. MMON-SO₂NH₂ demonstrated large surface area (304.4 m² g^-1), rapid magnetic responsiveness (38.3 emu g^-1, < 15 s), and good stability and reusability (> 8 times), being an ideal magnetic adsorbent for AAs. The established MMON-SO₂NH₂−MSPE-HPLC-UV method gave wide linear ranges (1–1000 µg L^-1), low limits of detection (0.3–1.0 µg L^-1) and limits of quantitation (1.0–3.0 µg L^-1), large enrichment factors (80.3–85.6), and good anti-interference ability. Satisfactory recoveries were obtained, which demonstrated the potential of MMON-SO₂NH₂ for efficient enrichment of trace AAs in complex samples and uncovered the promising of sulfonamide-functionalized magnetic adsorbent in sample pretreatment.

{"title":"Synthesis of sulfonamide-functionalized magnetic microporous organic network for magnetic solid-phase extraction of polar aromatic amines from tea beverages","authors":"Yi-Xin Zhong , Chun-Ying Xu , Yi-Fan Cao , Hong-Liang Li , Cheng-Xiong Yang","doi":"10.1016/j.chroma.2025.465773","DOIUrl":"10.1016/j.chroma.2025.465773","url":null,"abstract":"<div><div>Aromatic amines (AAs) are a typical class of carcinogenic contaminants frequently present in food packaging materials. Considering the huge consumption of tea beverages in our daily life and the frequently usage of packaging materials in tea beverages, establishment of sensitive and selective method to detect polar and trace AAs in tea beverages is urgently needed. Herein, a sulfonamide-functionalized magnetic microporous organic network (MMON-SO<sub>2</sub>NH<sub>2</sub>) was synthesized for the efficient magnetic solid-phase extraction (MSPE) of AAs from tea beverages through the pre-designed electrostatic attraction, π-π, hydrophobic, and hydrogen bonding interactions. MMON-SO<sub>2</sub>NH<sub>2</sub> demonstrated large surface area (304.4 m<sup>2</sup> g<sup>-1</sup>), rapid magnetic responsiveness (38.3 emu g<sup>-1</sup>, < 15 s), and good stability and reusability (> 8 times), being an ideal magnetic adsorbent for AAs. The established MMON-SO<sub>2</sub>NH<sub>2</sub>−MSPE-HPLC-UV method gave wide linear ranges (1–1000 µg L<sup>-1</sup>), low limits of detection (0.3–1.0 µg L<sup>-1</sup>) and limits of quantitation (1.0–3.0 µg L<sup>-1</sup>), large enrichment factors (80.3–85.6), and good anti-interference ability. Satisfactory recoveries were obtained, which demonstrated the potential of MMON-SO<sub>2</sub>NH<sub>2</sub> for efficient enrichment of trace AAs in complex samples and uncovered the promising of sulfonamide-functionalized magnetic adsorbent in sample pretreatment.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1746 ","pages":"Article 465773"},"PeriodicalIF":3.8,"publicationDate":"2025-02-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143427810","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Knox-Saleem kinetic performance limits in liquid chromatography. Part 2: Alternative interpretation – No upper limit to separation performance

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-02-11 DOI: 10.1016/j.chroma.2025.465753

Leonid M. Blumberg

In Part 1 of this series, the original Knox-Saleem study of the effects of column dimensions and operational conditions on the column performance was reformulated in contemporary language and expanded to a broader class of the columns and their operational conditions. However, the view of the effects in Part 1 was the same as in the original Knox-Saleem study. In both cases, the effects were treated as the performance limits. The following issues were addressed. What is the shortest time for obtaining a required separation performance if column pressure is limited? What is the highest separation performance achievable in a given time at a given pressure? And so forth. While addressing these issues, it has been established in Part 1 that there is no fundamental limit to the separation performance of any given column structure. For example, any separation performance of a packed column (e.g., any peak capacity) no matter how high can be obtained at any pressure no matter how low as long as the analysis time is acceptable. This and similar factors suggest that the effects of a column parameters and operational conditions on the column performance might be viewed not as the limits, but as the tradeoffs between the parameters, the operational conditions and the performance. This approach is developed in this report. The properties of the tradeoffs are evaluated, and potential performance of several column structures is compared.

