Gas chromatography

气相色谱法
  • 文章类型: Journal Article
    肠道微生物群及其代谢产物对动物的健康和生长发育至关重要。目前的研究表明,性别对肠道菌群的结构和功能有一定的影响,但是关于肠道微生物代谢产物的性别差异的报道很少,包括那些被阉割的雄性动物。本研究旨在探讨性别对海南特种野猪肠道微生物代谢产物的影响(10头公猪,10只母猪,和10只阉割的公猪,表示为EM,FE,和CM,分别)通过采用非靶向代谢组学和气相色谱法。共检测到1086种代谢物,在EM和FE之间观察到的差异代谢物数量最多(54种差异代谢物,包括18种上调和36种下调的代谢物),CM和FE之间最少(7种差异代谢物,包括1个上调和6个下调的代谢物),和CM和EM之间的中间数(47个差异代谢物,包括35种上调的代谢物和12种下调的代谢物)。差异代谢物参与EM和FE之间以及CM和EM之间的更多途径,包括氨基酸代谢和消化系统途径,而差异代谢物参与CM和FE之间最少的途径。相关分析显示,RuminocycaceaeUCG-009,未培养的_细菌_o_SAR324_cladeMarine_B组,和念珠菌糖藻属有助于产生代谢产物,如海藻糖,二十二碳三烯酸,D(-)-β-羟基丁酸,和乙酰-DL-亮氨酸。乙酸的含量,丙酸,丁酸,异丁酸,戊酸,EM和异戊酸明显高于FE,CM介于两者之间。链球菌,Lachnospileaceae_NK4A136_组和Rkenellaceae_RC9_gut_组与短链脂肪酸(SCFAs)的产生呈显着正相关,而[Eubacterium]_coprostanoligenies_组,未培养的_bacteria_f_p-251-o5和Ruminococaceae_UCG-005与SCFAs的产生呈显着负相关。这项研究为不同性别的海南特殊野猪的精确饲养策略提供了基础数据和重要见解,以及对动物肠道微生物代谢产物性别差异的研究。
    The intestinal microbiota and its metabolites are essential for the health and growth development of animals. Current research indicates that sex has a certain impact on the structure and function of the intestinal microbiota, but there are few reports on sex differences in intestinal microbiota metabolites, including those of castrated male animals. This study aimed to explore the impact of sex on the intestinal microbial metabolites of Hainan special wild boars (10 entire male pigs, 10 female pigs, and 10 castrated male pigs, denoted EM, FE, and CM, respectively) by employing non-targeted metabolomics and gas chromatography. A total of 1086 metabolites were detected, with the greatest number of differential metabolites observed between EM and FE (54 differential metabolites, including 18 upregulated and 36 downregulated metabolites), the fewest between CM and FE (7 differential metabolites, including 1 upregulated and 6 downregulated metabolites), and an intermediate number between CM and EM (47 differential metabolites, including 35 upregulated and 12 downregulated metabolites). Differential metabolites were involved in more pathways between EM and FE and between CM and EM, including amino acid metabolism and digestive system pathways, whereas differential metabolites were involved in the fewest pathways between CM and FE. Correlation analysis showed Ruminococcaceae UCG-009, uncultured_bacterium_o_SAR324_cladeMarine_group_B, and Candidatus Saccharimonas contributed to the production of metabolites such as trehalose, docosatrienoic acid, D(-)-beta-hydroxy butyric acid, and acetyl-DL-leucine. The levels of acetic acid, propionic acid, butyric acid, isobutyric acid, valeric acid, and isovaleric acid were significantly higher in EM than in FE, with CM falling between the two. Streptococcus, Lachnospiraceae_NK4A136_group and Rikenellaceae_RC9_gut_group showed a significant positive correlation with the production of short-chain fatty acids (SCFAs), while [Eubacterium]_coprostanoligenes_group, uncultured_bacterium_f_p-251-o5 and Ruminococcaceae_UCG-005 showed a significant negative correlation with the generation of SCFAs. This study provides foundational data and significant insights into precision feeding strategies for Hainan special wild boars of different sexes, as well as the study of sex differences in intestinal microbial metabolites in animals.
