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用于磷酸酯和甲基膦酸酯类化合物测定的固相微萃取新型涂层 总被引:1,自引:0,他引:1
以羟基硅油和二乙烯基苯为涂层材料 ,采用溶胶 凝胶技术和自由基引发交联的方法制备了一种新型的固相微萃取探头。采用顶空固相微萃取与气相色谱联用的方法模拟检测了水中磷酸酯和甲基磷酸酯类化合物。与商品化固相微萃取探头相比 ,该新型涂层可获得高的萃取效率。甲基膦酸二甲酯、磷酸三甲酯和磷酸三丁酯的最低检测限分别为 0 34,2 2 0和 0 0 1mg/L,相对标准偏差为 3 6 7%~ 6 4 4 % ,线性范围为 1~ 2个数量级 ,方法重现性好 ,回收率为 89 4 6 %~ 90 88%。 相似文献
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采用溶胶-凝胶技术涂层的新型固相微萃取方法及其应用 总被引:13,自引:0,他引:13
将溶胶-凝胶技术应用于SPME固相涂层的制备,涂制的端羟基-聚二甲基硅氧烷固相涂层热稳定性好,萃取时间和解吸时间短,对极性化合物及非极性化合物均有较强的萃取富集能力。扫描电镜图显示涂层表面为多孔结构。采用该涂层的SPME方法在对环境样品的分析中获得了令人满意的效果。 相似文献
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通过反复冷冻-解冻和溶胶-凝胶方法制备了聚乙烯醇/SiO2有机/无机双交联网络互穿的固相微萃取涂层, 并利用红外光谱(FTIR)、 热重分析(TGA)、 扫描电子显微镜(SEM)和气相色谱(GC)等方法对该涂层进行了结构及性能表征. 该固相微萃取涂层具有很好的热稳定性(Td>300 ℃), 通过化学键合作用于玻璃或石英纤维表面, 稳定性好, 不易脱落. 对正丙醇、 正丁醇、 异戊醇和甲苯进行萃取, 结果表明, 该纤维涂层对带有羟基的极性物质有很好的选择性, 并且相对标准偏差(RSD, n=3)小于5.0%. 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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在0.1 mol L-1苯胺+1.0 mol L-1HNO3水溶液中,通过循环伏安法在涂有疏水性离子液体1-辛基-3-甲基咪唑-六氟磷酸盐的不锈钢丝上制备了新型离子液体-聚苯胺(IL-PANI)复合萃取涂层.制得的IL-PANI涂层呈网状结构,比表面积比PANI大,IL则分散在PANI表面和网孔内.以几种苯酚衍生物为目标分析物,对所得萃取头的性能进行了考察.在优化后的实验条件下,对这些酚类化合物进行顶空固相微萃取–气相色谱检测,其线性范围为0.048~400μg L-1,检出限为6.1~98 ng L-1(S/N=3).同一萃取头萃取五次的相对标准偏差(RSD)小于5.5%;多根萃取头平行萃取的RSD为3.7%~12%(n=3).PANI-IL涂层有良好的稳定性,在使用150多次后萃取性能仅有很小的变化;在温度高至300℃时不分解.与聚苯胺涂层相比,其萃取效率更高. 相似文献
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Christelle Lemaitre-Guillier Agns Chartier Christelle Dufresne Antonin Douillet Stphanie Cluzet Josep Valls Nicolas Aveline Xavier Daire Marielle Adrian 《Molecules (Basel, Switzerland)》2022,27(18)
The present study is aimed at determining whether leaf volatile organic compounds (VOCs) are good markers of the grapevine response to defence elicitors in the field. It was carried out in two distinct French vineyards (Burgundy and Bordeaux) over 3 years. The commercial elicitor Bastid® (Syngenta, Saint-Sauveur, France) (COS-OGA) was first used to optimise the VOCs’ capture in the field; by bagging stems together with a stir bar sorptive extraction (SBSE) sensor. Three elicitors (Bastid®, copper sulphate and methyl jasmonate) were assessed at three phenological stages of the grapevines by monitoring stilbene phytoalexins and VOCs. Stilbene production was low and variable between treatments and phenological stages. VOCs—particularly terpenes—were induced by all elicitors. However, the response profiles depended on the type of elicitor, the phenological stage and the vineyard, and no sole common VOC was found. The levels of VOC emissions discriminated between weak (Bastid® and copper sulphate) and strong (methyl jasmonate) inducers. Ocimene isomers were constitutively present in the overall blends of the vineyards and increased by the elicitors’ treatments, whilst other VOCs were newly released throughout the growing seasons. Nonetheless, the plant development and climate factors undoubtedly influenced the release and profiles of the leaf VOCs. 相似文献
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固相萃取技术在食品痕量残留和污染分析中的应用 总被引:3,自引:0,他引:3
食品痕量残留和污染分析中,样品的前处理极为重要,也是其难点所在。由于食品和农产品样品的多样性和复杂性,目前还没有一种前处理技术能够适合所有情况下的所有样品。本文对近年来发展起来的新型固相萃取技术如固相微萃取、搅拌棒吸附萃取、基质固相分散萃取、分子印迹固相萃取、免疫亲和固相萃取、整体柱固相萃取、碳纳米管固相萃取等在食品痕量残留和污染分析中的应用进行了综述,对未来的发展前景作了展望。 相似文献
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Recent developments in solid-phase microextraction for on-site sampling and sample preparation 总被引:1,自引:0,他引:1
