Name: ultrafast lignin extraction from unusual mediterranean lignocellulosic residues
Uploaded: 2021-03-09T12:30:00
Description: Watch this Scientific Journal Video about Ultrafast Lignin Extraction from Unusual Mediterranean Lignocellulosic Residues at JoVE.com

MK 和 TB 感谢海瑟姆 ·阿耶布的统计分析和数字准备，瓦隆地区（欧洲区域发展-VERDIR）和高等教育和科学研究部长（陶菲克·贝塔伊布）提供资金。

1. 生物质的制备
<ol><li>生物质干燥<ol>
<li>将从地中海海滩收获的波西多尼亚叶子和大洋球（波西多尼亚海洋）放在40°C的烤箱中，72小时。</li>
		<li>将来自食品工业的杏仁壳（普鲁努斯杜丽花）和从橄榄油厂获得的橄榄果壳（欧罗巴利亚 L.）放在 40 °C 的烤箱中，以 72 小时的速度放置。</li>
		<li>将从森林中收集的松果（皮努斯哈莱彭西斯）和从地中海南部盆地收集的阿?...

<ol>
	<li>Kammoun, M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Hydrothermal+dehydration+of+monosaccharides+promoted+by+seawater+fundamentals+on+the+catalytic+role+of+inorganic+salts.">Hydrothermal dehydration of monosaccharides promoted by seawater fundamentals on the catalytic role of inorganic salts.</a> Frontiers in Chemistry. 7, 132 (2019).</li><li>Kammoun, M., Ayeb, H., Bettaieb, T., Richel, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Chemical+characterisation+and+technical+assessment+of+agri-food+residues,+marine+matrices,+and+wild+grasses+in+the+South+Mediterranean+area:+A+considerable+inflow+for+biorefineries.">Chemical characterisation and technical assessment of agri-food residues, marine matrices, and wild grasses in the South Mediterranean area: A considerable inflow for biorefineries.</a> Waste Management. 118, 247-257 (2020).</li><li>Zhang, C. W., Xia, S. Q., Ma, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Facile+pretreatment+of+lignocellulosic+biomass+using+deep+eutectic+solvents.">Facile pretreatment of lignocellulosic biomass using deep eutectic solvents.</a> Bioresource Technology. 219, 1-5 (2016).</li><li>Mora-Pale, M., Meli, L., Doherty, T. V., Linhardt, R. J., Dordick, J. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Room+temperature+ionic+liquids+as+emerging+solvents+for+the+pretreatment+of+lignocellulosic+biomass.">Room temperature ionic liquids as emerging solvents for the pretreatment of lignocellulosic biomass.</a> Biotechnology and Bioengineering. 108 (6), 1229-1245 (2011).</li><li>Chen, Z., Wan, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ultrafast+fractionation+of+lignocellulosic+biomass+by+microwave-assisted+deep+eutectic+solvent+pretreatment.">Ultrafast fractionation of lignocellulosic biomass by microwave-assisted deep eutectic solvent pretreatment.</a> Bioresource Technologie. 250, 532-537 (2018).</li><li>Francisco, M., Van Den Bruinhorst, A., Kroon, M. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=New+natural+and+renewable+low+transition+temperature+mixtures+(+LTTMs+):+screening+as+solvents+for+lignocellulosic+biomass+processing.">New natural and renewable low transition temperature mixtures ( LTTMs ): screening as solvents for lignocellulosic biomass processing.</a> Green Chemistry. 14 (8), 2153-2157 (2012).</li><li>Liu, Y. C., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Efficient+cleavage+of+lignin+-+carbohydrate+complexes+and+ultrafast+extraction+of+lignin+oligomers+from+wood+biomass+by+microwave-assisted+treatment+with+deep+eutectic+solvent.">Efficient cleavage of lignin - carbohydrate complexes and ultrafast extraction of lignin oligomers from wood biomass by microwave-assisted treatment with deep eutectic solvent.</a> Chem sus chem. 10, 1692-1700 (2017).