Solid phase microextraction

固相微萃取
  • 文章类型: Journal Article
    酸笋是一种传统的发酵美食,在国内和国际上都受到了赞赏。这项研究调查了毛竹(PP)发酵过程中主要来自盐渍和腌制竹笋的微生物群落和挥发性风味化合物的复杂动态。首先使用常规分离和培养方法结合高通量测序(HTS)彻底检查了微生物和挥发性风味化合物的动力学,顶空固相微萃取(HS-SPME),和气相色谱-质谱(GC-MS)。此外,我们分析了负责调节挥发性风味的核心微生物。我们的发现揭示了60种挥发性化合物,其中14个是发酵PP香气的主要贡献者。这一组主要包括酒精,醛类,和烯烃。值得注意的是,我们的调查确定乳杆菌和念珠菌为发酵中后期的优势微生物属。这两个属对特征性香气的形成有重要影响。此外,我们发现酸,糖,糖和蛋白质可枢转地影响微生物的演替。具体来说,酸和可溶性糖推动了乳球菌向乳杆菌和片球菌的转变,而可溶性蛋白促进了从念珠菌到Kazachstania和Issatchenkia的真菌演替。这些见解揭示了整个PP发酵过程中风味化合物的群落结构和演替模式。最终,它们为优化发酵工艺和确保酸笋生产中的质量控制提供了基础。
    Sour bamboo shoots are a traditional fermented delicacy that has garnered appreciation both domestically and internationally. This study investigates the intricate dynamics of microbial communities and volatile flavor compounds primarily derived from salted and pickled bamboo shoots during the fermentation process of Phyllostachys purpurea (PP). The dynamics of microorganisms and volatile flavor compounds were thoroughly examined initially using conventional isolation and cultivation methods in conjunction with high-throughput sequencing (HTS), headspace solid-phase microextraction (HS-SPME), and gas chromatography-mass spectrometry (GC-MS). In addition, we analyzed the core microorganisms responsible for modulating the volatile flavor profile. Our findings revealed 60 volatile compounds, 14 of which were the predominant contributors to the aroma of fermented PP. This group primarily comprised alcohols, aldehydes, and olefins. Notably, our investigation identified Lactobacillus and Candida as the dominant microbial genera during the middle and late stages of fermentation. These two genera exert a significant influence on the formation of characteristic aromas. Furthermore, we discovered that acids, sugars, and proteins pivotally influence the succession of microorganisms. Specifically, acids and soluble sugars drove the transition of Lactococcus to Lactobacillus and Pediococcus, whereas soluble proteins facilitated fungal succession from Candida to Kazachstania and Issatchenkia. These insights shed light on the community structure and succession patterns of flavor compounds throughout the PP fermentation process. Ultimately, they provide a foundation for optimizing the fermentation process and ensuring quality control in the production of sour bamboo shoots.
