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Method development for the determination of wood preservatives in commercially treated wood using gas chromatography-mass spectrometry

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ANALYTICA CHIMICA ACTA 2011年第2期702卷 205-212页

作者： St'avova, Jana Sedgeman, Carl A. Smith, Zachary T. Frink, Lillian A. Hart, Jessica A. Niri, Vadoud H. Kubatova, Alena Univ N Dakota Dept Chem Grand Forks ND 58202 USA

Fungicides and insecticides are commonly used preservatives to protect wood products against microbiological degradations. Currently, there is a lack of analytical methods addressing the quantitative determination of a wide range of wood preserving species in wood matrices. In this study, a reliable method was developed for the determination of a mixture of wood preserving agents with differing chemical structures (i.e., properties), including tebuconazole (TAZ), propiconazole (PAZ), 3-iodo-2-propynyl butylcarbamate (ipbc), and permethrin (PER), in pine wood. The analyte recoveries obtained by Soxhlet and multiple-stage sonication extractions were compared. While both extraction methods yielded similar results (80-100%). Soxhlet extraction was found to be less labor-intensive and thus preferred providing also lower RSDs of 1-6%. In comparison to methanol, commonly used as an extraction solvent for triazoles, acetone yielded similar extraction efficiencies for all analytes while reducing the time of sample concentration. The solid phase extraction method for triazoles was adapted to allow for a separation of ipbc and PER from the wood matrix. As opposed to previous studies, three recovery standards were employed, which enabled the correction of individual analyte losses during the sample preparation. The matrix-affected limits of detection (LODs) using gas chromatography with mass spectrometric detection were nearly the same for triazoles 0.07 and 0.21 ng g(-1) for PAZ and TAZ in sapwood and 0.18 and 0.21 ng g(-1) in heartwood, respectively. Higher LODs were observed for ipbc and PER: 3.9 and 1.7 ng g(-1) in sapwood, and 2.0 and 6.0 ng g(-1) in heartwood, respectively. The recoveries in the wood submitted to commercial sample treatment showed gradient distribution of analytes depending on the penetration of the treatment. (C) 2011 Elsevier B.V. All rights reserved.

关键词： Fungicide Gas chromatography-mass spectrometry Wood preservation Triazole ipbc Permethrin

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Penetration of 3-iodo-2-propynyl butylcarbamate (ipbc) in coniferous wood pre-treated with Physisporinus vitreus

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JOURNAL OF COATINGS TECHNOLOGY AND RESEARCH 2010年第6期7卷 721-726页

作者： Volkmer, Thomas Landmesser, Helge Genoud, Aline Schwarze, Francis W. M. R. Berner Fachhsch Architektur Holz & Bau CH-2500 Biel 6 Switzerland Swiss Fed Labs Mat Testing & Res EMPA Sect Wood Protect & Biotechnol Wood Lab St Gallen Switzerland Univ Freiburg D-79085 Freiburg Germany

The permeability of Norway spruce wood can be reduced to 1-5% of that of green timber when dried, resulting in only slight radial penetration of chemical solutions. We investigated the penetration of the biocide 3-iodo-2-propynyl butylcarbamate, (ipbc) in Norway spruce and Scots pine sapwood when applied in a water-based coating system. Penetration of both untreated wood and specimens pretreated with the white-rot fungus Physisporinus vitreus was analyzed by the absence or presence of blue staining after incubation with Aureobasidium pullulans and Sclerophoma pithyophila. The qualitative results were compared with quantitative data obtained by chemical analysis. It was assumed a pre-treatment with Physisporinus vitreus could make the surface of the substrate more porous and improve the penetration of fluid substances. All analytical investigations of the samples were done after an outdoor weathering period of 6 months. From a practical point of view the performance of the coated substrate is more relevant after a certain aging procedure then right after the application. The chemical measured uptake of ipbc for Scots pine was similar for all samples at the surface. The penetration depth was higher for those samples with a pre-treatment with Physisporinus vitreus. The colonization pattern of the samples by blue-stain fungi depended upon the pre-treatment but did not show a clear correlation between ipbc-content and staining. The cross-section of the samples with pre-treatment was completely stained, the cross-section of the samples without pre-treatment did show a distinctive blue stain-free zone. In Norway spruce, the chemical measured uptake of ipbc was similar for all samples at the surface independent of the pre-treatment. The penetration depth was higher for those samples with a pre-treatment with Physisporinus vitreus. But a clear visible colonization by blue-stain fungi was only observed for the samples with a pre-treatment with Physisporinus vitreus. The sampl