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  • 文章类型: Journal Article
    挥发性卤代烃(VHHs)每年产生并释放到环境中,对公众健康构成威胁。在这项研究中,一个简单的,快速,描述了基于顶空和电子捕获检测的气相色谱(GC)的灵敏自动化方法,用于测定水样中不同浓度水平的VHH。提出的顶空GC方法进行了初步优化,发现的最佳实验条件是将含有20%w/v氯化钠的10mL水样置于20mL小瓶中,并在60°C下搅拌35分钟,然后在DB-35MS毛细管柱上以12.5:1的分流比很好地分离了14个VHH。检出限在低μg/L水平,范围在0.01和0.6μg/L之间最后,将优化的方法应用于饮用水和环境水域中14种VHH的测定。自来水中VHHs的总平均浓度为34.962、26.183、3.228和647.344μg/L,纯净水与1年的滤芯,海水和废水,分别。然而,使用新的滤芯在纯净水中未检测到VHH。不同水基质的主要成分不同,这可能归因于它们的不同来源。
    Volatile halogenated hydrocarbons (VHHs) are annually produced and released into the environment, posing a threat to public health. In this study, a simple, rapid, sensitive and automated method based on headspace and gas chromatography (GC) with electron-capture detection was described for the determination of VHHs in different concentration levels in water samples. The proposed headspace GC method was initially optimized, and the optimum experimental conditions found were 10-mL water sample containing 20% w/v sodium chloride placed in a 20-mL vial and stirred at 60°C for 35 min, and then 14 VHHs were well separated on DB-35 MS capillary column with a split ratio of 12.5: 1. The limits of detection were in the low μg/L level, ranging between 0.01 and 0.6 μg/L. Finally optimized method was applied for determination 14 VHHs in drinking and environmental waters. The total mean concentrations of VHHs were 34.962, 26.183, 3.228 and 647.344 μg/L in tap water, purified water with 1-year-old filter element, seawater and effluents, respectively. However, no VHHs was detected in purified water with a new filter element. The main composition is different among different water matrix, which may be attributed to their different sources.
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  • 文章类型: Journal Article
    多环芳烃被认为对人类具有潜在的遗传毒性和致癌性。对于非吸烟人群,食物是多环芳烃接触的主要来源。由于它们的亲脂性,油脂是多环芳烃含量最高的食品之一。因此,食用油中多环芳烃的检测对促进人类健康至关重要。本文综述了样品预处理方法,例如基于液相的萃取方法,基于吸附剂的提取方法,和QuEChers(快,easy,便宜,有效,崎岖,和安全)方法,自2010年以来,结合质谱和基于色谱的检测技术,对食用油中的多环芳烃进行准确定量。概述本文讨论的方法的进展,加上对当前挑战和前景的评论,将指导研究人员重点开发更有效的检测方法和控制措施,以降低多环芳烃带来的潜在风险和危害。
    Polycyclic aromatic hydrocarbons are considered to be potentially genotoxic and carcinogenic to humans. For non-smoking populations, food is the main source of polycyclic aromatic hydrocarbons exposure. Due to their lipophilic nature, oils and fats rank among the food items with the highest polycyclic aromatic hydrocarbon content. Consequently, the detection of polycyclic aromatic hydrocarbons in edible oils is critical for the promotion of human health. This paper reviews sample pretreatment methods, such as liquid-phase-based extraction methods, adsorbent-based extraction methods, and the QuEChERS (quick, easy, cheap, effective, rugged, and safe) method, combined with detection techniques like mass spectrometry and chromatography-based techniques for accurate quantification of polycyclic aromatic hydrocarbons in edible oils since 2010. An overview on the advances of the methods discussed herein, along with a commentary addition of current challenges and prospects, will guide researchers to focus on developing more effective detection methods and control measures to reduce the potential risks and hazards posed by polycyclic aromatic hydrocarbons.