Chunfeng DuanZheng Shen Dapeng WuYafeng Guan 《Trends in analytical chemistry : TRAC》2011,30(10):1568-1574
On-site sampling and sample preparation favor portable, solventless or even solvent-free techniques. Solid-phase microextraction (SPME) has these advantages. This review focuses on developments between 2007 and early 2011 in microextraction techniques for on-site sampling and sample preparation, including fiber SPME, stir-bar sorptive extraction (SBSE), thin-film microextraction (TFME) and different types of in-needle SPME. The major trends in on-site applications of SPME appear to be fiber and thin-film SPME, microextraction by packed sorbent (MEPS) and the sorbent-packed needle-trap device (NTD). We discuss and compare several aspects of these types of SPME in on-site applications. We also describe sorbent phases for SPME that benefit on-site applications. Finally, we provide a perspective on SPME-based techniques for on-site applications. 相似文献
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以己烯雌酚为替代模板,利用整体材料的“原位”合成技术制备了分子印迹聚合物,并将其作为固相萃取搅拌棒的涂层(MIP-SBSE)制备了新的搅拌棒。详细考察了分子印迹聚合物制备条件中模板分子及功能单体用量对MIP-SBSE选择性萃取性能的影响,同时利用元素分析、扫描电镜和红外光谱对聚合物进行表征。以双烯雌酚(DS)和己烷雌酚(HS)为目标化合物,将MIP-SBSE与高效液相色谱-二极管阵列检测器联用,建立起复杂样品中DS和HS的分离分析方法。考察了吸附和解吸时间、解吸溶剂、离子强度和样品pH值等萃取条件对MIP-SBSE选择性萃取性能的影响。结果表明,在最佳萃取条件下,MIP-SBSE对DS和HS具有较高的选择性萃取性能,线性范围分别为1.0~400.0 μg/L和5.0~400.0 μg/L,利用氮吹再定容的方法,对DS和HS的检出限(S/N=3)分别可低至0.04和0.14 μg/L。在对实际污水、蜂蜜和牛尿样品的分析中取得了良好的加标回收率,其值为61.3%~120%。所建方法具有简便、高选择性和灵敏等特点,可用于复杂样品中双烯雌酚和己烷雌酚的分析监测。 相似文献
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高效液相色谱法分析矿泉水中酚类化合物 总被引:22,自引:1,他引:22
用带荧光检测器的高效液相色谱法同时测定了矿泉水中的苯酚、甲酚、双酚A、双酚F、4-叔丁酚、双酚A二环氧甘油醚和双酚F二环氧甘油醚等,水样经液-固萃取浓缩后再进行分析,检测限可达0.1~0.2μg/L。重复测定的标准偏差为1.12%~13.21%,水样测定的回收率为81%~105%。 相似文献
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Keita Saito Yoshiyuki Tokorodani Chihiro Sakamoto Hiroyuki Kataoka 《Molecules (Basel, Switzerland)》2021,26(19)
The odors and emanations released from the human body can provide important information about the health status of individuals and the presence or absence of diseases. Since these components often emanate from the body surface in very small quantities, a simple sampling and sensitive analytical method is required. In this study, we developed a non-invasive analytical method for the measurement of the body odor component 2-nonenal by headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry by selective ion monitoring. Using a StableFlex PDMS/DVB fiber, 2-nonenal was efficiently extracted and enriched by fiber exposition at 50 °C for 45 min and was separated within 10 min using a DB−1 capillary column. Body odor sample was easily collected by gauze wiping. The limit of detection of 2-nonenal collected in gauze was 22 pg (S/N = 3), and the linearity was obtained in the range of 1–50 ng with a correlation coefficient of 0.991. The method successfully analyzed 2-nonenal in skin emissions and secretions and was applied to the analysis of body odor changes in various lifestyles, including the use of cosmetics, food intake, cigarette smoking, and stress load. 相似文献
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基于整体材料搅拌棒固相萃取高效液相色谱联用测定饲料和水样中硝基呋喃类药物残留 总被引:1,自引:0,他引:1
利用自制的以聚(乙烯基咪唑-二乙烯基苯)(VIDB)整体材料为涂层的固相萃取搅拌棒(VIDB-SBSE)萃取3种硝基呋喃类药物,然后与高效液相色谱-二极管阵列检测器联用建立了测定饲料和水样品中硝基呋喃类药物残留的方法。详细考察了萃取过程中萃取和解吸时间、样品基质的pH值以及离子强度等实验条件对萃取效率的影响。在最佳条件下,呋喃唑酮的线性范围为0.5~200μg/L,呋喃妥因和呋喃西林的线性范围为0.25~200μg/L,3种目标物的检出限(LO D)(S/N=3)在0.068~0.11μg/L之间,所建方法具有理想的日内和日间重现性(R SD值均小于6%)。在对饲料和实际水样的测定中,不同加标浓度呋喃唑酮、呋喃妥因和呋喃西林的回收率在80.6%~108%之间。研究表明,所建立的方法具有简便、灵敏、环境友好等特点。 相似文献