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  • 文章类型: Journal Article
    为了满足开发高效提取材料的需求,以及基于小型化吸附剂的样品制备技术的发展,利用气泡模板方法获得了以硫作为杂原子掺杂的g-C3N4的中孔结构,同时避免了其他方法的苛刻条件。为了增加吸附位点的数量,然后用百里酚-香豆素NADES作为天然吸附剂改性剂对所得的剥落结构进行改性,然后通过静电纺丝工艺引入尼龙6聚合物。X射线衍射(XRD)傅里叶变换红外(FT-IR)光谱,场发射扫描电子显微镜(SEM),能量色散X射线光谱(EDS),和Brunauer-Emmett-Teller(BET)表面积分析验证了S掺杂的g-C3N4和复合材料的生产。所制备的静电纺纤维纳米复合材料,需要令人满意的加工性能,然后在液相色谱-串联质谱(LC-MS/MS)分析之前,成功地用作芯片上薄膜微固相萃取从唾液样品中提取非甾体抗炎药(NSAID)的吸附剂。利用芯片设备,薄膜μ-SPE与LC-MS/MS分析相结合,减少了样品溶液和有机溶剂,同时延长了薄膜吸附剂的使用寿命,取得了有希望的结果。优化了静电纺丝中DES修饰的S掺杂g-C3N4的量,以及吸附和解吸变量。在最优条件下,所选NSAIDs的线性范围为0.05-100.0ngmL-1,R2≥0.997.检出限在0.02和0.2ngmL-1之间。获得的日内和日间精度小于6.0%。相对回收率在93.3%至111.4%之间。
    To meet the needs of developing efficient extractive materials alongside the evolution of miniaturized sorbent-based sample preparation techniques, a mesoporous structure of g-C3N4 doped with sulfur as a heteroatom was achieved utilizing a bubble template approach while avoiding the severe conditions of other methods. In an effort to increase the number of adsorption sites, the resultant exfoliated structure was then modified with thymol-coumarin NADES as a natural sorbent modifier, followed by introduction into a nylon 6 polymer via an electrospinning process. X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, field-emission scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and Brunauer-Emmett-Teller (BET) surface area analysis validated S-doped g-C3N4 and composite production. The prepared electrospun fiber nanocomposite, entailing satisfactory processability, was then successfully utilized as a sorbent in on-chip thin film micro-solid-phase extraction of non-steroidal anti-inflammatory drugs (NSAIDs) from saliva samples prior to liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. Utilizing a chip device, a thin film μ-SPE coupled with LC-MS/MS analysis yielded promising outcomes with reduced sample solution and organic solvents while extending lifetime of a thin film sorbent. The DES-modified S-doped g-C3N4 amount in electrospun was optimized, along with adsorption and desorption variables. Under optimal conditions, selected NSAIDs were found to have a linear range of 0.05-100.0 ng mL-1 with an R2 ≥ 0.997. The detection limits were ranged between 0.02 and 0.2 ng mL-1. The intra-day and inter-day precisions obtained were less than 6.0%. Relative recoveries were between 93.3 and 111.4%.
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  • 文章类型: Journal Article
    对乳制品中的有机氯农药(OCP)残留进行灵敏而准确的分析提出了重大挑战。在这里,一种新型共价有机聚合物,Azo-COP-1是合成的,用于增强乳制品中OCPs的提取。偶氮-COP-1涂层的固相微萃取纤维通过氢键对OCPs表现出优异的萃取性能,卤素键合,π-π堆叠,和静电相互作用。与气相色谱-电子捕获检测相结合,我们开发了一种简便可靠的方法,用于检测六种乳制品中的OCPs,具有低检测限(2.0-400pgg-1)和高方法回收率(82.6-113%)。偶氮-COP-1涂层表现出良好的稳定性和耐久性。结果验证了使用基于Azo-COP-1的SPME提取乳制品样品中OCP残留的可行性,强调其在农药残留常规监测和食品安全评估方面的潜力。
    A sensitive and accurate analysis of organochlorine pesticide (OCP) residues in dairy products poses a significant challenge. Herein, a novel covalent organic polymer, Azo-COP-1, was synthesized for the enhanced extraction of OCPs in dairy products. The solid phase microextraction fiber coated with Azo-COP-1 demonstrated excellent extraction performance for the OCPs via hydrogen bonding, halogen bonding, π-π stacking, and electrostatic interactions. Coupled with gas chromatography-electron capture detection, we developed a facile and reliable method for detecting OCPs in six types of dairy products with low limits of detection (2.0-400 pg g-1) and high method recoveries (82.6-113%). Azo-COP-1 coatings exhibited good stability and durability. The results verified the feasibility of using Azo-COP-1-based SPME to extract OCP residues in dairy product samples, highlighting its potential for routine monitoring of pesticide residues and food safety assessments.
