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顶空-气相色谱-质谱联用分析桂花和叶中挥发性成分 总被引:9,自引:0,他引:9
采用谱库检索结合准确质量测定、保留指数、串联质谱技术的多维定性分析策略鉴定化合物, 能够提高定性分析的效率和准确性. 运用顶空-气相色谱-四极质谱、顶空-气相色谱-飞行时间质谱以及顶空-气相色谱-串联质谱联用技术对桂花样品进行了分析检测, 并采用多维定性分析思路对检出的挥发性成分进行了鉴定. 结果共确认出47种挥发性成分, 其中单萜类和倍半萜类化合物为主要组分. 该定性分析策略准确可靠, 可以广泛应用于复杂样品挥发性成分的定性分析中. 相似文献
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为了解紫丁香、白丁香和红丁香花蕾精油样品挥发性成分的差异,采用气相色谱-质谱联用技术(GC-MS)分析了三种丁香花精油样品的挥发性成分,并对三者的挥发性成分进行了主成分分析和聚类分析。结果从紫丁香、白丁香和红丁香精油中分别解析出46、64和56种挥发性物质,包括烷烃类、酯类、醇类、酮类、烯烃类、酚类、有机酸等,其中共有的挥发性成分为9种。三种丁香花精油样品的挥发性成分比较分析显示,酯类是含量最高的挥发性成分,其次是烷烃类,并且这两类物质在不同品种的丁香花精油中含量不同。统计分析结果表明三种样品的挥发性成分之间没有明显差别。本研究为增加丁香花精油的应用范围提供了理论依据。 相似文献
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采用顶空固相微萃取-气相色谱/质谱法(HS-SPME-GC/MS)分析了白肋烟烟叶中挥发性、半挥发性成分。20 mg烟粉在60℃条件下孵化8 min,采用聚二甲基硅氧烷/二乙烯基苯(PDMS/DVB)65 μm纤维头萃取40 min,然后在250℃解吸3 min,通过与标准品和质谱数据库进行比对,初步定性了白肋烟烟叶中122种挥发性、半挥发性成分,并采用内标法进行半定量分析。通过主成分分析(PCA)和偏最小二乘-判别分析(PLS-DA)等化学计量学方法,直观反映了白肋烟烘焙前后挥发性、半挥发性成分的变化。该方法具有样品用量小、前处理简单、灵敏度高等特点,结合化学计量学方法可用于白肋烟烘焙前后化学成分变化分析,为白肋烟烘焙条件的优化提供了科学的检测方法。 相似文献
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提出了基于低密度溶剂超声辅助-表面活性剂增强乳化微萃取-气相色谱-质谱法测定薄荷芳香水中的挥发性成分。优化的试验条件如下:1萃取剂为甲苯;21mg·L-1吐温80溶液的用量为30μL;3超声时间为1min。在气相色谱分离中用DB-5石英毛细管柱为固定相,在质谱分析中采用全扫描检测模式。方法用于薄荷样品的分析,薄荷芳香水中共鉴定出20种挥发性成分,薄荷挥发油中共鉴定出30种挥发性成分,其中所含的主要成分基本一致。 相似文献
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建立了低温富集/气相色谱-质谱测定南丰蜜桔果肉成分的方法。对样品前处理中的溶剂种类、冷冻温度以及冷冻时间进行了优化,最终确定低温富集的前处理条件:正己烷为萃取溶剂;冷冻温度为-40℃;冷冻时间选择1 h。结果表明,采用低温富集/GC-MS结合保留指数定性对南丰蜜桔果肉进行成分分析,共鉴别出64种主要成分,主要包括酯类、萜烯类、醇类以及烷烃类。将低温富集所得结果分别与常温液液萃取结果及文献结果进行比较,所建立的方法可选择性富集一些极性大、热稳定性较差、难挥发性的物质。 相似文献
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建立了低温富集/气相色谱-质谱测定南丰蜜桔果肉成分的方法。对样品前处理中的溶剂种类、冷冻温度以及冷冻时间进行了优化,最终确定低温富集的前处理条件:正己烷为萃取溶剂;冷冻温度为-40 ℃;冷冻时间选择1 h。结果表明,采用低温富集/GC-MS结合保留指数定性对南丰蜜桔果肉进行成分分析,共鉴别出64种主要成分,主要包括酯类、萜烯类、醇类以及烷烃类。将低温富集所得结果分别与常温液液萃取结果及文献结果进行比较,所建立的方法可选择性富集一些极性大、热稳定性较差、难挥发性的物质。 相似文献
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顶空气相色谱-质谱联用技术的应用进展 总被引:1,自引:0,他引:1
顶空分析作为一种无有机溶剂萃取的样品处理技术,通常与气相色谱-质谱(GC-MS)技术结合用来分析复杂基质中的挥发性有机物。顶空气相色谱-质谱(HS-GC-MS)技术具有快速、高效、环保、灵敏度高等特点,在常规分析中发挥着重要作用。该文简要概述了静态顶空、动态顶空、顶空固相微萃取分析以及GC-MS联用技术,并介绍了整个顶空分析系统的影响因素和优化过程。根据基质类型的分类,综述了HS-GC-MS在食品和饮料、环境、生物等样品中的应用实例。HS-GC-MS的研究非常活跃,不断出现新应用,在分析挥发性有机物方面具有广阔前景。 相似文献
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Summary A comparison of different isolation methods for volatile compounds from the leaves ofLedum palustre has been carried out. The aim of the investigation was not to identify all the isolated compounds, though some new compounds were found. Methods used were steam distillation, Soxhlet extraction with n-hexane and the purge & trap technique.The results obtained by the three methods of extraction were compared and it is was found that the very volatile compounds isolated by the purge & trap technique, could not be found by the more conventional methods. The very volatile compounds found by the purge & trap technique were mainly dienals. 相似文献