关键词： ipbc Fungi modification Water-based coating Blue stain

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Mixture toxicity assessment of wood preservative pesticides in the freshwater amphipod Gammarus pulex (L.)

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ECOTOXICOLOGY AND ENVIRONMENTAL SAFETY 2009年第2期72卷 441-449页

作者： Adam, Olivier Badot, Pierre-Marie Degiorgi, Francois Crini, Gregorio Univ Franche Comte CNRS UMR 6249 Chronoenvironm Dept F-25030 Besancon France

All over the world, insecticides and fungicides are used to protect wood against pathogens. To document the environmental toxicity of wood preservative mixtures, freshwater amphipods Gammarus pulex (L.) were submitted to organic pesticides given independently or in mixtures. When given independently at environmentally realistic concentrations, propiconazole and tebuconazole (triazoles fungicides) were not toxic for G. pulex, 3-iodo-2-propinyl butyl carbamate (ipbc, fungicide) was moderately toxic, and cypermethrin (pyrethroid insecticide) was extremely toxic. 96-h LC50 were, respectively, 4703, 1643, 604, and 0.09 mu g L-1. When amphipods were submitted to a mixture mimicking the composition of a commercial solution (18.2% of cypermethrin, 45.8% propiconazole, 17.2% tebuconazole, 18.8% ipbc), the overall toxicity was equal to that of the most toxic component, namely cypermethrin. But, when organisms were submitted to the real commercial mixture containing pesticides, solvents and additives, the toxic effects were markedly higher. Moreover, a third mixture with only 0.002% cypermethrin showed lethality 2.5-18-fold higher than those predicted by the commonly used models. The present results show that toxicity of wood preservative mixtures cannot be assessed starting only from the toxicities of each single component. Furthermore, the present data strongly suggest that the environmental impacts of wood preservative mixtures might be frequently underestimated. (C) 2008 Elsevier Inc. All rights reserved.

关键词： Wood preservative Mixture toxicity Additive Gammarus pulex Cypermethrin Propiconazole Tebuconazole ipbc

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Impacts of carbamate pesticides on olfactory neurophysiology and cholinesterase activity in coho salmon (Oncorhynchus kisutch)

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AQUATIC TOXICOLOGY 2004年第2期69卷 133-148页

作者： Jarrard, HE Delaney, KR Kennedy, CJ Simon Fraser Univ Dept Biol Sci Burnaby BC V5A 1S6 Canada

Many freshwater aquatic environments in the Pacific Northwest of North America contain neurotoxic pesticides, an issue of concern given the use of many of these habitats by Pacific salmon (Oncorhynchus sp.). Pesticides such as carbamates are known to affect fundamental physiological systems (such as the enzyme acetylcholinesterase (AChE)), and have been shown to affect salmonid olfactory-mediated behaviors. A neurophysiological measure of olfactory function, the electro-olfactogram (EOG), was used in this study to examine the impacts of acute localized exposure to three carbamates (the insecticide carbofuran, the antisapstain ipbc, and the fungicide mancozeb) on olfactory function in the coho salmon (Oncorhynchus kisutch). We also examine the potential for these pesticides to alter AChE levels in the,primary olfactory system and brain with brief exposures (30 min to only the olfactory rosette (OR)). In results, we find that the EOG in coho salmon is highly sensitive to brief localized exposures of two of these three carbamate pesticides. The effective nominal concentration required to cause a 50% reduction in EOG amplitude (EC50) for carbofuran was 10.4 mug/l and for ipbc was 1.28 mug/l. For mancozeb, the EC50 was higher at 2.05 mg/l. All three carbamates also affected AChE activity levels in the OR and brain (BR): carbofuran exposure at 200 mug/l significantly inhibited AChE activity in the OR, and both ipbc and mancozeb significantly increased AChE activity in BR at multiple concentrations with acute localized exposure. These carbamate effects highlight the sensitivity of salmon olfactory neurophysiology to pesticides acting not only potentially via AChE-inhibition, but also by other currently unknown modes of action. (C) 2004 Elsevier B.V. All rights reserved.