</li><li>Xu, G. C., Ding, J. C., Han, R. Z., Dong, J. J., Ni, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Enhancing+cellulose+accessibility+of+corn+stover+by+deep+eutectic+solvent+pretreatment+for+butanol+fermentation.">Enhancing cellulose accessibility of corn stover by deep eutectic solvent pretreatment for butanol fermentation.</a> Bioresource Technologie. 203, 364-369 (2016).</li><li>Jablonsk&#253;, M., Andrea, &. #. 3. 5. 2. ;., Kamensk&#225;, L., Vr&#353;ka, M., &#352;ima, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Deep+eutectic+solvents+fractionation+of+wheat+straw+deep+eutectic+solvents+fractionation+of+wheat+straw.">Deep eutectic solvents fractionation of wheat straw deep eutectic solvents fractionation of wheat straw.</a> Bioresources. 10 (4), 8039-8047 (2015).</li><li>Shen, X. J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Facile+fractionation+of+lignocelluloses+by+biomass-derived+deep+eutectic+solvent+(DES)+pretreatment+for+cellulose+enzymatic+hydrolysis+and+lignin+valorization.">Facile fractionation of lignocelluloses by biomass-derived deep eutectic solvent (DES) pretreatment for cellulose enzymatic hydrolysis and lignin valorization.</a> Green Chemistry. 21, 275-283 (2019).</li><li>Alvarez-Vasco, C., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Unique+low-molecular-weight+lignin+with+high+purity+extracted+from+wood+by+deep+eutectic+solvents+(DES):+a+source+of+lignin+for+valorization.">Unique low-molecular-weight lignin with high purity extracted from wood by deep eutectic solvents (DES): a source of lignin for valorization.</a> Green Chemistry. 18, 5133-5141 (2016).</li><li>Banu, J. R., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+review+on+biopolymer+production+via+lignin+valorization.">A review on biopolymer production via lignin valorization.</a> Bioresource Technologie. 290, 121790 (2019).</li><li>Gordobil, O., Olaizola, P., Banales, J. M., Labidi, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Lignins+from+agroindustrial+by-products+as+natural+ingredients+for+cosmetics+chemical+structure+and+in+vitro+sunscreen+and+cytotoxic+activities.">Lignins from agroindustrial by-products as natural ingredients for cosmetics chemical structure and in vitro sunscreen and cytotoxic activities.</a> Molecules. 25 (5), 1131 (2020).</li><li>Lee, C. S., Thu Tran, T. M., Weon Choi, J., Won, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Lignin+for+white+natural+sunscreens.">Lignin for white natural sunscreens.</a> International Journal of Biological Macromolecules. 122, 549-554 (2019).</li><li>Widsten, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Lignin-based+sunscreens-state-of-the-art,+prospects+and+challenges.">Lignin-based sunscreens-state-of-the-art, prospects and challenges.</a> Cosmetics. 7, 85 (2020).</li><li>Qian, Y., Qiu, X., Zhu, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Lignin:+a+nature-inspired+sun+blocker+for+broad-spectrum+sunscreens.">Lignin: a nature-inspired sun blocker for broad-spectrum sunscreens.</a> Royal Society of Chemistry. 17, 320-324 (2015).</li><li>Zijlstra, D. S., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Extraction+of+lignin+with+high+&#946;-O-4+content+by+mild+ethanol+extraction+and+its+effect+on+the+depolymerization+yield.">Extraction of lignin with high &#946;-O-4 content by mild ethanol extraction and its effect on the depolymerization yield.</a> Journal of Visualized Experiments. (143), e58575 (2019).</li></ol>

