Journal of Chromatography A最新文献_第2页

Automatic and precise identification of volatile organic compounds from gas chromatography in prolonged atmospheric monitoring

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-05-08 DOI: 10.1016/j.chroma.2025.466035

Wei Luo , Jingping Hu , Huijie Hou , Jiakuan Yang

{"title":"Automatic and precise identification of volatile organic compounds from gas chromatography in prolonged atmospheric monitoring","authors":"Wei Luo , Jingping Hu , Huijie Hou , Jiakuan Yang","doi":"10.1016/j.chroma.2025.466035","DOIUrl":"10.1016/j.chroma.2025.466035","url":null,"abstract":"<div><div>Long-term continuous monitoring of volatile organic compounds (VOCs) is pivotal for climate change research, air quality assessment, pollution source identification, and public health early warning systems. Prolonged VOC monitoring is routinely implemented by gas chromatographs. However, accurate identification of target contaminants heavily relies on time-consuming and error-prone manual processes conducted by professional personnel due to complex chromatograms and anomalous patterns. This study proposes an artificial intelligence-based model, ResGRU, for the automated and precise identification of VOCs in a chromatograph. By taking real data from a monitoring site in Shanghai, the model achieved a mean absolute error of 0.0144 min for retention time localization, which is 2.76 to 38.19 times smaller compared to conventional machine learning or deep learning models by previous reports. Moreover, it achieves precise recognition of subtle chromatographic peaks and exceptional adaptability to abnormal chromatograms. Notably, the vast majority of these weak peaks are attributed to olefinic compounds, which exhibit exceptionally high ozone formation potential. In addition, cross-transfer verification of data from four monitoring sites in Shanghai, Hubei, and Jiangsu, China further proved the robust transferability of this model. This work provides a novel methodology for precise analysis of GC data, enabling deeper exploration of the mechanisms behind VOCs pollution over extended temporal scales.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1754 ","pages":"Article 466035"},"PeriodicalIF":3.8,"publicationDate":"2025-05-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143942903","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

Green extraction of bioactives from Vitis vinifera L. cv. Tannat pomace and chemical characterization by comprehensive two-dimensional liquid chromatography (LC × LC)

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-05-08 DOI: 10.1016/j.chroma.2025.466030

Mikaela Rajchman , Lidia Montero , Adrián Aicardo , Rafael Radi , Miguel Herrero

{"title":"Green extraction of bioactives from Vitis vinifera L. cv. Tannat pomace and chemical characterization by comprehensive two-dimensional liquid chromatography (LC × LC)","authors":"Mikaela Rajchman , Lidia Montero , Adrián Aicardo , Rafael Radi , Miguel Herrero","doi":"10.1016/j.chroma.2025.466030","DOIUrl":"10.1016/j.chroma.2025.466030","url":null,"abstract":"<div><div>Grape pomace is an important by-product generated during winemaking that still possesses relevant concentrations of interesting bioactive compounds. As the production of this by-product is very high, developing strategies to produce its valorization in an effort to provide means for the generation of high-added value products is desired. Tannat grapes are particularly rich in phenolic compounds and, consequently, the pomace derived from them may still be rich in those components. The use of compressed fluids-based extraction techniques, such as supercritical fluid extraction (SFE) and pressurized liquids extraction (PLE) retains good potential for the isolation of bioactive compounds from natural matrices. In this work, the use of PLE is explored to obtain bioactive extracts from Tannat grape pomace rich in phenolic compounds presenting high antioxidant and anticholinergic activities. After optimization, the best extraction conditions implied the use of 55 % ethanol as a solvent at 141 °C for 20 min. Moreover, to correlate the observed bioactivities with the particular chemical composition of the extracts, a new two-dimensional comprehensive liquid chromatography (LC × LC) method coupled to mass spectrometry (MS) was developed to separate and identify the components present in the extract. The LC × LC analysis of the optimum extract separated >70 different analytes. Among them, proanthocyanidins were the most abundant phenolic compounds, although others such as flavonols and anthocyanins could also be identified. Overall, the obtained results demonstrate the strong potential of Tannat grape pomace to be valorized, retaining excellent possibilities for application in different fields.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1754 ","pages":"Article 466030"},"PeriodicalIF":3.8,"publicationDate":"2025-05-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143943625","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