关键词： carbofuran ipbc mancozeb electro-olfactogram AChE

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用于上浆整理的织物防霉抑菌剂作用机制及应用研究

用于上浆整理的织物防霉抑菌剂作用机制及应用研究

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作者：李颖浙江理工大学

学位级别：硕士

纺织工业是中国传统优势产业、重要支柱产业和民生产业,高质量发展是实现纺织强国目标的必由之路。坯布是纺织织造、功能织物、高附加值产品的初始端。在沿海地区,梅雨季节坯布发霉异味是纺织工厂面临的共性问题,棉布甚至锦纶、涤纶等... 详细信息

纺织工业是中国传统优势产业、重要支柱产业和民生产业,高质量发展是实现纺织强国目标的必由之路。坯布是纺织织造、功能织物、高附加值产品的初始端。在沿海地区,梅雨季节坯布发霉异味是纺织工厂面临的共性问题,棉布甚至锦纶、涤纶等布匹的发霉是企业碰到的实际难题。为解决该问题,本文致力于筛选适用于浆料的防霉抑菌剂、探究复配防霉抑菌剂的协同机制、并验证其在坯布上的应用效果,以期寻找一种经济高效、可用于上浆整理的复合型防霉抑菌剂。本文使用了抑菌圈、最低抑菌浓度、最小杀菌浓度、联合抑菌指数、织物防霉测试等测试方法表征防霉抑菌剂及整理后织物的防霉抑菌性能;使用扫描电子显微镜、万能试验机、白度测试仪、视频接触角测量仪等设备,对整理前后织物的理化性能等进行了表征。并通过生产实践应用,对开发的复合型防霉抑菌剂应用于上浆整理的有效性进行了验证。1.用于上浆整理的防霉抑菌剂性能比较及应用。选择常见的四类防霉抑菌剂:碘丙炔基正丁胺甲酸酯(ipbc)、吡啶硫酮锌(ZPT)、辛基异噻唑啉酮(OIT)及氯化银(Ag Cl)作为研究对象,以产黄青霉和杂色曲霉为模型菌种,筛选出防霉效力高、与浆料配伍性好的防霉抑菌剂,探索与不同浆料(丙烯酸酯类、聚乙烯醇类、淀粉类)混合应用于不同织物(锦纶、涤纶、棉)上的防霉效果。结果表明:四种防霉抑菌剂对产黄青霉和杂色曲霉均有一定的抑菌效果。Ag Cl防霉剂的抑菌能力最强,对两种霉菌的最小杀菌浓度(MBC)值均为0.156 mg/m L,其次是ipbc和OIT,均为0.313 mg/m L。ipbc和OIT与浆料的配伍性较好,淀粉浆料显著促进ipbc和OIT的抑菌效果,但降低了ZPT和Ag Cl防霉剂抑菌能力的发挥,尤其影响Ag Cl防霉抑菌剂的效果。涤纶和棉织物经含0.2 wt%的防霉抑菌剂整理后,对两种霉菌的防霉等级均能达到0级或1级,丙烯酸酯类上浆的锦纶表现出较差的防霉效果。2.纺织品防霉抑菌剂的复配及协同效果研究。选用与浆料配伍性较好的三款防霉抑菌剂原材料ipbc、ZPT、OIT进行复配防霉抑菌效果研究,以产黄青霉和杂色曲霉为真菌模型菌种,定量探究三种防霉抑菌剂两两复配的联合抑菌效果,并通过联合抑菌指数对其作用效果进行评价,且测定了三者复配使用的最佳比例;以金黄色葡萄球菌和大肠杆菌为细菌模型菌种,测定复配防霉抑菌剂的抑菌率,并比较其对细菌的联合抑菌效果。对整理后的织物进行防霉抑菌评价和物理性能评价。结果表明:ipbc与ZPT对抑制产黄青霉有协同作用,对抑制杂色曲霉为无关作用;ipbc与OIT、ZPT与OIT对抑制产黄青霉和杂色曲霉均为协同作用。三种防霉抑菌剂组合对抑制金黄色葡萄球菌和大肠杆菌均无协同作用,联合抑菌指数显示出相加作用和无关作用。三种防霉剂复配的最佳比例为ipbc︰ZPT︰OIT=1︰1︰1,对产黄青霉和杂色曲霉的MBC值分别为0.02 mg/m L和0.03 mg/m L;对金黄色葡萄球菌和大肠杆菌的抑菌率均高于99%。最后将优化比例的复合型防霉抑菌剂应用于锦纶织物上,整理后的锦纶织物获得了显著的防霉抑菌能力,且白度和拉伸强度无明显下降。3.纺织品复合型防霉抑菌剂上浆整理的应用研究。从成本考虑,中试阶段防霉抑菌剂更换为国产试剂。将配方为ipbc︰ZPT︰OIT=1︰1︰1,总浓度为0.2 wt%的复合型防霉抑菌剂投入应用,在实验室测定国产复合型防霉抑菌剂的防霉能力。进一步,在纺织工厂进行锦纶坯布防霉整理的中试试验,通过对坯布开卷验布评级方法评价防霉效果。结果表明:相较于进口防霉抑菌剂,含有相同活性物的国产防霉剂可满足纺织品对防霉效果、白度和拉伸强度的要求,成本为0.03元/m。中试结果表明:织造后的坯布对产黄青霉和杂色曲霉的防霉等级分别为1级和0级;在保存5-18天的情况下,整理织物的A级率是未整理织物的4.7倍,显著降低了次品率(C级和D级)。本文为解决纺织工厂坯布发霉的问题,对防霉抑菌剂进行了筛选、复合及应用研究,证明了使用的防霉抑菌剂复配存在协同作用,并得到其复配最佳比例。通过成本计算和应用,文中使用的纺织品复配防霉抑菌剂经济实用、高效协同、操作简便,有望进一步扩宽商业化应用。