这项研究有许多目标：首先是准备和使用具有离子液体和有机溶剂特性的低成本绿色溶剂。第二个目标是将生物量分成一步，提取木质素，而不需要初步步骤，例如使用碱性溶剂、基本或热物理技术使用 Soxhlet 或半纤维素提取可提取物。第三个目标是在治疗后通过简单的过滤来恢复木质素，无需调整pH度，而只需加入蒸馏水即可。使用微波辅助的基于 DES 的工艺从六种不同来源超高速提取木质素的...

可持续的生物精炼过程将生物质加工、其分馏成感兴趣的分子，并转化为增值产品1。在第二代生物修复中，预处理被认为是将生物质分成主要成分2的必要条件。利用化学、物理或生物策略的传统预处理方法已得到广泛应用。然而，这种预处理被认为是生物修复中最昂贵的一步，并具有其他缺点，如加工时间长，热和功耗高，溶剂杂质4。最近，DESs的特性与离子液体3相似，由于生物降解性、环保性、易合成性、治疗后恢复等优点，成为绿色溶剂。
DES 是至少一种 HBD 的混合物，如乳酸、粘液酸或草酸，以及氢键接受剂 （HBA） 的混合物，如贝坦或氯化胆 （ChCl）6。HBA-HBD 相互作用使催化机制能够使化学键裂开，导致生物质分裂和木质素分离。许多研究人员已经报告了基于DES的木质细胞素原料的预处理，如玉米棒上的ChCl-甘油和7号、8号、ChCl-尿素、 小麦稻草上的ChCl-草酸9，桉树锯末上的ChCl-乳酸10，木材上的ChCl-醋酸11和木上的ChCl-乙烯乙二醇。为了提高DES效率，预处理应与微波处理相结合，以加速生物质分馏5。许多研究人员报告了这种对8号木和玉米茎、开关草和米斯坎图斯5号的联合预处理（DES和微波），这为在短时间内对DES在木质细胞分馏和木质素提取方面的能力提供了新的见解。
木质素是一种酚类巨分子，作为生物聚合物生产的原料，是芳香单体和寡聚物等化学物质生产的替代品。此外，木质素具有抗氧化和紫外线吸收活动13。一些研究已经报告了木质素在化妆品中的应用14，15。其在商业防晒产品的集成改善了产品的防晒系数（SPF）从SPF 15到SPF 30，只增加了2 wt % 的木质素和高达SPF 50，增加了10瓦特%的木质素16。本文描述了一种超快的木质素 - 碳水化合物方法，辅之以地中海生物量的 DES - 微波预处理。这些生物量由农业食品副产品组成，特别是橄榄豆和杏仁壳。被调查的其他生物量是海洋原产物（波西多尼亚叶和海生物）和源自森林的生物量（松果和野生草）。本研究的重点是测试低成本的绿色溶剂，以评估这种联合预处理对原料分馏的影响，调查其对木质素纯度和产量的影响，并研究其对提取木质素中的分子量和化学功能组的影响。