A 3D printed cryogenic device for gas chromatography: Design, and performance demonstrated for multidimensional and enantioselective separations 一种用于气相色谱的3D打印低温装置：多维和对映选择性分离的设计和性能证明

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-05-08 DOI: 10.1016/j.chroma.2025.466017

Ian A. Wittman , Tom Jarvis , Milton T.W. Hearn , Philip J. Marriott

{"title":"A 3D printed cryogenic device for gas chromatography: Design, and performance demonstrated for multidimensional and enantioselective separations","authors":"Ian A. Wittman , Tom Jarvis , Milton T.W. Hearn , Philip J. Marriott","doi":"10.1016/j.chroma.2025.466017","DOIUrl":"10.1016/j.chroma.2025.466017","url":null,"abstract":"<div><div>This paper describes the development of a device 3D printed using stainless steel that is intended to operate as a cold trapping assembly when cooled by liquid CO<sub>2</sub>, in a manner similar to a longitudinally modulated cryogenic system (LMCS). The cold trap enclosure design is detailed, and the system's performance is tested to assess its suitability for use as a collection and rapid re-mobilisation device for gas chromatography analysis of volatile organic compounds (VOC). Precision of modulation period timing was evaluated, showing a maximum error of 8 μs and an average variation of <1 ns across 10,000 successive modulations. The system's trapping capabilities were tested using an alkane series (C<sub>5</sub>-C<sub>9</sub>), successfully trapping all analytes and producing peaks with full width at half height (FWHH) as low as 65 ms. Maximum trapping time was assessed for hexane, with the modulator retaining the compound for up to 9 s in a 100 °C oven before breakthrough was observed. The modulator was then applied to investigate enantioselective separation of limonene. Whilst a single chiral column was used, various lengths (20 cm – 5.0 m) of column were drawn through the modulator, where these lengths effectively function as enantioselective second dimension (<sup>2</sup>D) columns. Injected (<em>R,S</em>)-limonene enantiomers were collected as a single entity, then rapidly released to the <sup>2</sup>D column. Comprehensive two-dimensional gas chromatography was demonstrated to be viable using the 3D printed modulator for a tea tree oil sample.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1754 ","pages":"Article 466017"},"PeriodicalIF":3.8,"publicationDate":"2025-05-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143936884","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

Ultra-fast and selective extraction of phenolic acids by multifunctional and magnetic nanomaterials in honeysuckle 多功能磁性纳米材料超快速选择性提取金银花中酚酸

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-05-07 DOI: 10.1016/j.chroma.2025.466028

Jianhui Dong , Xiaoyi Chen , Chenyang Wang , Xiaolong Yao , Juanjuan Zhao , Shengxiang Zhang , Yating Shi , Junjie Ou , Ruixia Gao , Nan Deng , Yangyang Bian

