Journal of Chromatography A最新文献

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Development of a SnO2-based 44Ti/44Sc generator for medical applications 开发基于二氧化锡的 44Ti/44Sc 医疗应用发生器。
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2024-08-08 DOI: 10.1016/j.chroma.2024.465245
{"title":"Development of a SnO2-based 44Ti/44Sc generator for medical applications","authors":"","doi":"10.1016/j.chroma.2024.465245","DOIUrl":"10.1016/j.chroma.2024.465245","url":null,"abstract":"<div><p>Towards application of <sup>44</sup>Sc for diagnostic nuclear medicine, a <sup>44</sup>Ti/<sup>44</sup>Sc generator based on an inorganic resin has been evaluated. Unlike other radionuclide generators used for medical applications, the long-term retention of the parent <sup>44</sup>Ti is vital due to its long half life. Herein, tin dioxide (SnO<sub>2</sub>), a robust inorganic-based resin, has been synthesized and used as the stationary phase for a <sup>44</sup>Ti/<sup>44</sup>Sc generator. The sorption behavior of <sup>44</sup>Ti/<sup>44</sup>Sc was tested on SnO<sub>2</sub> with varying acids, concentrations, and times. Preliminary batch study results showed &gt;88 % <sup>44</sup>Ti retention to the resin at lower acid concentrations (0.05 M HNO<sub>3</sub> and 0.05 M HCl). A pilot generator was evaluated for a year, demonstrating 85.3 ± 2.8 % <sup>44</sup>Sc elution yields and 0.71 ± 0.14 % <sup>44</sup>Ti breakthrough in 5 M HNO<sub>3</sub>. Based on capacity studies, a 7.4 MBq (200 µCi) upscaled generator system was constructed for further evaluation of the SnO<sub>2</sub> resin stability and the efficacy of the eluted <sup>44</sup>Sc for radiolabeling. <sup>44</sup>Sc could be regularly eluted from this generator in 5 M HNO<sub>3</sub> with an overall average radiochemical yield 84.7 ± 9.5 %. Post-elution processing of the <sup>44</sup>Sc with DGA-normal resin removed all <sup>44</sup>Ti present and allowed for high <sup>44</sup>Sc-DOTA labeling yields of 94.2 ± 0.5 %. Overall, SnO<sub>2</sub> has been shown to be a viable material for a <sup>44</sup>Ti/<sup>44</sup>Sc generator.</p></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-08-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141974679","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
Structural elucidation of Sulodexide with multidimensional chromatography and online in-source acid-induced dissociation mass spectrometry 利用多维色谱法和在线源内酸诱导解离质谱法阐明舒洛地特的结构
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2024-08-08 DOI: 10.1016/j.chroma.2024.465242
{"title":"Structural elucidation of Sulodexide with multidimensional chromatography and online in-source acid-induced dissociation mass spectrometry","authors":"","doi":"10.1016/j.chroma.2024.465242","DOIUrl":"10.1016/j.chroma.2024.465242","url":null,"abstract":"<div><p>Sulodexide, a heparinoid medicine, is wildly used in clinic for prophylaxis and treatment of thromboembolic diseases and diabetic nephropathy. Despite its widespread use, the structure of Sulodexide remains poorly understood. It consists of various polysaccharides characterized by differing sugar compositions, linkages, and sulfonation patterns, yet they share common features such as strong hydrophilicity, high native charges, and considerable polydispersity, posing significant challenges for conventional chromatographic and online mass spectrometry (MS) characterization. In this work, a novel analytical method combining multiple-heart cut 2D-LC and in-source acid-induced dissociation (inAID) MS was developed. Three polysaccharides in Sulodexide were separated by high efficient strong-anion-exchange chromatography, followed by desalting with the second dimensional size-exclusion chromatography before MS. A novel MS strategy employing inAID technique was utilized for online analysis, leading to the initial identification of Sulodexide polysaccharide components. The results were validated through disaccharide composition analysis of those three polysaccharide components after offline preparation. This advanced strategy, merging various techniques, enable a comprehensive structural elucidation of such complex drugs and provides a viable tool for potential routine analysis of complex biomolecules.</p></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-08-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141997766","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 novel ultra-high-performance supercritical fluid chromatography hyphenated to tandem mass spectrometry method for the analysis of urinary endogenous steroids in the anti-doping context 一种新型超高效超临界流体色谱-串联质谱法,用于分析反兴奋剂背景下的尿液内源性类固醇