<table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always">
	<tbody>
		<tr>
			<td>HPLC Gel Permeation Chromatography</td>
			<td>Agilent 1200 series</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>1 methylimadazole</td>
			<td>Acros organics</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>2-deoxy-D-glucose (internal standard)</td>
			<td>Sigma Aldrich (St. Louis, USA)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Acetic acid</td>
			<td>Sigma Aldrich (St. Louis, USA)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Acetic anhydride</td>
			<td>Sigma Aldrich (St. Louis, USA)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Adjustables pipettors</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Alkali</td>
			<td></td>
			<td></td>
			<td>alkali-extracted lignin</td>
		</tr>
		<tr>
			<td>Arabinose (99%)</td>
			<td>Sigma Aldrich (St. Louis, USA)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Autoclave</td>
			<td>CERTO CLAV (Model CV-22-VAC-Pro)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Water Bath at 70 &#176;C</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Boric acid</td>
			<td>Sigma Aldrich (St. Louis, USA)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Bromocresol</td>
			<td>Sigma Aldrich (St. Louis, USA)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Catalyst</td>
			<td>CTQ (coded A22) (1.5 g K2SO4 + 0.045 g CuSO4.5 H2O + 0.045 g TiO2)</td>
			<td>Merck</td>
			<td></td>
		</tr>
		<tr>
			<td>Centrifugation container</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Centrifuge</td>
			<td>BECKMAN COULTER</td>
			<td>Avanti J-E centrifuge</td>
			<td></td>
		</tr>
		<tr>
			<td>Ceramic crucibles</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Choline chloride 99%</td>
			<td>Acros organics</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Column</td>
			<td>Agilent PLGel Mixed C (alpha 3,000 (4.6 &#215; 250 mm, 5 &#181;m) preceded by a guard column (TSK gel alpha guard column 4.6 mm &#215; 50 mm, 5 &#181;m)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Column</td>
			<td>HP1-methylsisoxane (30 m, 0.32 mm, 0.25 mm)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Crucible porosity N&#176;4 ( Filtering crucible)</td>
			<td>Shott Duran Germany</td>
			<td>boro 3.3</td>
			<td></td>
		</tr>
		<tr>
			<td>Deonized water</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Dessicator</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Dimethylformamide</td>
			<td>VWR BDH Chemicals</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Dimethylsulfoxide</td>
			<td>Acros organics</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Erlenmeyer flask</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Ethanol</td>
			<td>Merck (Darmstadtt, Germany)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Filtering crucibles, procelain</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Filtration flasks</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Fourrier Transformed Inra- Red</td>
			<td>Vertex 70 Bruker apparatus 
			equipped with an attenuated total reflectance (ATR) module. 
			Spectra were recorded in the 4,000&#8211;400 cm&#8722;1 range with 32 scans 
			at a resolution of 4.0 cm&#8722;1</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Galactose (98%</td>
			<td>Sigma Aldrich (St. Louis, USA)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Gaz Chromatography</td>
			<td>Agilent (7890 series)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Glass bottle 100 mL</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Glass tubes ( borosilicate) with teflon caps 10 mL</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Glucose (98%</td>
			<td>Sigma Aldrich (St. Louis, USA)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Golves</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Graduated cylinder 50 mL /100 mL</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>H2SO4 Titrisol (0.1 N)</td>
			<td>Merck (Darmstadtt, Germany)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>H2SO4 (95-98%)</td>
			<td>Sigma Aldrich (St. Louis, USA)</td>
			<td>BUCHI R-114)</td>
			<td></td>
		</tr>
		<tr>
			<td>Hummer cutter equiped with 1 mm and 0.5 mm sieve</td>
			<td>Mill Ttecator (Sweden)</td>
			<td>Cyclotec 1093</td>
			<td></td>
		</tr>
		<tr>
			<td>Indulin</td>
			<td></td>
			<td></td>
			<td>Raw lignin control</td>
		</tr>
		<tr>
			<td>Kjeldahl distiller</td>
			<td>Kjeltec 2300 (Foss)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Kjeldahl tube</td>
			<td>FOSS</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Kjeldhal rack</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Kjeldhal digester</td>
			<td>Kjeltec 2300 (Foss)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Kjeldhal suction system</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Lab Chem station Software</td>
			<td></td>
			<td></td>
			<td>GC data analysis</td>
		</tr>
		<tr>
			<td>Lactic acid</td>
			<td>Merck (Darmstadtt, Germany)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Lithium chloride LiCl</td>
			<td>Sigma Aldrich (St. Louis, USA)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Mannose (98%)</td>
			<td>Sigma Aldrich (St. Louis, USA)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Methyl red</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Microwave</td>
			<td>START SYNTH MILESTONE Microwave laboratory system</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Microwave temperature probe</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Microwave container</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Muffle Furnace</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>NaOH</td>
			<td>Merck (Darmstadtt, Germany)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Nitrogen free- paper</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Opus</td>
			<td></td>
			<td></td>
			<td>spectroscopy software</td>
		</tr>
		<tr>
			<td>Oven</td>
			<td>GmbH Memmert SNB100</td>
			<td>Memmert SNB100</td>
			<td></td>
		</tr>
		<tr>
			<td>Oxalic acid</td>
			<td>VWR BDH Chemicals</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>P 1000</td>
			<td></td>
			<td></td>
			<td>Soda-processed lignin</td>
		</tr>
		<tr>
			<td>pH paper</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>precision balance</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Infrared spectroscopy</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Quatz cuvette</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Rhamnose (98%)</td>
			<td>Sigma Aldrich (St. Louis, USA)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Rotary vacuum evaporator</td>
			<td>Bucher</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Round-bottom flask 500 mL</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>sodium borohydride NaBH4</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Schott bottle</td>
			<td></td>
			<td></td>
			<td>glass bottle</td>
		</tr>
		<tr>
			<td>Sovirel tubes</td>
			<td>sovirel</td>
			<td></td>
			<td>Borosilicate glass tubes</td>
		</tr>
		<tr>
			<td>Spatule</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Special tube</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Spectophotometer</td>
			<td>UV-1800 Shimadzu</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Sterilization indicator tape</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Stir bar in teflon</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Stirring plate</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Syringes</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Sodium borohydride</td>
			<td>Sigma Aldrich (St. Louis, USA)</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Titrisol</td>
			<td>Merck</td>
			<td>Merck 109984</td>
			<td>0.1 N H2SO4</td>
		</tr>
		<tr>
			<td>Urea</td>
			<td>VWR BDH Chemicals</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Vials</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>VolumetriC flask 2.5 L /5 L</td>
			<td>Bucher</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Vortex</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Xylose (98%)</td>
			<td>Sigma Aldrich (St. Louis, USA)</td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