{"title":"Ultra-fast and selective extraction of phenolic acids by multifunctional and magnetic nanomaterials in honeysuckle","authors":"Jianhui Dong , Xiaoyi Chen , Chenyang Wang , Xiaolong Yao , Juanjuan Zhao , Shengxiang Zhang , Yating Shi , Junjie Ou , Ruixia Gao , Nan Deng , Yangyang Bian","doi":"10.1016/j.chroma.2025.466028","DOIUrl":"10.1016/j.chroma.2025.466028","url":null,"abstract":"<div><div>Novel multifunctional magnetic nanomaterials were developed for ultra-fast and selective extraction of phenolic acids across a wide pH range. The magnetic core was firstly coated with SiO<sub>2</sub>, followed by surface modification with 4-vinylphenylboronic acid (VPBA), 1-vinylimidazole (VI) and methacrylamido propyl trimethyl ammonium chloride (MAPTAC) as functional monomers. The characterization, repeatability, adsorption kinetics, and adsorption isotherms were investigated, and five different phenolic acids were used to demonstrate its selectivity. A maximum adsorption capacity of 86.58 mg/g was determined by the Langmuir adsorption model. The limits of detection and quantification of the method were 0.01 μg/mL and 0.04 μg/mL, respectively. The experimental results exhibited that the resultant multifunctional nanomaterials had satisfactory magnetic property, fast kinetics, favorable adsorption capacity, excellent specificity and higher repeatability. The Fe<sub>3</sub>O<sub>4</sub>@MPS-SPE exhibited ultra-fast kinetics with a complete adsorption of 2 s and a wide pH range of 3∼8. The multifunctional magnetic nanomaterials were successfully used as sorbents for selective extraction of phenolic acids in honeysuckle.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1755 ","pages":"Article 466028"},"PeriodicalIF":3.8,"publicationDate":"2025-05-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144068108","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

Supercritical fluid CO2 extraction followed by polystyrene/divinylbenzene stationary phase complementary supercritical fluid chromatography and reversed-phase liquid chromatography separation of unsaturated fatty acids 超临界流体CO2萃取-聚苯乙烯/二乙烯基苯固定相互补-超临界液相色谱-反相液相色谱分离不饱和脂肪酸

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-05-07 DOI: 10.1016/j.chroma.2025.466029

Yingying Tong, Qilan Wang, Jun Dang

{"title":"Supercritical fluid CO2 extraction followed by polystyrene/divinylbenzene stationary phase complementary supercritical fluid chromatography and reversed-phase liquid chromatography separation of unsaturated fatty acids","authors":"Yingying Tong, Qilan Wang, Jun Dang","doi":"10.1016/j.chroma.2025.466029","DOIUrl":"10.1016/j.chroma.2025.466029","url":null,"abstract":"<div><div>Supercritical fluid chromatography (SFC) has emerged as a powerful separation technique with extensive applications in pharmaceutical analysis, environmental monitoring, and food safety testing. In this study, weakly polar unsaturated fatty acids were successfully extracted and separated via a polystyrene/divinylbenzene (PS-DVB) stationary phase complementary supercritical fluid chromatography and reversed-phase liquid chromatography (RPLC) approach. The weakly polar sample was obtained using supercritical fluid extraction (SFE) of <em>Floccularia luteovirens</em> powder. The extracted weakly polar sample was first separated using a PS-DVB stationary phase SFC, yielding 304.7 mg of the target fraction Fr2. Then, the established complementary SFC and RPLC method was applied to the separation and purification of compounds from the target fraction Fr2. Finally, three unsaturated fatty acids with purities exceeding 95 % were successfully prepared. This approach has significant potential for analyzing and purifying weakly polar natural products on the same stationary phase using SFC and RPLC.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1754 ","pages":"Article 466029"},"PeriodicalIF":3.8,"publicationDate":"2025-05-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143929184","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

Multi-response optimization and validation analysis in the detection of acetochlor and butachlor by HPLC based on D-optimal design methodology 基于d -最优设计的高效液相色谱法检测乙草胺和丁草胺的多响应优化及验证分析

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-05-06 DOI: 10.1016/j.chroma.2025.466025