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2024-08-08 DOI: 10.1016/j.chroma.2024.465224
{"title":"A novel ultra-high-performance supercritical fluid chromatography hyphenated to tandem mass spectrometry method for the analysis of urinary endogenous steroids in the anti-doping context","authors":"","doi":"10.1016/j.chroma.2024.465224","DOIUrl":"10.1016/j.chroma.2024.465224","url":null,"abstract":"<div><p>The first step in the detection of testosterone (T) doping is to measure the urinary steroid profile for the athlete biological passport (ABP). To harmonise the analysis between anti-doping laboratories, urinary steroid profiling is parametrised in deep detail and shall be performed by gas chromatography hyphenated to mass spectrometry (GC–MS). However, due to its requirement for extensive sample preparation, alternatives to GC–MS are being actively pursued. The aim of this study was the evaluation of Ultra-High-Performance Supercritical Fluid Chromatography hyphenated to tandem Mass Spectrometry (UHPSFC-MS/MS) as an alternative for the quantification of endogenous urinary steroids. In this context, we developed a high throughput sample extraction method, followed by a novel UHPSFC-MS/MS method for the analysis of 10 endogenous urinary steroids which are relevant for doping control analysis. Depending on the steroid, the herein presented method is capable of quantification from 0.5 ng/mL up to 10 µg/mL. After validation, the applicability of the method was evaluated by analysing 132 authentic urine samples, which demonstrated results similar to classical GC–MS analysis. Steroid concentrations determined by UHPSFC-MS/MS were slightly overestimated in comparison with GC–MS, but the ratios had &lt;10 % difference between the two methods. As the ABP considers the steroid ratios for passport evaluation, the herein presented method could be used for steroid profiling without reducing the sensitivity of the ABP. Thus, we would propose to consider UHPSFC-MS/MS as an alternative to GC–MS after more tests would have been performed to support our findings. Furthermore, we have also investigated the potential of this technology for sample purification prior to Isotope Ratio Mass Spectrometry (IRMS) for the differentiation between exogenous and endogenous origin of T and its metabolites. While the achieved separation was sufficient to purify urine samples for IRMS analysis in our proof-of-concept study, the instrumental parameters should be further refined for future use.</p></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-08-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S0021967324005983/pdfft?md5=26f14cef50f65a6973e35cb25674c4ad&pid=1-s2.0-S0021967324005983-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142076871","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Cryogenic-zone-compression gas chromatography-mass spectrometry for the determination of 16 polycyclic aromatic hydrocarbons in extra virgin olive oil 低温区压缩气相色谱-质谱法测定特级初榨橄榄油中的 16 种多环芳烃。
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2024-08-08 DOI: 10.1016/j.chroma.2024.465248
{"title":"Cryogenic-zone-compression gas chromatography-mass spectrometry for the determination of 16 polycyclic aromatic hydrocarbons in extra virgin olive oil","authors":"","doi":"10.1016/j.chroma.2024.465248","DOIUrl":"10.1016/j.chroma.2024.465248","url":null,"abstract":"<div><p>The present study is based on the development of a straightforward method for the determination (semi-quantification) of 16 polycyclic aromatic hydrocarbons (PAHs) in extra virgin olive oil (EVOO) using \"cryogenic-zone-compression\" (CZC) gas chromatography-single quadrupole mass spectrometry (GC-QMS). The use of CZC (through a loop-type cryogenic modulator) to achieve enhanced signal-to-noise ratios (<em>s/n</em>), enabled a simplification of the sample preparation step. In fact, a single extraction process (using only 500 µL of acetonitrile) was performed prior to injection. The CZC GC-QMS method aligns with the principles of green analytical chemistry, and enabled an average <em>s/n</em> increase of 14-fold compared to conventional GC-QMS.