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引用次数: 0

Application of deep eutectic solvents for the simultaneous determination of organophosphorus and pyrethroid pesticides in aqueous matrices and the assessment of its level of whiteness

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-02-11 DOI: 10.1016/j.chroma.2025.465770

William Henrique Slominski, Vanessa Boz dos Santos, Fernando Roberto Xavier, Rogério Aparecido Gariani, Edmar Martendal

This work presents as a novelty the development of a method for the simultaneous determination of organophosphorus and pyrethroid pesticides in aqueous samples using only deep eutectic solvents (DES) followed by a gas chromatography-mass spectrometry analysis. Combining 4 hydrogen bond acceptors and 6 hydrogen bond donors, 17 DES were prepared. Menthol:thymol in a 1:1 molar ratio presented the best extraction performance and was, therefore, characterized by Fourier transform infrared spectroscopy (FTIR), hydrogen-nuclear magnetic resonance (¹H NMR) and nuclear Overhauser effect spectroscopy (NOESY-NMR), comparing the spectra from the pure components and from the DES. In the FTIR analysis, the main shifts occurred in the CO bonds. The NMR analyses allowed a better understanding of the interactions occurring during solvent formation, which were attributed to the interaction between the hydroxyls from menthol and thymol. Vortex-assisted dispersive liquid-liquid microextraction (DLLME) required no dispersing solvents. The main variables affecting the extraction were optimized using full factorial design, including a triplicate center point. For a fixed 10-mL sample volume, the optimum ranges obtained were: 3.0 ± 0.60 g of NaCl, pH in the range from 5 to 9, a vortex stirring time of 4 ± 2 min and 150 μL of a DES composed of menthol and thymol in a 1:1 molar ratio. Satisfactory figures of merit were then obtained: coefficients of determination greater than 0.99, linear working ranges from 1 μg/L to 400 μg/L, limit of detections of 0.3 μg/L, an inter-day precision from 1.33 % to 9.86 % (n = 12), and an intra-day precision from 4.65 % to 15.52 % (n = 4). The application was carried out in six different aqueous matrices, with methyl parathion being detected in a lake sample. An excellent mean recovery of 98.0 % was obtained for the three levels evaluated and all analytes. The comparison with other methods was based on the principles of White Analytical Chemistry using Algorithm 12, by which the method proposed in this work showed a higher level of whiteness compared to the others.

{"title":"Application of deep eutectic solvents for the simultaneous determination of organophosphorus and pyrethroid pesticides in aqueous matrices and the assessment of its level of whiteness","authors":"William Henrique Slominski, Vanessa Boz dos Santos, Fernando Roberto Xavier, Rogério Aparecido Gariani, Edmar Martendal","doi":"10.1016/j.chroma.2025.465770","DOIUrl":"10.1016/j.chroma.2025.465770","url":null,"abstract":"<div><div>This work presents as a novelty the development of a method for the simultaneous determination of organophosphorus and pyrethroid pesticides in aqueous samples using only deep eutectic solvents (DES) followed by a gas chromatography-mass spectrometry analysis. Combining 4 hydrogen bond acceptors and 6 hydrogen bond donors, 17 DES were prepared. Menthol:thymol in a 1:1 molar ratio presented the best extraction performance and was, therefore, characterized by Fourier transform infrared spectroscopy (FTIR), hydrogen-nuclear magnetic resonance (<sup>1</sup>H NMR) and nuclear Overhauser effect spectroscopy (NOESY-NMR), comparing the spectra from the pure components and from the DES. In the FTIR analysis, the main shifts occurred in the C<img>O bonds. The NMR analyses allowed a better understanding of the interactions occurring during solvent formation, which were attributed to the interaction between the hydroxyls from menthol and thymol. Vortex-assisted dispersive liquid-liquid microextraction (DLLME) required no dispersing solvents. The main variables affecting the extraction were optimized using full factorial design, including a triplicate center point. For a fixed 10-mL sample volume, the optimum ranges obtained were: 3.0 ± 0.60 g of NaCl, pH in the range from 5 to 9, a vortex stirring time of 4 ± 2 min and 150 μL of a DES composed of menthol and thymol in a 1:1 molar ratio. Satisfactory figures of merit were then obtained: coefficients of determination greater than 0.99, linear working ranges from 1 μg/L to 400 μg/L, limit of detections of 0.3 μg/L, an inter-day precision from 1.33 % to 9.86 % (<em>n</em> = 12), and an intra-day precision from 4.65 % to 15.52 % (<em>n</em> = 4). The application was carried out in six different aqueous matrices, with methyl parathion being detected in a lake sample. An excellent mean recovery of 98.0 % was obtained for the three levels evaluated and all analytes. The comparison with other methods was based on the principles of White Analytical Chemistry using Algorithm 12, by which the method proposed in this work showed a higher level of whiteness compared to the others.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1745 ","pages":"Article 465770"},"PeriodicalIF":3.8,"publicationDate":"2025-02-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143420593","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Finding potentially erroneous entries in METLIN SMRT