Yu Wang , Yang Yang , Si Zhang , Chao Chi , Bohan Wang , Junfeng Su

{"title":"Multi-response optimization and validation analysis in the detection of acetochlor and butachlor by HPLC based on D-optimal design methodology","authors":"Yu Wang , Yang Yang , Si Zhang , Chao Chi , Bohan Wang , Junfeng Su","doi":"10.1016/j.chroma.2025.466025","DOIUrl":"10.1016/j.chroma.2025.466025","url":null,"abstract":"<div><div>Acetochlor and butachlor, widely used herbicides, pose environmental and health risks through water contamination. This study developed a high-performance liquid chromatography (HPLC) method for analyzing these compounds, employing a multi-response approach and D-optimal design. The D-optimal design reduced the number of required experiments from 36 to 14. The response model was analyzed by variance and residual diagnosis, and a multi-response optimization process was implemented to minimize the retention time and maximize the peak area of the two analytes. The optimal conditions were determined: a column temperature of 30 °C, a mobile phase composition of 80:0:20 (CH<sub>3</sub>OH:CH<sub>3</sub>CN:H<sub>2</sub>O) by volume, a flow rate of 0.9 mL min<sup>-1</sup>, an injection volume of 25 μL, and a detection wavelength of 215 nm. The method achieved complete separation of acetochlor and butachlor within 10 min. The detection limits were 0.0018 mg L<sup>−1</sup> for acetochlor and 0.01 mg L<sup>−1</sup> for butachlor, with quantitation limits of 0.009 mg L<sup>−1</sup> and 0.06 mg L<sup>−1</sup>, respectively. The linear ranges extended from 0.009 to 9 mg L<sup>−1</sup> for acetochlor and 0.06 to 15 mg L<sup>−1</sup> for butachlor, with a correlation coefficient (R<sup>2</sup>) of 0.9998, indicating excellent linearity. The recoveries ranged from 98.36 % to 103.13 % for acetochlor and 80.30 % to 107.74 % for butachlor, with the relative standard deviations both below 2 % (<em>n</em> = 6). This accurate, rapid, and sensitive method is well-suited for quantitative detection of these herbicides in water. It also serves as an invaluable reference for analyzing structurally similar chloroacetamide herbicides using HPLC.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1754 ","pages":"Article 466025"},"PeriodicalIF":3.8,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143929187","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

Comprehensive analysis of mandarin essential oils: Simultaneous qualitative, quantitative, chiral, and isotopic profiling via enantio-selective multidimensional gas chromatography coupled to isotopic ratio mass spectrometry

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-05-06 DOI: 10.1016/j.chroma.2025.466026

Francesca Cannizzaro , Lorenzo Cucinotta , Elisa Irrera , Paolo Oliveri , Tania Maria Grazia Salerno , Danilo Sciarrone , Luigi Mondello

{"title":"Comprehensive analysis of mandarin essential oils: Simultaneous qualitative, quantitative, chiral, and isotopic profiling via enantio-selective multidimensional gas chromatography coupled to isotopic ratio mass spectrometry","authors":"Francesca Cannizzaro , Lorenzo Cucinotta , Elisa Irrera , Paolo Oliveri , Tania Maria Grazia Salerno , Danilo Sciarrone , Luigi Mondello","doi":"10.1016/j.chroma.2025.466026","DOIUrl":"10.1016/j.chroma.2025.466026","url":null,"abstract":"<div><div>The current study aimed to provide a comprehensive analytical profile of the volatile fraction of sixty-three genuine mandarin essential oil (EO) samples, by exploiting a single instrument. For this purpose, a novel analytical approach was implemented, based on a heart-cut enantio‑selective multidimensional gas chromatographic system coupled in parallel to an isotopic ratio mass spectrometer and a single quadrupole mass spectrometer (Es-MDGC<img>C-IRMS/qMS). For the first time, the stand-by analysis in the first dimension, usually employed to transfer target compounds to the second dimension, was here utilized to perform quali-quantitative analyses. Furthermore, the second dimension, equipped with a chiral stationary phase and coupled to a qMS and an IRMS, allowed the simultaneous evaluation of selected target components' chiral and carbon isotopic ratios. To the best of the Authors' knowledge, this research reports for the first time the <em>δ</em>¹³C values of specific enantiomers in mandarin EOs. The data gathered from Es-MDGC<img>C-IRMS/qMS analyses revealed clear seasonal and geographical trends, while chemometric investigation confirmed the validity of the results obtained. This method allowed us to overcome the limitations associated with a monodimensional GC approach, while substantially reducing total analysis time, energy use, solvent consumption, and waste production, making it a powerful tool for authenticity assessment.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1754 ","pages":"Article 466026"},"PeriodicalIF":3.8,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143943494","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