</p><p>The method limits of quantification were in the 0.07–8.33 µg kg<sup>−1</sup> range. Accuracy (at the 2 μg kg<sup>−1</sup> and 10 μg kg<sup>−1</sup> concentration levels) was in the 82–103 % range. Intra-day and inter-day precision (at 2 μg kg<sup>−1</sup> and 10 μg kg<sup>−1</sup> concentration levels) were in the 1.9–14.7 % and 5.9–9.1 % ranges, respectively, while the recovery values (at 10 µg kg<sup>−1</sup>) ranged from 24 % to 99 %. For all the PAHs investigated, a positive matrix effect was observed. Two PAHs were detected (in the selected-ion-monitoring mode) in six EVOOs among the ten samples (not more than one PAH <em>per</em> sample).</p></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-08-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S0021967324006228/pdfft?md5=e04228daae76a1a98a89366597cd93f7&pid=1-s2.0-S0021967324006228-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141915754","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
A rapid and validated GC-MS/MS method for simultaneous quantification of serum Myo- and D-chiro-inositol isomers 一种快速有效的 GC-MS/MS 方法,用于同时定量检测血清肌醇和 D-chiro 肌醇异构体。
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2024-08-08 DOI: 10.1016/j.chroma.2024.465246
{"title":"A rapid and validated GC-MS/MS method for simultaneous quantification of serum Myo- and D-chiro-inositol isomers","authors":"","doi":"10.1016/j.chroma.2024.465246","DOIUrl":"10.1016/j.chroma.2024.465246","url":null,"abstract":"<div><h3>Background</h3><p><em>Myo</em>-inositol (MI) and D<em>-chiro</em>-inositol (DCI) are two paramount isomers of inositol, both vital in glucose and steroid metabolism. Deficits in MI, DCI or MI/DCI ratio are expressly concerned with several pathological process, whereas MI and DCI lack practical measurement for human specimen.</p></div><div><h3>Methods</h3><p>To quantify MI and DCI in serum samples simultaneously, a gas chromatography tandem mass spectrometry (GC-MS/MS) method was established. The process flow was optimized in ion source, derivative agent volume and reaction time. The performance characteristics were verified by commercial standards and clinical serums.</p></div><div><h3>Results</h3><p>This method was confirmed to be sensitive (LOD ≤ 30 ng/mL of MI, ≤3 ng/mL of DCI) and reproducible (RSD &lt; 6 % for repeated analyses). Quantitative determinations performed good linearity within the measurement range of 0.500–10.00 and 0.005–0.500 μg/mL for MI and DCI respectively (R<sup>2</sup> &gt; 0.999). The recoveries of MI and DCI were 97.11–99.35 % and 107.82–113.09 %, respectively. This method was successfully applied to 114 clinical specimens. No significant matrix effect was observed in serum samples under current conditions.</p></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-08-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141915752","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
Impact of photo-oxidation on long term storage of affinity chromatography media used in multi-specific antibody manufacturing processes 光氧化对长期储存多特异性抗体生产过程中使用的亲和层析介质的影响。
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2024-08-08 DOI: 10.1016/j.chroma.2024.465247
{"title":"Impact of photo-oxidation on long term storage of affinity chromatography media used in multi-specific antibody manufacturing processes","authors":"","doi":"10.1016/j.chroma.2024.465247","DOIUrl":"10.1016/j.chroma.2024.465247","url":null,"abstract":"<div><p>Large scale manufacture of complex biotherapeutic formats such as multi-specific antibodies can require development of custom biomanufacturing platforms, particularly for purification processes. Substantial advances in affinity chromatography media have allowed monoclonal antibody-like processes for these formats, and simplified process development to enable fast speed to the clinic. Thorough assessment of chromatography media performance and stability is critical to ensure robust operation and consistent product quality over repeated cycles throughout its lifetime. However, evaluation of repeated cycling and extended storage for chromatography media is resource consuming, which typically delays rigorous study to later development stages and often is acquired