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  • 文章类型: Journal Article
    金属有机笼(MOCs),作为一种新兴的离散超分子化合物,在分离中受到了广泛的关注,生物医学,气体捕获,催化作用,和分子识别由于它们的孔隙度,可调性和稳定性。在这里,我们提出了一种新的手性MOCFeII4L4涂层毛细管柱,用于气相色谱(GC)分离不同类型的有机化合物,包括正构烷烃,n-醇,烷基苯,异构体,尤其是外消旋化合物。有20种不同的外消旋体(例如,酒精,醚,环氧化物,酯类,烯烃,和醛)在FeII4L4手性色谱柱上很好地拆分,1-苯基-1-丙醇的最大拆分值达到6.17。FeII4L4涂层的色谱柱显示出高的色谱柱效率(正十二烷3100板m-1)和良好的对映体拆分,与商业β-DEX120色谱柱和先前报道的手性MOC[Fe4L6](ClO4)8涂层柱互补。缩水甘油和硝基甲苯的峰面积和保留时间的相对标准偏差(RSD)低于1.2%。本研究揭示了手性MOCs在色谱分离中具有良好的应用前景。
    Metal organic cages (MOCs), as an emerging discrete supramolecular compounds, have received widespread attention in separation, biomedicine, gas capture, catalysis, and molecular recognition due to their porosity, adjustability and stability. Herein, we present a new chiral MOC FeII4L4 coated capillary column prepared for gas chromatographic (GC) separation of different types of organic compounds, including n-alkanes, n-alcohols, alkylbenzenes, isomers, especially for racemic compounds. There are 20 different kinds of racemates (e.g., alcohols, ethers, epoxides, esters, alkenes, and aldehydes) were well resolved on the FeII4L4 chiral column and a maximum resolution value for 1-phenyl-1-propanol reaches 6.17. The FeII4L4 coated column exhibited high column efficiency (3100 plates m-1 for n-dodecane) and good enantiomeric resolution complementary to that of a commercial β-DEX 120 column and the previously reported chiral MOC [Fe4L6] (ClO4)8 coated column. The relative standard deviation (RSDs) of the peak area and retention time of glycidol and nitrotoluene were below 1.2 %. This study reveals that chiral MOCs have good application prospects in chromatographic separation.
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  • 文章类型: Journal Article
    在这项工作中,开发了利用三维(3D)打印微型烘箱和柔性不锈钢毛细管柱的微芯片气相色谱(GC)柱组件。对程序集的性能和分离能力进行了表征。关键部件包括带有3米长的圆形螺旋通道的3D打印铝板(7.50×7.50×0.16厘米),作为烤箱,和色谱柱盘绕在通道上,内径为320μm,固定相为OV-1。将加热陶瓷板固定在板的相对侧上。该组件重40.3克。该设计允许轻松拆卸,或堆叠加热装置和柱子,使调整列长度的灵活性。当在140°C下使用n-C13作为测试分析物时,a保留因子(k)为8.5,获得7797板(2599板/m)。大会,采用电阻加热,证明了对含烷烃样品的有效分离性能,芳烃,醇和酮,具有良好的重现性。与烘箱加热相比,理论板的减少仅为2.95%。在C6至C18的沸点范围内,以119.512W的功耗实现了快速程序升温(120°C/min)。该组件成功地用于分离苯系列化合物,汽油和挥发性有机化合物(VOCs),表现出优异的分离性能。这种创新设计解决了制造工艺的复杂性和低可重复性以及与微芯片柱相关的高成本的挑战。此外,它的多功能性使其适用于户外分析应用。
    In this work, a microchip gas chromatography (GC) column assembly utilizing a three-dimensional (3D) printed micro oven and a flexible stainless steel capillary column was developed. The assembly\'s performance and separation capabilities were characterized. The key components include a 3D printed aluminum plate (7.50 × 7.50 × 0.16 cm) with a 3-meter-long circular spiral channel, serving as the oven, and the column coiled on the channel with an inner diameter of 320 μm and a stationary phase of OV-1. A heating ceramic plate was affixed on the opposite side of the plate. The assembly weighed 40.3 g. The design allows for easy disassembly, or stacking of heating devices and columns, enabling flexibility in adjusting column length. When using n-C13 as the test analyte at 140 °C, a retention factor (k) was 8.5, and 7797 plates (2599 plates/m) were obtained. The assembly, employing resistance heating, demonstrated effective separation performance for samples containing alkanes, aromatics, alcohols and ketones, with good reproducibility. The reduction in theoretical plates compared to oven heating was only 2.95 %. In the boiling point range of C6 to C18, rapid temperature programming (120 °C/min) was achieved with a power consumption of 119.512 W. The assembly was successfully employed to separate benzene series compounds, gasoline and volatile organic compounds (VOCs), demonstrating excellent separation performance. This innovative design addresses the challenges of the complexity and low repeatability of the fabrication process and the high cost associated with microchip columns. Furthermore, its versatility makes it suitable for outdoor analysis applications.