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  • 文章类型: Journal Article
    椰奶产品容易受到细菌损害,需要经常损害营养和香气完整性的灭菌方法。本研究采用顶空气相色谱-离子迁移谱(HS-GC-IMS)和顶空固相微萃取气相色谱-质谱(HS-SPME-GC-MS)研究了不同热灭菌方法对椰奶香气的影响。我们评估了巴氏灭菌的影响(PAS,70°C,25分钟),高温灭菌(HTS,121.1°C,15分钟),和超高温灭菌(UHT,130°C,5s)通过聚类热图和相关性分析。观察到显著差异(p<0.05),通过HS-GC-IMS和HS-SPME-GC-MS检测到37和52种物质,分别,确定12种关键香气化合物。UHT处理主要减少8种酸,保持类似于生椰奶的成分结构和感官特征。PAS和HTS处理降低了整体椰奶香气的感官强度,奶油,和花卉笔记,与2-庚醇的存在相关,非肛门,4-甲基戊酸,和2-十三烷酮.这些方法增加了煮熟的笔记,与5-甲基-3-庚酮有关,3-butyn-1-ol,羟基丙酮,和丙酮。酸败与酸如异丁酸有关,异戊酸,和庚酸,高温有效地减少这些化合物。PAS和HTS的长时间温度变化加速了脂质氧化降解和美拉德反应,在醇的形成中涉及游离脂肪酸,醛类,酯类,和内酯。这些发现为研究椰奶风味变质提供了理论依据。
    Coconut milk products are susceptible to bacterial damage, necessitating sterilization methods that often compromise nutrient and aroma integrity. This study investigates the effects of different thermal sterilisation methods on coconut milk aroma using headspace gas chromatography-ion mobility spectrometry (HS-GC-IMS) and headspace solid-phase microextraction gas chromatography-mass spectrometry (HS-SPME-GC-MS). We assessed the impact of pasteurisation (PAS, 70 °C, 25 min), high-temperature sterilisation (HTS, 121.1 °C, 15 min), and ultra-high temperature sterilisation (UHT, 130 °C, 5 s) through clustered heat maps and correlation analyses. Significant differences were observed (p < 0.05), with 37 and 52 substances detected by HS-GC-IMS and HS-SPME-GC-MS, respectively, identifying 12 key aroma compounds. UHT treatment primarily reduced 8 acids, maintaining a compositional structure and sensory profile similar to raw coconut milk. PAS and HTS treatments decreased the sensory intensity of overall coconut milk aroma, creamy, and floral notes, correlating with the presence of 2-heptanol, nonanal, 4-methylvaleric acid, and 2-tridecanone. These methods increased cooked notes, associated with 5-methyl-3-heptanone, 3-butyn-1-ol, hydroxyacetone, and acetoin. Rancidity was linked to acids such as isobutyric acid, isovaleric acid, and heptanoic acid, with high temperatures effectively reducing these compounds. Prolonged temperature changes in PAS and HTS accelerated lipid oxidative degradation and the Maillard reaction, involving free fatty acids in the formation of alcohols, aldehydes, esters, and lactones. These findings provide a theoretical basis for studying coconut milk flavour deterioration.
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  • 文章类型: Journal Article
    通过顶空固相微萃取气相色谱-质谱(HS-SPME-GC/MS)结合电子鼻(E-nose)和电子舌(E-t舌)分析,检查了小麦粉在成熟过程中的挥发性特征。小麦粉在三个不同的条件下经历了预定持续时间的成熟。尽管GC/MS与E-t舌联用在经历不同成熟条件的小麦粉样品中表现出辨别能力,电子鼻分析仅依靠主成分分析无法实现判别。在小麦粉中鉴定出83种挥发性化合物,在25°C下成熟50d的样品中观察到的丰度最高。值得注意的是,反式-2-壬烯醛,decanal,和nonanal是小麦粉特征风味特征的主要贡献者。HS-SPME-GC/MS与E-舌的整合表明,在25°C下成熟50d的小麦粉中,具有出色的风味发展和实际生存能力。这项研究为增强小麦粉及其衍生产品的风味提供了理论基础。
    The volatile profiles of wheat flour during maturation were examined through headspace solid-phase micro-extraction gas chromatography-mass spectrometry (HS-SPME-GC/MS) combined with electronic nose (E-nose) and electronic tongue (E-tongue) analyses. The wheat flour underwent maturation under three distinct conditions for predetermined durations. While GC/MS coupled with E-tongue exhibited discernment capability among wheat flour samples subjected to varying maturation conditions, E-nose analysis solely relying on principal component analysis failed to achieve discrimination. 83 volatile compounds were identified in wheat flour, with the highest abundance observed in samples matured for 50 d at 25 °C. Notably, trans-2-Nonenal, decanal, and nonanal were the main contributors to the characteristic flavor profile of wheat flour. Integration of HS-SPME-GC/MS with E-tongue indicated superior flavor development and practical viability in wheat flour matured for 50 d at 25 °C. This study furnishes a theoretical groundwork for enhancing the flavor profiles of wheat flour and its derivative products.