through increased operational experience. These areas can present quality risks if not properly understood. In this work, a class of affinity chromatography media employing camelid antibody-fragment ligands were evaluated for extended storage in benzyl alcohol solution as an alternative to ethanol storage. Initial laboratory studies revealed resin discoloration after 12 months of exposure to ambient light at room temperature. Resin photo-stress studies confirmed light exposure as the root cause, with benzyl alcohol storage conditions producing a substantially greater degree of discoloration compared to ethanol. Extreme photo-stress over the course of 7 days was also found to negatively impact resin dynamic binding capacities, with more severe declines observed with benzyl alcohol storage conditions. Binding capacity loss of 54 % was observed for photo-stressed CaptureSelect Kappa XP compared to control conditions. Addition of antioxidants reduced or eliminated resin discoloration during photo-stress, indicating that benzyl alcohol storage accelerates photo-oxidation of the affinity chromatography ligands. The addition of <span>l</span>-methionine to benzyl alcohol solution prevented resin discoloration and maintained a dynamic binding capacity of 41 g/L for CaptureSelect Kappa XP even after extreme photo-stress. Of practical importance, a study of LambdaFabSelect resin used and stored in benzyl alcohol solution, under recommended conditions (2–8 °C storage, protected from light) in an internal GMP facility over a period of three years, showed no impact to resin color, performance, or product quality.</p></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-08-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S0021967324006216/pdfft?md5=01c863fe9ce130a06c384547e127707e&pid=1-s2.0-S0021967324006216-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141915755","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Characterization and identification of the wide-polarity multicomponents from Prunella vulgaris by offline two-dimensional liquid chromatography and hydrophilic interaction chromatography coupled to ion mobility-quadrupole time-of-flight mass spectrometry 离线二维液相色谱和亲水作用色谱-离子淌度-四极杆飞行时间质谱联用技术表征和鉴定普鲁内拉中的宽极性多成分
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2024-08-08 DOI: 10.1016/j.chroma.2024.465233
{"title":"Characterization and identification of the wide-polarity multicomponents from Prunella vulgaris by offline two-dimensional liquid chromatography and hydrophilic interaction chromatography coupled to ion mobility-quadrupole time-of-flight mass spectrometry","authors":"","doi":"10.1016/j.chroma.2024.465233","DOIUrl":"10.1016/j.chroma.2024.465233","url":null,"abstract":"<div><p>Metabolites identification is crucial to develop functional foods or perform quality control. <em>Prunella vulgaris</em> (Xia-Ku-Cao) is a medicinal and edible plant used as the herbal medicine or main additive in functional beverage. However, current analytical strategies can only on-line characterize tens of compounds, restricted by insufficient chromatographic resolution and low coverage of the mass spectrometric scan methods. This work was designed to characterize the wide-polarity components from the ear of <em>P. vulgaris</em>. The total extract was fractionated by semi-preparative high-performance liquid chromatography into the retained medium-polarity fraction and unretained polar fraction, which were further analyzed by offline two-dimensional liquid chromatography (2D-LC) and hydrophilic interaction chromatography, respectively. Data-independent high-definition MS<sup>E</sup> of the Vion™ ion mobility time-of-flight mass spectrometer was utilized enabling the high-coverage acquisition of collision-induced dissociation-MS<sup>2</sup> data. The offline 2D-LC, configuring the XBridge Amide and HSS T3 columns, gave high orthogonality (0.81) and effective peak capacity (1555). Automatic peak annotation facilitated by the UNIFI™ bioinformatics platform and comparison with 62 reference compounds achieved the efficient and more reliable structural elucidation. We could characterize 255 compounds from <em>P. vulgaris</em>, with numerous phenylpropanoid phenolic acids and triterpenoid <em>O</em>-glycosides newly reported. Especially, collision cross section (CCS) prediction and targeted isolation of three compounds assisted in the identification of 39 groups of isomers. Additionally, 17 hydrophilic compounds, involving oligosaccharides and organic acids, were characterized from the unretained polar fraction<em>.</em> Conclusively, the in-depth metabolites identification of <em>P. vulgaris</em> was accomplished, and the results can benefit the development and better quality control of this valuable plant.</p></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-08-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141979925","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