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-02-09 DOI: 10.1016/j.chroma.2025.465761

Mikhail Khrisanfov , Dmitriy Matyushin , Andrey Samokhin

METLIN SMRT is a widely-used dataset of retention times for high-performance liquid chromatography (HPLC). Besides direct application it is used for training models aimed at predicting retention times in HPLC. Although there are quite a number of articles featuring METLIN SMRT, the pipelines used for filtering from errors are either simplistic or nonexistent. Therefore, a reliable method for filtering potentially erroneous entries is still required. An approach to filter potentially erroneous entries, suggested in our earlier work for a database of gas chromatography retention indexes, was repurposed for METLIN SMRT using five predictive models (GNN, CNN, FCFP, FCD, and CatBoost). The retention times were predicted for the whole dataset using a 5-fold cross-validation strategy. Entries with retention times differing significantly from the predictions obtained from a given model (bottom 5%) were flagged with a “yellow card”. This procedure was repeated for each model, leading to a group containing about 1500 entries (or 2% of the dataset) with 5 “yellow cards”. According to our estimate (derived from analyzing trends and distributions for groups with varying numbers of “yellow cards”) about 1200 entries were strongly suspected to be erroneous, while 300 were likely predicted inaccurately. This work demonstrates the viability of the approach and its potential to improve the quality of other large-scale chromatography-related databases for both machine learning and experimental use.

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引用次数: 0

In-situ formation of deep eutectic supramolecule based extraction method coupled to valve switching ion chromatography mass spectrometry for the determination of aminoglycosides in meat

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2025-02-09 DOI: 10.1016/j.chroma.2025.465757

Xuxia Liang , Zhixiong Zhong , Jianchao Deng , Runkun Zhang

A novel extraction methodology was developed for extracting nine aminoglycosides (AGs) from meats based on the in-situ formation of deep eutectic supramolecule between analytes and gallic acid. Good chromatographic separation was achieved on a cation-exchange column utilizing solely a diluted organic acid as the eluent. A matrix-switching system was created to divert common inorganic cations from the column effluent to waste, reducing conductance peak values by 99.8 % and mitigating ion suppression in high-resolution electrospray ionization. The methodology was validated and exhibited excellent linearity across a concentration range of 20–800 μg L⁻¹, with correlation coefficients (r) ranging from 0.9982 to 0.9997. The limits of detection and quantification were in the range of 7.1–13.8 μg kg⁻¹ and 22.8–44.0 μg kg⁻¹, respectively. The method was applied to the analysis of nine AGs in forty-five samples, attaining recovery values ranging from 89.1 % to 102.1 % with relative standard deviations of 1.9 %-6.4 %. The study provides a reliable procedure that complies with the requirements of the EU's official methods of analysis for identifying and quantifying the restricted and prohibited substances. The method simplifies operations and shortens extraction times by ingeniously integrating various techniques. It also eliminates the need for toxic reagents and streamlines operations compared to the conventional liquid chromatography. The results showed that IC-MS is a convenient and selective complementary approach to other modes of chromatography for determining multiple AGs in complex samples.

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引用次数: 0