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  • 文章类型: Journal Article
    黑茶(DT)在中国拥有丰富的文化历史,并因其独特的风味和潜在的健康益处而获得了相当大的消费者。在这项研究中,顶空固相微萃取(HS-SPME)结合气相色谱-质谱(GC-MS),相对气味活性值(ROAV),用化学计量学方法检测和分析了不同地理区域的五种黑茶的香气成分差异。结果表明,来自不同地理区域的五个DT类型不同,数量,和挥发性化合物的相对浓度。HS-SPME-GC-MS在56个DT样品中鉴定出了1372种挥发性化合物。使用ROAV和化学计量学方法,基于ROAV>1和VIP>1。18种关键香气化合物可作为DT分类的潜在指标,包括二氢Actinidiolide,芳樟醇,1,2,3-三甲氧基苯,香叶基丙酮,1,2,4-三甲氧基苯,cedrol,3,7-二甲基-1,5,7-辛三烯-3-醇,β-紫罗兰酮,4-乙基-1,2-二甲氧基苯,水杨酸甲酯,α-紫罗兰酮,香叶醇,芳樟醇氧化物I,芳樟醇氧化物II,6-甲基-5-庚烯-2-酮,α-松油醇,1,2,3-三甲氧基-5-甲基苯,和1,2-二甲氧基苯。这些化合物为区分不同地理区域的5种DTs的差异提供了一定的理论依据。这项研究为鉴定DTs中的挥发性物质和阐明关键香气化合物的差异提供了一种潜在的方法。缩写:DT,黑茶;FZT,腐竹茶;LPT,广西六保茶;QZT,湖北青专茶;TBT,四川藏茶;PET,云南普洱茶;ROAV,相对气味活性值;OT,气味阈值;HS-SPME,顶空固相微萃取;GC-MS,气相色谱-质谱法;PCA,主成分分析;PLS-DA,偏最小二乘判别分析;HCA,层次聚类分析。
    Dark tea (DT) holds a rich cultural history in China and has gained sizeable consumers due to its unique flavor and potential health benefits. In this study, headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS), relative odor activity value (ROAV), and chemometrics approaches were used to detect and analyze aroma compounds differences among five dark teas from different geographical regions. The results revealed that the five DTs from different geographical regions differed in types, quantities, and relative concentrations of volatile compounds. A total of 1372 volatile compounds of were identified in the 56 DT samples by HS-SPME-GC-MS. Using ROAV and chemometrics approaches, based on ROAV>1 and VIP>1. Eighteen key aroma compounds can be used as potential indicators for DT classification, including dihydroactinidiolide, linalool, 1,2,3-trimethoxybenzene, geranyl acetone, 1,2,4-trimethoxybenzene, cedrol, 3,7-dimethyl-1,5,7-octatrien-3-ol, β-ionone, 4-ethyl-1,2-dimethoxybenzene, methyl salicylate, α-ionone, geraniol, linalool oxide I, linalool oxide II, 6-methyl-5-hepten-2-one, α-terpineol, 1,2,3-trimethoxy-5-methylbenzene, and 1,2-dimethoxybenzene. These compounds provide a certain theoretical basis for distinguishing the differences in five DTs from different geographical regions. This study provides a potential method for identifying the volatile substances in DTs and elucidating the differences in key aroma compounds. Abbreviations: DT, dark tea; FZT, Fuzhuan tea; LPT, Guangxi Liupao tea; QZT, Hubei Qingzhuan tea; TBT, Sichuan Tibetan tea; PET, Yunnan Pu-erh tea; ROAV, Relative odor activity value; OT, Odor threshold; HS-SPME, Headspace solid-phase microextraction; GC-MS, Gas chromatography-mass spectrometry; PCA, Principal components analysis; PLS-DA, Partial least squares-discriminant analysis; HCA, Hierarchical clustering analysis.