ultrafast lignin extraction from unusual mediterranean lignocellulosic residues

预处理仍然是木质细胞学生物精炼过程中最昂贵的一步。它必须通过最大限度地减少化学需求、功率和热量消耗以及使用环保溶剂来实现成本效益。深乳酸盐溶剂 （DES） 是可持续生物定义中的关键、绿色和低成本溶剂。它们是透明混合物，其特点是至少由一个氢键供体和一个氢键接受者产生的低冰点。虽然 DES 是很有前途的溶剂，但有必要将其与经济加热技术（如微波辐照）相结合，以获得具有竞争力的盈利能力。微波辐照是缩短加热时间和提高分馏的一项很有前途的策略，因为它可以迅速达到适当的温度。本研究的目的是开发一种单步、快速的生物质分馏和木质素提取方法，使用低成本和可生物降解的溶剂。 
在这项研究中，使用三种DES进行了60年代的微波辅助DES预处理，在800 W。DES混合物由胆碱氯化物（ChCl）和三个氢键捐赠者（HBDs）简单制备：单碳酸（乳酸）、二甲基糖酸（草酸）和尿素。这种预处理用于从海洋残留物（波西多尼亚叶和藻类）、农业食品副产品（杏仁壳和橄榄果）、森林残留物（松果）和常年木质细胞草（斯蒂帕特纳西西玛）中恢复生物质分馏和木质素。进一步分析以确定回收木质素的产量、纯度和分子重量分布。此外，DESs对提取木质素中的化学功能组的影响由富利埃转化红外（FTIR）光谱仪确定。结果表明，ChCl-草酸混合物具有最高的木质素纯度和最低的产量。本研究表明，DES微波工艺是一种超高速、高效且具有成本竞争力的木质细胞生物质分馏技术。

图2A-C描绘了在混合微波-DES预处理后从图1A-F中显示的六种原料中提取的木质素产量。结果表明，DES1（ChCl-草酸）（图2A）获得的木质素产量低于DES2（氯化物酸）和DES3（ChCl-尿素）（图2B，C）获得的产量。此外，松果（PC）和橄榄波?...

Watch this Scientific Journal Video about Ultrafast Lignin Extraction from Unusual Mediterranean Lignocellulosic Residues at JoVE.com

Ultrafast Lignin Extraction from Unusual Mediterranean Lignocellulosic Residues

深乳酸溶剂基，微波辅助预处理是一个绿色，快速，高效的过程，为木质细胞分馏和高纯度木质素回收。

超高速利格宁从不寻常的地中海木质细胞残留物中提取

Pretreatment is still the most expensive step in lignocellulosic biorefinery processes. It must be made cost-effective by minimizing chemical requirements ...