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Pyrolysis gas chromatography–mass spectroscopy (PGC–MS) has been proved to be a powerful method to analyze both the volatile additives and the macromolecular structure of polymer materials. In this paper, flash evaporation technique was used to analyze the volatile degradation products of polymer materials during natural and artificial aging. In high density polyethylene (HDPE) composites, mainly n-alkanes with carbon number from 14 to 29 were detected after natural aging, while no oxidative product was found. Different composites have different n-alkane distributions. In contrast, various oxidative products including ketones, alcohols, esters and unsaturated species could be found in aged polypropylene (PP) nanocomposites. Nanoparticles accelerated the chain scission of PP and increased the formation of oxidative products significantly. During thermal oxidation of nitrile rubber (NBR) seal rubbers, heat/oxidation-induced extra crosslinking predominated and no volatile degradation products was detected. The main change happened in the volatiles is the decrease of additives, especially paraffins, antioxidant RD and hindered phenol. This resulted in the hardening of the rubber and the weakening of the protection from oxidation. Furthermore, the additive distribution along the depth was investigated, showing different migration speeds of different additives. From the additive levels remained in the NBR rubber, it is possible to predict the degradation status. In summary, PGC–MS can supply abundant information of polymer degradation and is helpful for mechanism research. 相似文献
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《Spectrochimica Acta Part B: Atomic Spectroscopy》1998,53(10):1469-1474
A donut-shaped spray chamber has been developed for the introduction of aerosol and/or volatile chemical species into the inductively coupled plasma. Compared with the Fassel–Scott spray chamber, it gives a higher efficiency of aerosol generation and transportation and superior stable inner pressure. As a result, it brings the benefits of higher intensity signal, lower background, higher measurement precision, and better detection limits. Using this spray chamber, it is more convenient to introduce volatile chemical species into the sampling system, and more flexible for the choice of introducing aerosol and volatile chemical species separately or simultaneously into the plasma. It is also suitable for FIA technique. 相似文献
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气相色谱-质谱技术分析姜油树脂中的挥发性及非挥发性成分 总被引:3,自引:0,他引:3
用超临界CO2萃取生姜根茎中的姜油树脂,并用气相色谱-质谱联用技术对其进行了成分分析。从姜油树脂中分析出77种化合物,其中挥发油成分50种,主要是α-姜烯(22.29%)、 β-倍半水芹烯(8.58%)、α-法尼烯(3.93%)、 β-没药烯(3.87%)和α-姜黄烯(2.63%)等倍半萜类化合物;姜辣素成分27种,主要成分为6-姜酚(9.38%)、6-姜烯酚(7.59%)和分析过程中由姜酚类或姜烯酚类化合物受热分解而形成的姜油酮(9.24%)。在姜辣素成分中,6-异姜酚、(Z)-10-异姜烯酚和(E)-10-异姜烯酚3种化合物是新发现的未见报道的化合物。实验中对这3种新化合物进行了质谱裂解分析。 相似文献
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A sensitive solid-phase microextraction and gas chromatography-pulsed flame photometric detection technique was developed to quantify volatile sulfur compounds in wine. Eleven sulfur compounds, including hydrogen sulfide, methanethiol, ethanethiol, dimethyl sulfide, diethyl sulfide, methyl thioacetate, dimethyl disulfide, ethyl thioacetate, diethyl disulfide, dimethyl trisulfide and methionol, can be quantified simultaneously by employing three internal standards. Calibration curves were established in a synthetic wine, and linear correlation coefficients (R2) were greater than 0.99 for all target compounds. The quantification limits for most volatile sulfur compounds were 0.5 ppb or lower, except for methionol which had a detection limit of 60 ppb. The recovery was studied in synthetic wine as well as Pinot noir, Cabernet Sauvignon, Pinot