Supercritical fluid chromatography versus high-performance liquid chromatography – Performance, robustness and selectivity in the separation of vitamin A acetate and related substances 超临界流体色谱法与高效液相色谱法。分离维生素A醋酸酯及相关物质的性能、稳健性和选择性

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-05-05 DOI: 10.1016/j.chroma.2025.466021

Mo Legelli , Philipp Otzen , Max Eberle , Michaela Wirtz , Stefan Lamotte

{"title":"Supercritical fluid chromatography versus high-performance liquid chromatography – Performance, robustness and selectivity in the separation of vitamin A acetate and related substances","authors":"Mo Legelli , Philipp Otzen , Max Eberle , Michaela Wirtz , Stefan Lamotte","doi":"10.1016/j.chroma.2025.466021","DOIUrl":"10.1016/j.chroma.2025.466021","url":null,"abstract":"<div><div>This study presents the separation of vitamin A acetate (VAA) and other retinoids, as well as their respective stereoisomeric forms, with the help of supercritical fluid chromatography (SFC). The basis for this was a method of reversed-phase high-performance liquid chromatography (HPLC), presented by Schräder <em>et al</em>. (2024). There, the separation of retinoids and VAA stereoisomers was performed on a Chiralpak IG-3 chiral stationary phase and the retention mechanism was investigated via van ‘t Hoff experiments. The presented study aimed for method transfer to SFC and the comparison to HPLC in terms of robustness and selectivity. During the initial method development, peak deformations were observed and investigated with systematic alterations of the chromatographic conditions to find the limits of a robust separation. It was found that the proper desorption of analytes is only possible above a certain system pressure threshold, meaning a robust method required a minimum elution strength of the mobile phase. Comparison of both methods revealed differences in terms of selectivity. Most notable was a reversal in retention order for the retinoids based on their polarity, but not of the stereoisomers within the retinoid groups. With the help of van ‘t Hoff experiments, it was concluded that the separation mode of SFC was more akin to normal-phase, with the non-polar retinoids eluting before the polar retinoids. At the same time, the plots confirmed that the molecular shape recognition capabilities of the utilised stationary phase also applied to the SFC separation of the respective isomers.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1754 ","pages":"Article 466021"},"PeriodicalIF":3.8,"publicationDate":"2025-05-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143929186","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

Rapid processing of liquid chromatography mass spectrometry data for compound screening and characterization in complex matrix based on python: with Meconopsis quintuplinervia Regel as an example 基于python的复杂矩阵中化合物筛选与表征的液相色谱质谱数据快速处理——以绿毛蒿（Meconopsis quintuplinervia Regel）为例

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-05-05 DOI: 10.1016/j.chroma.2025.466022