关键词：防霉剂抑菌剂复配协同上浆整理 OIT ipbc ZPT

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高效液相色谱测定防腐木中ipbc含量的方法研究

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木材科学与技术 2022年第5期36卷 71-77页

作者：张景朋张卿硕韩利平蒋明亮中国林业科学研究院木材工业研究所北京100091

为实现防腐处理材中碘代丙炔基丁基氨基甲酸酯(3-iodo-2-propynyl butylcarbamate,ipbc)含量的精确分析,建立ipbc的高效液相色谱(HPLC)分析方法,并对比研究了超声波提取方法中提取溶剂种类、溶剂用量、提取时间等因素对防腐杉木中ipbc... 详细信息

为实现防腐处理材中碘代丙炔基丁基氨基甲酸酯(3-iodo-2-propynyl butylcarbamate,ipbc)含量的精确分析,建立ipbc的高效液相色谱(HPLC)分析方法,并对比研究了超声波提取方法中提取溶剂种类、溶剂用量、提取时间等因素对防腐杉木中ipbc提取效果的影响。采用紫外检测器及C18反相色谱柱,优化得到分析ipbc的色谱条件:V_(乙腈)∶V_(水)=52∶48为流动相,流速1.0 mL/min,检测波长200 nm。ipbc在5~120 mg/L范围内,标准曲线决定系数为0.9998,具有显著线性相关;分析样品的变异系数0.66%,样品的回收率为99.5%~100.6%。超声波提取法中,在优化条件:V_(甲醇)∶V_(水)=7∶3、液料比20 mL/g、提取时间30 min,4种材料中ipbc的回收率为97.5%~106.4%,标准偏差在0.3%~2.6%。本方法可用于检测处理材中ipbc的含量,前处理程序简便快捷,准确度高,重现性好。