Integrated supercritical fluid extraction of essential oils 综合超临界流体萃取精油
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2024-08-07 DOI: 10.1016/j.chroma.2024.465240
{"title":"Integrated supercritical fluid extraction of essential oils","authors":"","doi":"10.1016/j.chroma.2024.465240","DOIUrl":"10.1016/j.chroma.2024.465240","url":null,"abstract":"<div><p>Supercritical fluid extraction (SFE) stands out as an incredibly efficient, environmentally conscious, and fast method for obtaining essential oils (EOs) from plants. These EOs are abundant in aromatic compounds that play a crucial role in various industries such as food, fragrances, cosmetics, perfumery, pharmaceuticals, and healthcare. While there is a wealth of existing literature on using supercritical fluids for extracting plant essential oils, there's still much to explore in terms of combining different techniques to enhance the SFE process. This comprehensive review presents a sophisticated framework that merges SFE with EO extraction methods. This inclusive categorization encompasses a range of methods, including the integration of pressurized liquid processes, ultrasound assistance, steam distillation integration, microfluidic techniques, enzyme integration, adsorbent facilitation, supercritical antisolvent treatments, molecular distillation, microwave assistance, milling process and mechanical pressing integration. Throughout this in-depth exploration, we not only elucidate these combined techniques but also engage in a thoughtful discussion about the challenges they entail and the array of opportunities they offer within the realm of SFE for EOs. By dissecting these complexities, our objective is to tackle the current challenges associated with enhancing SFE for commercial purposes. This endeavor will not only streamline the production of premium-grade essential oils with improved safety measures but also pave the way for novel applications in various fields.</p></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-08-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141997764","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
The Series of L-lysine-Derived Gelators-Modified Multifunctional Chromatography Stationary Phase for Separation of Chiral and Achiral Compounds 用于分离手性和非手性化合物的 L-赖氨酸衍生凝胶剂改性多功能色谱固定相系列。
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2024-08-07 DOI: 10.1016/j.chroma.2024.465228
{"title":"The Series of L-lysine-Derived Gelators-Modified Multifunctional Chromatography Stationary Phase for Separation of Chiral and Achiral Compounds","authors":"","doi":"10.1016/j.chroma.2024.465228","DOIUrl":"10.1016/j.chroma.2024.465228","url":null,"abstract":"<div><p>In this study, using chiral L-lysine as the molecular skeleton, three kinds of L-lysine-derived gelators (G<sub>BLB</sub>, G<sub>BLF</sub> and G<sub>FLF</sub>) were synthesized and then bonded to the surface of silica matrix (5 μm) by amide condensation to prepare a series of multifunctional chromatography stationary phases (G<sub>BLB</sub>-SiO<sub>2</sub>, G<sub>BLF</sub>-SiO<sub>2</sub>, and G<sub>FLF</sub>-SiO<sub>2)</sub> were prepared. The L-lysine-derived gelators not only possess chiral recognition ability, but also can spontaneously form oriented and ordered network structures in liquid medium through the interaction of non-covalent bonding forces such as hydrogen bonding, π-π stacking, and van der Waals forces. The comprehensive effect of multiple weak interaction sites enhances the molecular recognition ability and further improves the separation diversity of different types of compounds on stationary phases. The separation and evaluation of chiral compounds showed that benzoin, 1-phenyl-ethanol, 