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固相微萃取法结合GC-MS分析八角茴香中挥发性化合物 总被引:12,自引:0,他引:12
采用均相聚合物涂层———自制聚丙烯酸树脂(PA)萃取头,顶空萃取八角茴香中挥发性有机物.对萃取温度、样品量、解吸时间等参数进行了优化,得到了最佳萃取条件.该方法快速、简便,重现性好.通过气相色谱-质谱联用技术定性分析,鉴定了53种成分.同时,与商品多相聚合物涂层CAR/PDMS、DVB/CAR/PDMS分析结果比较,显示自制均相聚丙烯酸树脂萃取头对八角中挥发性有机物的萃取更全面. 相似文献
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Solid Phase Microextraction (SPME) 总被引:1,自引:0,他引:1
Solid phase microextraction (SPME) was developed to address the need for a fast, solvent-free and field compatible sample preparation method. It has been applied to a range of applications including environmental, industrial hygiene, process monitoring, clinical, forensic, food and drug analysis. In SPME, coated fibers are used to isolate and concentrate analytes into a range of coating materials. After extraction, the fibers are transferred, with the help of the syringe-like handling device, to analytical instruments for separation and quantification of the target analytes.In the past 20 years the number of instrumental techniques available to the chemist has grown exponentially. In order to help our readers keep up with this rapidly growing field, tutorial articles on chemical instrumentation will be a regular feature of The Chemical Educator. The articles are designed to serve as a brief introduction to emerging instrumetal techniques with an outline of the underlying principles and major applications. —Martin Schimpf, Series Editor 相似文献
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固相微萃取-气相色谱-质谱法分析常春油麻藤花挥发油成分 总被引:1,自引:0,他引:1
利用固相微萃取-气相色谱-质谱(SPME-GC-MS)联用技术对常春油麻藤的挥发油成分进行了分析,共鉴定出52种成分,占挥发油总成分的78.60%。常春油麻藤挥发油主要化学成分是1-辛烯-3-醇(15.38%),n-十六酸(6.01%),壬醛(5.23%),3-辛酮(5.17%),1-辛烯-3-酮(4.19%),2-戊烯醛(3.96%),己醛(3.43%),1-己醇(2.98%)等。 相似文献
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顶空固相微萃取-气质联用分析小麦储藏过程中挥发性成分变化 总被引:16,自引:0,他引:16
采用顶空固相微萃取(HS-SPME)和气相色谱-质谱联用(GC-MS)对不同储藏时间弱(强)筋小麦中的挥发性物质进行提取、鉴定与分析.选用复合萃取纤维二乙烯基苯-炭烯-聚二甲硅氧烷共聚物(DVB/CAR/PDMS)50 μm涂层,对萃取温度、时间、样品用量和解析时间进行优化.结果表明: HS-SPME测定挥发性物质的最佳前处理条件样品量20 g, 萃取温度75 ℃, 萃取时间60 min, 260 ℃条件下解析5 min;经鉴定分析小麦挥发性成分主要有烃类、醛类,其次为醇类、酮类;挥发性成分总含量在储藏6个月内均呈现先降后增的趋势.弱筋小麦的烃类挥发物相对量随储藏时间延长而快速增加,醛类相对含量先降后升,而酮类和醇类相对含量则逐渐下降;强筋小麦中除烃类相对含量呈先下降而后快速增加外,其余各类挥发物含量均与弱筋小麦呈现相同的规律.储藏6个月后,变化较明显的挥发性物质有己醇、己醛、2,6,10-三甲基-十二烷、十五烷和二十烷. 相似文献
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顶空固相微萃取技术用于海产品中丁基锡化合物的测定 总被引:2,自引:0,他引:2
采用顶空固相微萃取技术对生物样品中丁基锡化合物进行测定。用醋酸溶液浸提海产品中的丁基锡化合物,分析物经氢化衍生后用顶空固相微萃取方法富集,再以气相色谱分离,表面发射火焰光度检测器测定。整个过程简单快速,且无需消耗大量有毒的有机溶剂。方法的线性范围0~ 2000 ng/g (以锡的含量表示),相关系数 0.993?5 ~ 0.994?8 ,最低检测限(按S/N=3计算)3.4~52.4 ng/g (以锡的含量表示)。用该方法对贻贝标准参考物质CRM477进行测定,3种丁基锡化合物测定值的相对误差为0. 相似文献