关键词： ipbc 高效液相色谱防腐木超声波提取方法

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化妆品中防腐剂ipbc的测定

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现代预防医学 2006年第5期33卷 839-840页

作者：刘奋戴京晶聂绍发深圳市福田区疾病预防控制中心华中科技大学同济医学院公共卫生学院流行病与卫生统计学系

目的:建立气相色谱测定化妆品中的防腐剂ipbc的方法。方法:用甲醇提取化妆品中的ipbc,用气相色谱法(GC-FID)定量,气相色谱—质谱法(GC/MS)确证。结果:方法检出限为0.18 ng;在10~100μg/ml范围内呈良好线性,相关系数大于0.995;回收率92.... 详细信息

目的:建立气相色谱测定化妆品中的防腐剂ipbc的方法。方法:用甲醇提取化妆品中的ipbc,用气相色谱法(GC-FID)定量,气相色谱—质谱法(GC/MS)确证。结果:方法检出限为0.18 ng;在10~100μg/ml范围内呈良好线性,相关系数大于0.995;回收率92.2%;相对标准偏差2.33%。结论:本方法适用于化妆品中ipbc的测定,简便,灵敏度高,特异性强。

关键词： ipbc 气相色谱法化妆品防腐剂

来源：中国生物医学学术期刊万方医学期刊

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ipbc防腐处理材的防腐性和抗流失性研究

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西北林学院学报 2010年第5期25卷 187-190页

作者：肖忠平陆继圣扬州工业职业技术学院建筑工程系江苏扬州225127 福建农林大学材料工程学院福建福州350002

对经过超临界CO2流体携带3-碘-2-丙炔基丁基氨基甲酸丁酯(ipbc)防腐剂处理后的杉木、马尾松以及中密度纤维板和刨花板的防腐性及ipbc防腐剂的抗流失性进行测定。结果表明,杉木、马尾松、中密度纤维板和刨花板经ipbc处理后,防腐能力都得... 详细信息

对经过超临界CO2流体携带3-碘-2-丙炔基丁基氨基甲酸丁酯(ipbc)防腐剂处理后的杉木、马尾松以及中密度纤维板和刨花板的防腐性及ipbc防腐剂的抗流失性进行测定。结果表明,杉木、马尾松、中密度纤维板和刨花板经ipbc处理后,防腐能力都得到了较大提高,在绵腐卧孔菌或彩绒革盖菌的腐蚀下杉木、马尾松的质量损失率降为10%以下,中密度纤维板和刨花板的质量损失率降为5%以下;ipbc防腐剂的抗流失性较好。

关键词： ipbc 防腐性能抗流失性能

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Biozide in Gebäudefassaden – ökotoxikologische Effekte, Auswaschung und Belastungsabschätzung für Gewässer

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Environmental Sciences Europe 2009年第1期21卷 36-47页

作者： M. Burkhardt M. Junghans S. Zuleeg M. Boller U. Schoknecht X. Lamani K. Bester R. Vonbank H. Simmler Abteilung Siedlungswasserwirtschaft Eawag – Das Wasserforschungs-Institut des ETH-Bereichs Dübendorf Schweiz BMG Engineering AG Schlieren Schweiz Fachgruppe IV.1 ‚Biologie im Umwelt- und Materialschutz‘ Bundesanstalt für Materialforschung und -prüfung (BAM) Berlin Deutschland Institut für Umweltanalytik Universität Duisburg-Essen Essen Deutschland Department of Biotechnology Chemistry and Environmental Engineering Universität Aalborg Aalborg Dänemark Abteilung Bautechnologien Eidgenössische Materialprüfungs- und Forschungsanstalt (Empa) Dübendorf Schweiz