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  • 文章类型: Journal Article
    枯萎是决定白茶(WT)质量的关键过程。据报道,太阳枯萎(SW)有助于WT的香气质量。然而,在受到SW的WT中形成香气的机制尚不清楚。在这项研究中,通过顶空固相微萃取-气相色谱-质谱(HS-SPME-GC-MS)和转录组学,我们发现13个关键基因富含甲羟戊酸和甲基赤藓糖醇磷酸途径,如1-脱氧-D-木酮糖-5-磷酸合酶和萜品醇合酶,显着上调,促进α-萜品油烯的积累,香叶醇,还有Nerolidol,赋予经过SW的WT以花香和果味。此外,富含脂氧合酶途径的脂氧合酶的显著上调促进己醇的积累,1-octen-3-ol,(E,Z)-3,6-壬丁-1-醇,和非肛门,这有助于在受到SW的WT中产生绿色和新鲜的气味。这项研究首次全面了解了SW对WT香气形成的影响机制。
    Withering is a crucial process that determines the quality of white tea (WT). Solar withering (SW) is reported to contribute to the aroma quality of WT. However, the mechanism by which aroma is formed in WT subjected to SW remains unclear. In this study, through headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) and transcriptomics, we found that 13 key genes enriched in the mevalonic acid and methylerythritol phosphate pathways, such as those of 1-deoxy-D-xylulose-5-phosphate synthase and terpineol synthase, were significantly upregulated, promoting the accumulation of α-terpinolene, geraniol, and nerolidol, which imparted floral and fruity odors to WT subjected to SW. Additionally, the significant upregulation of lipoxygenases enriched in the lipoxygenase pathway promoting the accumulation of hexanol, 1-octen-3-ol, (E, Z)-3,6-nonadien-1-ol, and nonanal, which contributed to the green and fresh odor in WT subjected to SW. This study provided the first comprehensive insight into the effect mechanism of SW on aroma formation in WT.
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  • 文章类型: Journal Article
    微生物代谢对美玉独特风味的形成具有重要意义,一种中国传统的发酵鱼片。然而,发酵过程中微生物与风味成分的相互作用关系尚不清楚。在这项研究中,采用电子鼻和顶空-固相微萃取-气相色谱-质谱联用技术对美玉发酵过程中的风味成分进行了鉴定,并进行了绝对微生物定量,以鉴定微生物群落的多样性和演替。在发酵过程中,挥发性化合物的种类有所增加。醇,醛类,芳香族化合物和酯类是主要的风味化合物,在美玉中显著增加,而碳氢化合物和醛类明显减少。乳酸菌的绝对丰度,发酵3天后,乳球菌和Weissella显著增加,与1-壬醇的产生密切相关,2-甲氧基-4-乙烯基苯酚,愈创木酚,棕榈酸乙酯和辛酸乙酯可能与脂肪酸生物合成和氨基酸代谢有关。然而,这些属与吲哚的产生呈负相关。此外,3天内发酵的美玉的总挥发性碱性氮(TVB-N)水平在25mgTVB-N/100g鱼的范围内,游离氨基酸含量和脂氧合酶活性明显低于发酵4天。鉴于食品安全和风味,建议在室温下自然发酵的美玉应控制在3天内。这项研究强调了绝对定量在传统发酵美玉微生物组分析中的应用,并为微生物在发酵过程中风味形成中的作用提供了新的见解。
    Microbial metabolism is important for the unique flavor formation of Mei yu, a kind of traditional Chinese fermented fish pieces. However, the interactive relationship between microorganisms and flavor components during fermentation is still unclear. In this study, electronic nose and headspace-solid-phase microextraction-gas chromatography-mass spectrometry analysis were performed to identify flavor components in Mei yu during the fermentation, and the absolute microbial quantification was conducted to identify the diversity and succession of microbial communities. During fermentation, there was an increase in the types of volatile compounds. Alcohols, aldehydes, aromatics and esters were the main flavor compounds and significantly increased in Mei yu, while hydrocarbon and aldehydes significantly decreased. The absolute abundances of