Grigio, and Chardonnay wines. Although the sulfur compounds behaved differently depending on the wine matrix, recoveries of greater than 80% were achieved for all sulfur compounds. This technique was applied to analyze volatile sulfur compounds in several commercial wine samples; methionol concentrations were found at the ppm level, while the concentrations for hydrogen sulfide, methanethiol, and methyl thioacetate were at ppb levels. Only trace amounts of disulfides and trisulfides were detected, and ethanethiol was not detected. 相似文献
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A method was developed to analyze and quantitate volatile fatty acids such as acetic, propionic, butyric, iso-butyric, valeric, and iso-valeric acid from samples of biological origin. A capillary column system including an automatic on-column injection device as well as a precolumn of larger internal diameter than the analytical column was elaborated for this purpose. In order to obtain well resolved and correctly quantifiable chromatographic peaks it turned out to be essential to work under acidic/aqueous conditions. To achieve a better sample transfer into the chromatographic system an organic solvent had to be used together with the aqueous milieu, thus improving wetting properties of the liquid sample plug introduced into the column. Cold on-column injection was applied in order to avoid discrimination of the various acids due to sample splitting and the automatic technique was chosen in view of the large number of samples from biological extractions which had to be analyzed. 相似文献
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Sample pretreatment before chromatographic analysis is the most time consuming and error prone part of analytical procedures, yet it is a key factor in the final success of the analysis. A quantitative and fast liquid phase microextraction technique termed as gas purge microsyringe extraction (GP-MSE) has been developed for simultaneous direct gas chromatography-mass spectrometry (GC-MS) analysis of volatile and semivolatile chemicals without cleanup process. Use of a gas flowing system, temperature control and a conventional microsyringe greatly increased the surface area of the liquid phase micro solvent, and led to quantitative recoveries of both volatile and semivolatile chemicals within short extraction time of only 2 min. Recoveries of polycyclic aromatic hydrocarbons (PAHs), organochlorine pesticides (OCPs) and alkylphenols (APs) determined were 85-107%, and reproducibility was between 2.8% and 8.5%. In particular, the technique shows high sensitivity for semivolatile chemicals which is difficult to achieve in other sample pretreatment techniques such as headspace-liquid phase microextraction. The variables affecting extraction efficiency such as gas flow rate, extraction time, extracting solvent type, temperature of sample and extracting solvent were investigated. Finally, the technique was evaluated to determine PAHs, APs and OCPs from plant and soil samples. The experimental results demonstrated that the technique is economic, sensitive to both volatile and semivolatile chemicals, is fast, simple to operate, and allows quantitative extraction. On-site monitoring of volatile and semivolatile chemicals is now possible using this technique due to the simplification and speed of sample treatment. 相似文献