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Essential oil of aerial parts of Tymus vulgaris L. from Babaaman montains of Iran were isolated by hydrodistillation with an average oil yield 1.9 w/w%. The components of the oil were identified by gas chromatography mass spectrometry. On a separate experiments the compositions of volatile emission of the plant were studied by headspace solid phase microextraction and gas chromatography mass spectrometry. The tempratures used during the sample preparation were 25°C and 50°C. In order to determine the effect of solvent (water) on the separation, the experiments were done in the presence and absence of distilled water in the extraction vial at the tempratures mentioned above. Ten majour components were obtained in four different experimental headspace solid phase microextraction conditions and the hydrodistillation methods from the plant. Thymol was found to be the most abundant costituent (27.2–73.09%), follwoed by p‐cymene (6.86–31.76%), γ‐terpinene (1.02–9.26%), myrcene (0.05–8.84%), α‐pinene (0.25–6.63%), caryophyllene (3.09–5.56%), thymol methyl ether (0.99–2.97%), thymolacetate (0.11–2.05%), carvacrol (0.49–1.70%) and α‐cadinol (0.38–1.10%). 相似文献
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固相微萃取技术在形态分析中的应用进展 总被引:3,自引:0,他引:3
形态分析比传统的元素分析能提供更为丰富的信息,成为当今分析化学领域前沿课题之一,而固相微萃取(SPME)是近十年来发展起来的新型分离富集技术,简便快速、无污染、易于和其它技术联用.近几年来才开始将固相微萃取应用到形态分析,二者结合对形态分析的发展具有促进作用,本文就固相微萃取技术在元素有机化合物形态分析中的应用进行了评述. 相似文献
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固相微萃取技术及其在有机锡和有机汞分析中的应用 总被引:18,自引:0,他引:18
固相微萃取是近年来发展起来的一种简便便快捷的样品前处理技术,这项技术不需要有机萃取剂,是一种环境友好的萃取过程。本文在前人工作和我们自己研究的基础上,讨论了SPME技术在有机锡和有机汞分析中的应用及各项参数对测定的影响。 相似文献
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固相微萃取参数选择及其对有机锡分析的影响 总被引:1,自引:0,他引:1
固相微萃取是一种新型的、不断发展和完善的样品前处理方法,它与其它技术联用可对多种样品基体中挥发、半挥发性有机化合物进行测定。目前,该技术在毒性金属有机化合物中的应用很少。本文分析参数选择对固相微萃取的影响的同时,还对其在有机锡化合物分析中的应用作了综述。 相似文献
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固相微萃取-气相色谱法测定塑料食品包装袋中的痕量挥发性有机物 总被引:10,自引:1,他引:10
采用固相微萃取与气相色谱联用技术,对塑料制品-保鲜薄膜、牛奶包装袋中的痕量挥发性有机物异丙醇、乙酸乙酯、丁酮、甲苯进行定量测定.该方法的线性范围大于l0^2数量级,检出限低于4.4ng/mL水平,相对标准偏差为2.3%-4.7%.方法灵敏度高、重现性较好. 相似文献
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《Analytical letters》2012,45(15):2457-2465
In order to explore the analytical performance of Headspace-Solid-phase Microextraction (HS-SPME), the sensitivity of gas chromatography (GC)-Mass Spectrometry (MS) determinations was examined in terms of calibration slopes, that is, response factor values of selected volatile organic compounds (VOC). The HS-SPME was applied to extract two kinds of gaseous VOC analytes, namely group I (methyl ethyl ketone, isobutyl alcohol, methyl isobutyl ketone, and butyl acetate, all having high water solubility) and group II (benzene, toluene, styrene, and xylene, all having moderate water solubility) from water solutions. The results, derived by both external and internal calibration, were then evaluated by considering headspace sample volume and solute volatility. In the case of solutes consisting of group I, sensitivity seems to increase with increasing HS size, although there are no such discernible patterns for group II solutes. The observed relative patterns in extraction efficiency may be accounted for by the differences in intermolecular forces present between the compounds of groups I and II and the possible effects of diffusion kinetics of the VOCs to the SPME fiber or competitive adsorption between different VOCs. As such, sensitivity of HS-SPME is tightly affected by the air-water partitioning properties of the target compounds and the response of SPME to such properties. 相似文献