Lactobacillus, Lactococcus and Weissella increased significantly after 3 days\' fermentation, which were closely associated with the productions of 1-nonanol, 2-methoxy-4-vinylphenol, guaiacol, ethyl palmitate and ethyl caprylate that might though pathways related to fatty acid biosynthesis and amino acid metabolism. However, these genera were negatively correlated with the production of indole. Additionally, the total volatile basic nitrogen (TVB-N) levels of Mei yu fermented during 3 days were within the limits of 25 mg TVB-N/100 g fish, with the contents of free amino acids and lipoxygenase activities were significant lower than that of 4 days\' fermentation. In view of food safety and flavor, it suggested that the natural fermented Mei yu at room temperature should be controlled within 3 days. This study highlights the application of absolute quantification to microbiome analysis in traditional fermented Mei yu and provides new insights into the roles of microorganisms in flavor formation during fermentation.
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  • 文章类型: Journal Article
    啤酒的世界是由不同风格编织而成的丰富挂毯,每个人都有其独特的性格。Lager,以其脆度而闻名,在较低温度下发酵,而啤酒,在温暖的地方,拥有广泛的香气。比利时啤酒因其复杂性而令人眼花缭乱,从果味的Trappist啤酒到酸味的羊肉。德国小麦啤酒,像Hefeweizens,魅力与他们的泡腾和果味的底色。印度苍白的艾尔斯(IPA)展示了一个跳跃的爆发,而酸麦芽酒则以其浓郁而诱人。工艺,历史,和区域成分交织在这个酿造世界中,为爱好者提供一系列愉快的体验。对精酿啤酒香气的研究有限,分子指纹可能至关重要。迄今为止,没有研究集中在表征化合物的特征来区分啤酒的风格。顶空固相微萃取(HS-SPME)方法提供了一种快速无溶剂的挥发性化合物方法。本研究旨在通过使用HS-SPME/GC-MS技术结合多变量数据处理来表征各种啤酒的香气特征。总共收集了120个啤酒样品,并将其分为五类:比尔森(n=28);拉格(n=23);阿莱(n=32);酸(n=24);和比利时的艾尔斯(n=13)。在比尔森啤酒中,在含有啤酒花提取物和啤酒花的啤酒中发现了18种独特的化合物,和2用于含有啤酒花提取物(乙酸辛酯;和α-松油醇)的啤酒。当将其余的组相互比较时,比利时啤酒展示了5种独特的化合物,Lagers有一个(非肛门)。Sours和Ales没有独特的化合物,但与比利时组共享2种不同的化合物。我们得出的结论是,就各种与香气有关的化合物而言,比利时啤酒是最复杂的,并且可以从啤酒花提取物中区分使用纯啤酒花的啤酒。
    The world of beer is a rich tapestry woven with diverse styles, each with its unique character. Lager, known for its crispness, ferments at lower temperatures, while ale, at warmer ones, boasts a wide spectrum of aromas. Belgian beers dazzle with their complexity, from fruity Trappist ales to sour lambics. German wheat beers, like hefeweizens, charm with their effervescence and fruity undertones. India Pale Ales (IPAs) showcase a hoppy burst, while sour ales tantalize with their tanginess. Craftsmanship, history, and regional ingredients intertwine in this world of brewing, offering aficionados an array of delightful experiences. Research on craft beer aromas is limited, and molecular fingerprint could be crucial. To date, there have been no studies focused on characterizing compound profiles to differentiate beer styles. The Headspace Solid Phase Microextraction (HS-SPME) method provides a rapid and solvent-free approach to volatile compound. The present study aims to characterize the aroma profile of a wide range of beers by using HS-SPME/GC-MS technique combined with multivariate data processing. A total of 120 beer samples were