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  • 文章类型: Journal Article
    肉桂茶(RGT)是典型的武夷岩茶(WRT),以其浓郁的口感和多变的香气受到消费者的青睐。RGT的香气受到绿色制造过程的极大影响,但其机制尚不清楚。因此,在这项研究中,采摘了春季RGT的新鲜叶子,绿色制造(包括摇动和传播)和传播(不摇动),分别,在太阳枯萎后施用。然后,用GC-TOF-MS分析,这表明,丰富的挥发性化合物与鲜花和水果的香气,比如橙花醇,茉莉内酯,Jasmone,吲哚,己酸己酯,(E)-3-己烯基丁酸酯和乙酸1-己酯,在绿色制造的叶子中,显着高于散布的叶子。转录组和蛋白质组研究表明,长期的机械损伤和脱水可以激活与香气形成途径相关的基因的上调表达,但对蛋白表达的调控并不完全一致。绿色制造过程中的机械损伤更有利于正调节氧化丙二烯合酶(AOS)分支的α-亚麻酸代谢途径,其次是萜类化合物骨架生物合成的甲羟戊酸(MVA)途径,从而促进茉莉酸衍生物和倍半萜产物的合成。蛋白质相互作用分析表明,茉莉酸衍生物合成途径的关键蛋白为酰基辅酶A氧化酶(ACX),烯酰辅酶A水合酶(MFP2),OPC-8:0辅酶A连接酶1(OPCL1)等。本研究为进一步解释WRT制造过程中香气物质的形成机理提供了理论依据。
    Rougui Tea (RGT) is a typical Wuyi Rock Tea (WRT) that is favored by consumers for its rich taste and varied aroma. The aroma of RGT is greatly affected by the process of green-making, but its mechanism is not clear. Therefore, in this study, fresh leaves of RGT in spring were picked, and green-making (including shaking and spreading) and spreading (unshaken) were, respectively, applied after sun withering. Then, they were analyzed by GC-TOF-MS, which showed that the abundance of volatile compounds with flowery and fruity aromas, such as nerolidol, jasmine lactone, jasmone, indole, hexyl hexanoate, (E)-3-hexenyl butyrate and 1-hexyl acetate, in green-making leaves, was significantly higher than that in spreading leaves. Transcriptomic and proteomic studies showed that long-term mechanical injury and dehydration could activate the upregulated expression of genes related to the formation pathways of the aroma, but the regulation of protein expression was not completely consistent. Mechanical injury in the process of green-making was more conducive to the positive regulation of the allene oxide synthase (AOS) branch of the α-linolenic acid metabolism pathway, followed by the mevalonate (MVA) pathway of terpenoid backbone biosynthesis, thus promoting the synthesis of jasmonic acid derivatives and sesquiterpene products. Protein interaction analysis revealed that the key proteins of the synthesis pathway of jasmonic acid derivatives were acyl-CoA oxidase (ACX), enoyl-CoA hydratase (MFP2), OPC-8:0 CoA ligase 1 (OPCL1) and so on. This study provides a theoretical basis for the further explanation of the formation mechanism of the aroma substances in WRT during the manufacturing process.