Hintergrund, Ziel und Zweck Die Belastung von Flieβgewässern durch organische Mikroverunreinigungen wirft häufig die Frage der Quellenzuordnung auf. Baumaterialien als Quellen problematischer Spurenstoffe finden in der Gewässerbeurteilung bisher wenig Beachtung, obwohl bereits heute biozide Wirkstoffe aus Materialschutzanwendungen zu einer Belastung des Regenwasserabflusses führen. In der vorliegenden Untersuchung wurden (1) die ökotoxikologischen Kenngrößen für typische Biozide in Fassadenbeschichtungen ermittelt, (2) die Auswaschung von besonders problematischen Bioziden aus Fassaden quantifiziert und (3) das Belastungsrisiko für Gewässer mittels Stofftransportmodellierung abgeschätzt. Methoden Acht Biozide wurden untersucht, die in kunstharzgebundenen Fassadenbeschichtungen verwendet werden. Dazu gehören auch Wirkstoffe, deren Umwelteintrag bisher eher der Landwirtschaft zugerechnet wurde, z. B. Diuron, Carbendazim und Terbutryn. Für jedes Biozid wurden ökotoxikologische Qualitätskriterien für aquatische Organismen bestimmt. Die Auswaschung von vier Bioziden aus einer verputzten Fassade wurde im Laborversuch unter Berücksichtigung von UV-Bestrahlung untersucht, wobei die Temperatur variiert wurde. Über 80 Beregnungsintervalle in 28 Tagen wurden Proben des Fassadenabflusses entnommen, die Wirkstoffkonzentrationen gemessen und die ausgewaschenen Wirkstoffmengen berechnet. Basierend auf einem Austragsszenario wurde das mögliche Belastungsrisiko im Gewässer durch das Biozid Cybutryn mit einer Stofftransportmodellierung abgeschätzt. Die ermittelten wirkstoffspezifischen Qualitätskriterien und die Auswaschcharakteristik wurden darin berücksichtigt. Ergebnisse Die akuten und chronischen Kriterien sowie vorhergesagten Konzentrationen ohne Effekt weisen auf eine hohe Ökotoxizität der betrachteten Biozide hin. Die Ergebnisse zum Auswaschungsverhalten von vier Bioziden (Diuron, Terbutryn, Cybutryn und Carbendazim) zeigen, dass die Wirkstoffe im Fassadenabfluss vorkommen und

关键词： Auswaschung Baumaterialien Biozide Carbendazim Cybutryn DCOIT Diuron Fassaden ipbc Irgarol ® 1051 Modellierung OIT Ökotoxikologische Effekte Risikobewertung Terbutryn Zinkpyrithion Biocides Carbendazim Construction products Cybutryn DCOIT Diuron Ecotoxicological effects Environmental risk assessment Facades ipbc Irgarol ® 1051 Leaching Modelling OIT Terbutryn Zinc pyrithione

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Performance of copper and non-copper based wood preservatives in terrestrial microcosms

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HOLZFORSCHUNG 1999年第4期53卷 369-375页

作者： Edlund, ML Nilsson, T Swedish Univ Agr Sci Dept Wood Sci S-75007 Uppsala Sweden

The use of wood preservatives based on copper, chromium and arsenic (CCA) has become restricted in several countries due to environmental concerns. As a consequence, several chromium and arsenic free preservatives based on fungicides, regarded as more environmentally acceptable, have been developed. Most of these preservatives have only been tested in the laboratory against pure cultures of basidiomycetes and their long term effectiveness in practice is in many cases unknown. The effectiveness of six different preservatives, representing different types and combinations of fungicides, against mixed natural populations of micro-organisms, was evaluated during one year in terrestrial microcosms with soils known to provide high activity of different types of wood destroying micro-organisms. Of the fungicides tested, copper compounds provided the best protection against wood destroying micro-organisms. Copper free preservatives provided good protection against pure cultures of brown- and white rot fungi, but were ineffective when treated stakes were exposed in unsterile soils.

关键词： terrestrial microcosms azaconazole tebuconazole propiconaozle Cu-HDO ipbc benzalconium chloride DDAC CCA

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