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称取美甲贴样品0.0010g置于20mL顶空瓶中,在选定的条件下[孵化温度为36℃,孵化时间为15min,振动器转速为300r·min^-1,固相微萃取(SPME)温度为常温和样品的萃取次数为10次]进行顶空采样和固相微萃取,并将所得挥发性有机物(VOCs,包括所需测定的丙酮、正己烷、乙酸乙酯、乙酸异丙酯、甲苯和乙酸丁酯等6种化合物)引入气相色谱-质谱仪中进行分析。用HP-VOC色谱柱(60m×0.25mm,0.25μm)在40~250℃区间以程序升温模式进行色谱分离,并在电子轰击离子源和选择离子扫描模式等条件下进行质谱测定。采用外标法定量。测得上述6种VOCs的质量在相同的范围(2~250ng)内与其相应的峰面积呈线性关系,其检出限(3.14s)也相同(0.5ng)。以实际样品为基体,在5个浓度水平上加入标准溶液进行回收试验,测得其回收率为80.0%~110%,测定值的相对标准偏差(n=7)为0.030%~5.0%。 相似文献
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Dimitra A. Lambropoulou Ioannis K. Konstantinou Triantafyllos A. Albanis 《International journal of environmental analytical chemistry》2013,93(3-4):223-240
Abstract This study develops a method for solid phase microextraction (SPME) of ten widespread herbicides from water. The selected herbicides belong to different chemical groups are EPTC, molinate, propachlor, trifluralin, atrazine, propazine, terbuthylazine, prometryne, alachlor. Their determination was carried out by gas chromatography with flame thermionic and mass spectrometric detection. To perform the SPME, two types of fibre have been assayed: Carbowax-divinylbenzene (CW-DVB) of 65 μm thickness and polydimethylsiloxane-divinylbenzene (PDMS-DVB) of 65 μm thickness. The main factors affecting the SPME process such as pH, ionic strength, methanol content, memory effect, stirring rate and adsorption-time profile were studied. The method was applied to spiked natural waters such as ground water, sea water, lake water and river water in a concentration range of 0.1 to 10 μg/L. Limits of detection with each of the detectors were determined to be 1 – 20 ng/L in PDMS-DVB and 2–20 ng/L CW-DVB fibres. The recoveries of herbicides compared to distilled water were in relatively high levels 78.3–127.3 % and the average r2 values of the calibration curves were above 0.99 for all the analytes. The SPME conditions were finally optimized in order to obtain maximum sensitivity and samples were applied for the trace-level determination in river water samples originating from Ioannina region (Greece). 相似文献
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微波蒸馏-固相微萃取-气相色谱-质谱-嗅觉检测器联用分析鳙鱼鱼肉中的挥发性成分 总被引:12,自引:0,他引:12
用微波蒸馏(MD)-固相微萃取装置(SPME)提取鳙鱼鱼肉中的挥发性成分,利用气相色谱-质谱联用仪(GC-MS)对气味化合物成分进行了定性分析,同时利用嗅觉检测器鉴别了部分挥发性物质的气味特征。实验中优化了MD的操作条件(加热功率、加热时间及载气流速等)、SPME参数(萃取头种类、萃取温度、萃取时间、无机盐离子浓度及搅拌速率等)。通过NIST 02质谱数据库检索共定性确定出鳙鱼鱼肉挥发性成分中的53种化合物,其中主要为 C6~C9 的羰基化合物和挥发性醇类。经过嗅觉检测器分析,这些成分分别具有青草味、鱼腥味、泥土味等气味特征,其协同作用构成了鳙鱼鱼肉特殊的鱼腥味、泥腥味。该方法可用于水产品中挥发性成分的分析,并可为不良风味化合物的定量研究提供参考。 相似文献