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  • 文章类型: Journal Article
    茶产品,如速溶茶,已被证明可以改善肉制品的香气。然而,茶产品增强肉类香气的机制尚未得到充分解释。在这项研究中,我们分析了速溶茶对鸭肉香气的影响。我们的结果表明,用速溶茶处理导致花的增加,烤,和草的音符,同时减少鱼腥味和脂肪的音符。几种醇,醛类,酮,吲哚和二氢吖啶内酯表现出显着增加的OAV。相反,某些饱和醛,不饱和醛和醇显示出显着减少的OAVs。增强的花卉,烘烤和草香归因于速溶茶中存在的挥发性化合物。鱼腥味和脂肪味的减少与速溶茶中的多酚与壬醛相互作用有关,Undecanal,(E)-2-octenal,(E)-2-壬烯,(E)-2-decenal,和2,4-癸二烯醛通过疏水相互作用和电子效应。这项研究增强了我们对茶产品如何改善肉类香气的理解。
    Tea products, such as instant tea, have been shown to improve the aroma of meat products. However, the mechanisms by which tea products enhance meat aroma have not been adequately explained. In this study, we analyzed the impact of instant tea on the aroma of duck meat. Our results showed that treatment with instant tea led to increases in floral, baked, and grassy notes while reducing fishy and fatty notes. Several alcohols, aldehydes, ketones, indole and dihydroactinidiolide exhibited significantly increased OAVs. Conversely, certain saturated aldehydes, unsaturated aldehydes and alcohols displayed significantly decreased OAVs. The enhanced floral, baked and grassy notes were attributed to volatile compounds present in instant tea. The reduction in fishy and fatty notes was linked to polyphenols in instant tea interacting with nonanal, undecanal, (E)-2-octenal, (E)-2-nonenal, (E)-2-decenal, and 2,4-decadienal through hydrophobic interactions and electronic effects. This study enhances our understanding of how tea products improve meat aromas.
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  • 文章类型: Journal Article
    回收和分离人为排放的电子特种气体(F-气体,例如半导体部门的CF4和SF6)至关重要。在这项工作中,通过高内相乳液策略构建了分层多孔UiO-66-Br2@PS/DVB填充柱。UiO-66-Br2@PS/DVB表现出IAST预测的CF4/N2(2.67)和SF6/N2(3.34)的优异选择性,这是由于微孔中的扩散限制和气体骨架亲和力。尤其是,UiO-66-Br2@PS/DVB显示出显着的CF4和SF6保留,并使CF4/N2和SF6/N2成功分离,分辨率分别为2.37和8.89,在气相色谱中用作填充柱。与PorapakQ柱相比,UiO-66-Br2@PS/DVB填充柱的HETP降低,并显示出良好的重现性。这项研究不仅为制造分层多孔MOF填充柱提供了方便的方法,而且还展示了MOFs用于分离F-气体/N2混合物的前景。
    Recovery and separation of anthropogenic emissions of electronic specialty gases (F-gases, such as CF4 and SF6) from the semiconductor sector are of critical importance. In this work, the hierarchical porous UiO-66-Br2@PS/DVB-packed column was constructed by a high internal phase emulsions strategy. UiO-66-Br2@PS/DVB exhibits a superior selectivity of CF4/N2 (2.67) and SF6/N2 (3.34) predicted by the IAST due to the diffusion limitation in the micropore and the gas-framework affinity. Especially, UiO-66-Br2@PS/DVB showed significant CF4 and SF6 retention and enabled the successful separation of CF4/N2 and SF6/N2 with a resolution of 2.37 and 8.89, respectively, when used as a packed column in gas chromatography. Compared with the Porapak Q column, the HETP of the UiO-66-Br2@PS/DVB-packed column decreased and showed good reproducibility. This research not only offers a convenient method for fabricating a hierarchical porous MOF-packed column but also showcases the prospective utilization of MOFs for the separation of the F-gas/N2 mixture.