Jiahao Yang , Xialin Zhu , Le Li , Fan Yang , Zhixin Tang , Haiqiang Jiang

{"title":"Rapid processing of liquid chromatography mass spectrometry data for compound screening and characterization in complex matrix based on python: with Meconopsis quintuplinervia Regel as an example","authors":"Jiahao Yang , Xialin Zhu , Le Li , Fan Yang , Zhixin Tang , Haiqiang Jiang","doi":"10.1016/j.chroma.2025.466022","DOIUrl":"10.1016/j.chroma.2025.466022","url":null,"abstract":"<div><div>Herbal extracts are time-consuming and laborious to analyse by traditional methods due to the complexity of their composition. Therefore, it is necessary to develop a rapid identification tool. In this study, a mass spectrometry data processing workstation was designed based on python language, which can rapidly screen and comprehensively characterize the components of herbal medicines. The main steps are as follows: (1) data acquisition by ultra-high-performance liquid chromatography coupled with Q-Exactive MS/MS (UPLC-QE-MS/MS); (2) conversion of mass spectrometry raw data file format and collection of key information; (3) enumeration of permutations and combinations of core structures and substituents based on the structural features of common flavonoids, and establishment of a database of precursor ions. (4) matching precursor ions from mass spectrometry data to a database and labeling mass spectrometry fragment ions based on structural information provided by the database;(5) establishment of a rating system for evaluating compound combinations based on mass spectrometry fragmentation information; (6) information on combinations of highly rated compounds was collected, analyzed for retention times and ionic behavior, and compared with online databases for further structural confirmation. Taking <em>Meconopsis quintuplinervia Regel</em> as an example, 140 flavonoids were finally preliminarily characterized. The results showed that the collection and identification of mass spectrometry information with the help of the mass spectrometry data processing workstation is fast and effective, and can be used for the rapid screening and characterization of compounds in traditional Chinese medicine or other complex matrix.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1753 ","pages":"Article 466022"},"PeriodicalIF":3.8,"publicationDate":"2025-05-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143917325","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

Comprehensive two-dimensional liquid chromatographic analysis of Cannabis phenolics and first evidence of flavoalkaloids in Cannabis 大麻酚类物质的综合二维液相色谱分析和大麻中黄酮类生物碱的首个证据

IF 3.8 2区化学

Journal of Chromatography A Pub Date : 2025-05-05 DOI: 10.1016/j.chroma.2025.466023

Magriet Muller, André de Villiers

{"title":"Comprehensive two-dimensional liquid chromatographic analysis of Cannabis phenolics and first evidence of flavoalkaloids in Cannabis","authors":"Magriet Muller, André de Villiers","doi":"10.1016/j.chroma.2025.466023","DOIUrl":"10.1016/j.chroma.2025.466023","url":null,"abstract":"<div><div><em>Cannabis</em> contains a large number of diverse metabolites. Compared to the well-studied cannabinoids and terpenoids, characterization of the phenolic composition of <em>Cannabis</em> has received little attention. With studies reporting synergistic effects in <em>Cannabis</em>, the importance of investigating polyphenols in <em>Cannabis</em> is becoming more apparent. We report an on-line comprehensive 2D HILIC × RP-LC method hyphenated to high resolution (HR) MS for the detailed characterization of polar phenolics in <em>Cannabis</em> inflorescence and leaf samples of three commercial strains. Optimal HILIC × RP-LC conditions were derived using an automated method optimization program, and provided excellent separation performance (peak capacity > 3000) and high orthogonality. Diode array and HR-MS data enabled tentative identification of 79 compounds, comprising mainly flavone and (hydroxy)cinnamic acid derivatives. Compound assignment was facilitated by the group-type separation obtained between the phenolic acids and flavonoids, as well as the structured elution patterns for the flavone glycosides. The presence of three <em>C</em>-glycosylated flavones, as well as several of their <em>O</em>-glycosylated derivatives, distinguished one of the strains from the other two. In the same strain, flavoalkaloids were detected, mainly in the leaf extracts. The structures of the alkaloid moieties could not be unambiguously assigned based on the available HR-MS data, but four classes of flavoalkaloids comprising 16 flavone derivates could be tentatively identified. This is the first time that this relatively rare and chemically interesting class of compounds has been detected in <em>Cannabis</em>. These findings highlight the diversity of <em>Cannabis</em>, and the utility of HILIC × RP-LC-HR-MS for the in-depth study of its phenolic composition.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1754 ","pages":"Article 466023"},"PeriodicalIF":3.8,"publicationDate":"2025-05-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143936828","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