collected and divided into five categories: Pilsen (n = 28); Lager (n = 23); Ale (n = 32); Sour (n = 24); and Belgian Ales (n = 13). Among the Pilsen beers, 18 unique compounds were found for beers with hop extract and hops, and 2 for beers with hop extract (Octyl acetate; and alpha-Terpineol). When comparing the remaining groups to each other, Belgian beers exhibited 5 unique compounds, and Lagers had one (nonanal). Sours and Ales did not have unique compounds but shared 2 distinct compounds with the Belgian group each. We concluded that Belgian beers are the most complex in terms of various aroma-related compounds, and that it is possible to distinguish beers that use pure hops from hop extract.
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  • 文章类型: Journal Article
    甲醛(HCHO)是一种人体毒素,既是污染物又是内源性代谢产物。据报道,人类生物样品中的HCHO浓度在微摩尔范围内;然而,缺乏灵敏的分析方法会损害准确的定量。为了解决这个问题,我们先前报道了一种使用半胱胺作为HCHO清除剂的基于SPME-GC-MS的新型HCHO检测方法。该方法表明半胱胺是比广泛使用的O-(2,3,4,5,6-五氟苄基)羟胺更有效的清除剂,并且能够检测纳摩尔范围内的水性HCHO和微摩尔范围内的定量。然而,在此范围内的定量需要浸入式提取HCHO衍生的噻唑烷,同时也观察到高背景信号。根据这些研究,我们现在报告一种使用半胱胺的优化顶空萃取SPME-GC-MS方法,这提供了类似灵敏的HCHO定量浸入法,但避免了大量的洗涤步骤,因此更适合筛选应用。然而,仍然观察到高背景HCHO水平。使用基于2-aza-Cope的HCHO清除剂的补充GC-MS分析也揭示了高背景HCHO水平;因此,组合结果表明,HCHO以高(即微摩尔)浓度存在于水性样品中,这妨碍了低于微摩尔范围的准确定量。这一观察结果对正在进行的水中HCHO定量研究具有重要意义。包括生物样本。
    Formaldehyde (HCHO) is a human toxin that is both a pollutant and endogenous metabolite. HCHO concentrations in human biological samples are reported in the micromolar range; however, accurate quantification is compromised by a paucity of sensitive analysis methods. To address this issue, we previously reported a novel SPME-GC-MS-based HCHO detection method using cysteamine as an HCHO scavenger. This method showed cysteamine to be a more efficient scavenger than the widely used O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine, and enabled detection of aqueous HCHO in the nanomolar range and quantification in the micromolar range. However, quantification in this range required immersive extraction of the HCHO-derived thiazolidine, while a high background signal was also observed. Following on from these studies, we now report an optimised head-space extraction SPME-GC-MS method using cysteamine, which provides similarly sensitive HCHO quantification to the immersive method but avoids extensive wash steps and is therefore more amenable to screening applications. However, high background HCHO levels were still observed A Complementary GC-MS analyses using a 2-aza-Cope-based HCHO scavenger also revealed high background HCHO levels; therefore, the combined results suggest that HCHO exists in high (i.e. micromolar) concentration in aqueous samples that precludes accurate quantification below the micromolar range. This observation has important implications for ongoing HCHO quantification studies in water, including in biological samples.
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