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  • 文章类型: Journal Article
    在过去的几十年里,合成代谢雄激素类固醇(AAS)因其性能增强和肌肉锻炼特性而在竞争中被滥用。传统上,通常在初始测试程序中使用气相色谱-质谱法检测AAS,以进行掺杂控制。气相色谱-Orbitrap高分辨率质谱(GC-Orbitrap-HRMS)是一种新技术,与GC-MS相比具有许多优势(例如,最大分辨能力240,000(FWHM在m/z200),出色的亚ppm质量精度,数据采集后的回顾性数据分析)。鼓励反兴奋剂从业人员充分利用色谱-质谱联用的最新技术,具体,和AAS的快速筛查方法。开发并验证了一种使用GC-Orbitrap-HRMS筛选人尿中多种AAS的新方法。该方法可以根据世界反兴奋剂机构的最低要求性能极限定性确定70种合成代谢雄激素类固醇。此外,经验证的方法成功地应用于口服美地烯酮后尿液中6种代谢物的检测,并对其体内排泄曲线进行了研究。甲二烯酮M6(17β-羟甲基-17α-甲基-18-去甲-1,4,13-三烯-3-酮)已被确定为长期的尿代谢产物,可以检测到长达7周,因此,与以前的研究相比,提供了更长的检测窗口。本研究为GC-Orbitrap-HRMS在药物代谢和非靶向筛选中的应用提供了理论基础。
    Over the past few decades, anabolic androgenic steroids (AASs) have been abused in and out of competition for their performance-enhancing and muscle-building properties. Traditionally, AASs were commonly detected using gas chromatography-mass spectrometry in the initial testing procedure for doping control purposes. Gas chromatography-Orbitrap high-resolution mass spectrometry (GC-Orbitrap-HRMS) is a new technology that has many advantages in comparison with GC-MS (e.g., a maximum resolving power of 240,000 (FWHM at m/z 200), excellent sub-ppm mass accuracy, and retrospective data analysis after data acquisition). Anti-doping practitioners are encouraged to take full advantage of the updated techniques of chromatography-mass spectrometry to develop sensitive, specific, and rapid screening methods for AASs. A new method for screening a wide range of AASs in human urine using GC-Orbitrap-HRMS was developed and validated. The method can qualitatively determine 70 anabolic androgenic steroids according to the minimum required performance limit of the World Anti-Doping Agency. Moreover, the validated method was successfully applied to detect six metabolites in urine after the oral administration of metandienone, and their excretion curves in vivo were studied. Metandienone M6 (17β-hydroxymethyl-17α-methyl-18-nor-androst-1,4,13-trien-3-one) has been identified as a long-term urinary metabolite which can be detected up to 7 weeks, thus providing a longer detection window compared with previous studies. This study provides a rationale for GC-Orbitrap-HRMS in drug metabolism and non-targeted screening.
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  • 文章类型: Journal Article
    ω-3多不饱和脂肪酸(ω-3PUFA),一种有许多健康益处的脂肪酸,越来越令人关注。在这里,我们开发了一种快速酯化和富集鸡蛋中ω-3PUFAs的方法,其中包括微波辅助酯化(MAE)和电增强固相微萃取(EE-SPME)。结合气相色谱,在鸡蛋中实现了ω-3PUFAs的有效检测。在微波辐射下,酯化效率显着提高了5.06至10.65倍。EE-SPME方法将提取时间从50分钟减少到15分钟。此外,探索了萃取纤维涂层材料的改进,保证了ω-3PUFAs的高效提取。在最优条件下,该方法具有较低的检出限(1.01-1.54μgL-1),良好的回收率(85.82%-106.01%),和宽线性范围(7.5-1000μgL-1),该方法已成功应用于实际鸡蛋样品中ω-3PUFA的测定。
    Omega-3 polyunsaturated fatty acids (ω-3 PUFAs), a type of fatty acid that has many health benefits, are of increasing concern. Herein, we developed a method for the rapid esterification and enrichment of ω-3 PUFAs in eggs, which includes microwave-assisted esterification (MAE) and electrically enhanced solid-phase microextraction (EE-SPME). Combined with gas chromatographic, efficient detection of ω-3 PUFAs was achieved in eggs. Under microwave radiation, the esterification efficiency exhibited a significant increase ranging from 5.06 to 10.65 times. The EE-SPME method reduced extraction time from 50 to 15 min. In addition, improvements in extractive fiber coating materials were explored, which ensured efficient extraction of ω-3 PUFAs. Under the optimal conditions, the method displayed a low detection limit (1.01-1.54 μg L-1), good recoveries (85.82%-106.01%), and wide linear range (7.5-1000 μg L-1), which was successfully applied to determine ω-3 PUFAs in real egg samples.
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