1-phenyl-propanol and 6-hydroxyflavanone could be separated in normal phase mode (NPLC). The separation of different types of non-chiral compounds, such as sulfonamides, nucleosides, nucleobases, polycyclic aromatic hydrocarbons (PAHs), anilines, and aromatic acids, were achieved in hydrophilic interaction/reversed-phase/ion-exchange mode (HILIC/RPLC/IEC), and the separation of polarized compounds could be performed under the condition of ultrapure water as the mobile phase, which has the typical retention characteristics of per aqueous liquid chromatography (PALC). The effects of organic solvent content, temperature, pH value, and buffer salt concentration on the retention and separation performance of the column were investigated. Comparison of the three prepared columns showed that the separation performance (such as aromatic selectivity) could be improved by increasing the types of functional groups on the surface of the stationary phase and the number of aromatic groups. In a word, the prepared stationary phase have multiple retention properties, can simultaneously separate chiral compounds and various types of achiral compounds. This work provides an idea for developing multifunctional liquid chromatography stationary phase materials, and further expands the application of gelators in separation science.</p></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-08-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142008029","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
Comparative analysis of additive decomposition using one-dimensional and two-dimensional gas chromatography: Part I - Irganox 1010, Irganox 1076, and BHT 使用一维和二维气相色谱法对添加剂分解进行比较分析:第一部分 - Irganox 1010、Irganox 1076 和 BHT。
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2024-08-07 DOI: 10.1016/j.chroma.2024.465243
{"title":"Comparative analysis of additive decomposition using one-dimensional and two-dimensional gas chromatography: Part I - Irganox 1010, Irganox 1076, and BHT","authors":"","doi":"10.1016/j.chroma.2024.465243","DOIUrl":"10.1016/j.chroma.2024.465243","url":null,"abstract":"<div><p>Plastics incorporate diverse additives, including primary antioxidants with a typical amount between 0.05 to 3 wt.%, to enhance plastics functionality and durability, preventing their oxidation and maintaining their mechanical properties. While these antioxidants offer substantial benefits, their degradation can significantly impact plastic pyrolysis by changing the pyrolysis oil product distribution. Understanding the intricate distribution of decomposition products resulting from pyrolysis is essential yet often overlooked. This study delved into the analysis of the decomposition of common primary antioxidants, namely, Irganox 1010, Irganox 1076, and butylated hydroxytoluene (BHT), utilizing both one–dimensional gas chromatography coupled with a quadruple mass spectrometer (GC–MS) and two–dimensional gas chromatography equipped with flame ionization detector and time–of–flight mass spectrometer (GC×GC–FID/TOF–MS). This study showed that GC×GC–FID/TOF–MS provided a more detailed characterization of the pyrolysis product distribution of primary antioxidants used in plastics in comparison to GC–MS. For each of the antioxidants, using the GC×GC–FID/TOF–MS analytical approach enhanced the identification of degradation products at least fivefold. Furthermore, GC×GC–FID/TOF–MS identified products of more chemical classes than GC–MS. For instance, compounds from 14 chemical classes were identified from GC×GC–FID/TOF–MS in the pyrolysis of Irganox 1010, whereas only 9 chemical classes were identified in GC–MS. Olefins were the major chemical class for both Irganox 1010 and Irganox 1076 in the decomposition process, accounting for 23.25 wt.% and 20.76 wt.%, respectively. Ketones were the major chemical class in the case of BHT, having a 6.68 wt.% yield. This research enhanced the understanding of the decomposition of primary antioxidant and their product distribution during pyrolysis and shed light on the potential necessity for using two-dimensional gas chromatography.</p></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-08-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141915753","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
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