我们协议的目的是将生物量分成一步，提取木质素。使用这种方法，木质素可以通过简单的过滤后处理，而不调整pH度，但只需添加蒸馏水恢复。本研究的重点是评估这种原料分馏联合处理的影响，它对木质素纯度和产量的影响，以及它对提取的木质素中的分子量和化学功能组的影响。深乳酸溶液微波工艺是一种超快、高效、具有成本竞争力的木质细胞生物质分馏和高纯度木质素回收技术。按照文本手稿中描述的，在 500 毫升圆形底部烧瓶中准备深真皮溶液。然后将5克原料、50毫升深乳酸溶液和搅拌棒放在封闭的聚二甲苯反应堆的微波炉中。用适当的盖子关闭微波容器，并附加温度上限。将其放在转盘边缘，确保它不断激动并运行微波炉一分钟。使用合适的手套，将容器从微波炉中取出，让混合物冷却。准备同质抗溶剂溶液，并在处理过的原料中加入 50 毫升的溶液。用玻璃滤芯将混合物离心5分钟，3000倍G.过滤超自然物。收集剩余的纤维素残留物，通过添加25毫升抗溶剂溶液和离心液进行清洗。将过滤的富含木质素的馏分和过滤后的洗涤添加到 500 毫升圆底烧瓶中。在 50 摄氏度和 110 毫巴下使用旋转蒸发器蒸发乙醇。然后在浓缩的白酒中加入150毫升的除离子水。通过离心沉淀木质素。收集木质素作为颗粒，用25毫升蒸馏水洗四次。然后将木质素合二为一，或在40摄氏度的烤箱中干燥。将滤芯放在 550 摄氏度的消声炉中，放置四个小时。当烤箱冷却到150摄氏度时，取出熔炉，放在干燥器中冷却。然后称它。将大约30毫克的木质素加入博罗西酸玻璃管中。然后在样品中加入一毫升72%的硫磺，放在30摄氏度的浴缸中60分钟。取出样品并将其转移到 100 毫升玻璃瓶中。然后加入28毫升蒸馏水，将酸稀释到4%的浓度，将玻璃瓶放入121摄氏度的高压灭菌器中60分钟。然后从高压灭菌剂中取出瓶子，让它冷却。要分析酸不溶性木质素，使用真空下熔炉过滤水解盐，并用除离子水收集玻璃瓶中的剩余固体。将含有固体的熔炉放入 105 摄氏度的烤箱中干燥 16 小时。然后在干燥器中冷却并称量样品。将熔炉放在550摄氏度的消声炉中，放置4小时。在干燥器中干燥后称重样品。用于分析酸溶性木质素，使用光谱仪测量水解盐过滤的吸收量，温度为 205 纳米，使用石英小瓶。要分析提取木质素的化学功能，处理背景单通道无样品。然后调整参数，将样品的一毫克放在晶体上。按样品单通道并处理获得光谱。为了确定提取的木质素的分子量，用0.5%氯化锂溶解三毫升DMF中的三毫克木质素样品。将溶解的木质素放入小瓶中，然后安装由护栏进行的柱子。将样品注入高性能液相色谱紫外线系统。分析数据后，计算文本稿件中描述的提取木质素的分子量。在玻色酸玻璃管中称量50毫克的木质素样本，并加入三毫升一摩尔硫酸。然后在100摄氏度下加热混合物3小时，冷却。加入一毫升15摩尔氢氧化铵，并检查pH值，以确保它是中性或碱性。作为内部标准，在每个样品中加入一毫升2脱氧糖。然后将此溶液中的 400 微升添加到包含 400 微升混合溶液的特殊管中。加入两毫升二甲基硫化钠溶液。关闭管子，在40摄氏度的水浴中孵育90分钟。从水浴中取出管子，加入0.6毫升冰川醋酸、0.4毫升1甲基苯甲酸和约4毫升醋酸。15分钟后，加入10毫升蒸馏水。凉。并加入大约三毫升二氯甲烷。两小时后，收集大约一毫升的下有机相，并注入装有火焰电离探测器毛细管柱的气相色谱仪中。用深乳酸溶液获得的木质素产量一草酸低于深乳酸溶液获得的产量，二是乳酸和深乳酸溶液三尿素。三种生物质的预处理，除深乳酸溶液外，三尿素预处理α叶、艾加罗皮拉和杏仁壳的纯度均超过70%，其中木质素纯度最高超过90%，是用深乳酸溶液获得的一种治疗方法。木质素纯度和产量数据经过主要成分分析，结果表明深乳酸溶液一种处理方法与木质素纯度呈正相关，并确认其为产量最低的最纯木质素。使用深乳酸溶液提取的木质素中的糖含量为最高，其次是从二号和一号溶液中提取的糖含量。同样，深乳酸溶液一个木质素提取物的氮含量低于从第二和第三溶液中获得的氮含量。提取的木质素中的糖类型也具有特征，将D-xylose和D-葡萄糖描述为最丰富的单糖。FTIR光谱仪对提取的石灰因中存在的化学功能组进行了研究。此处介绍了 3，500 到 800 公分之间不同利格纳的红外光谱。用深乳酸溶液提取的木质素光谱一和二显示了未受损害和共生的碳基组的拉伸振动，这在三种商业利格南中是不存在的：生、苏打加工和碱提取的石灰。车箱酸信号C双键O表示某些木质素功能与酸在提取过程中与酸结合的可能性，并与微波辅助深乳酸溶剂处理溶解。这些结果表明，有可能从地中海生物质中提取高纯度的高附加值木质素，目前这种物质被低估，有助于确定最佳的深乳酸溶剂，同时确保木质素的纯度。

Research

JoVE Journal

Chemistry

Towards Biomimicking Wood: Fabricated Free-standing Films of Nanocellulose, Lignin, and a Synthetic Polycation

朝仿生学木：纳米纤维素，木质素的装配式自由站立电影和合成聚阳离子

Woody materials are comprised of plant cell walls that contain a layered secondary cell wall composed of structural polymers of polysaccharides and ...

科研

化学

Preparing Silica Aerogel Monoliths via a Rapid Supercritical Extraction Method

通过快速超临界萃取法制备二氧化硅气凝胶巨石

A procedure for the fabrication of monolithic silica aerogels in eight hours or less via a rapid supercritical extraction process is described. The ...

Optimization of Synthetic Proteins: Identification of Interpositional Dependencies Indicating Structurally and/or Functionally Linked Residues

优化合成蛋白质：Interpositional依赖性的鉴定指示在结构和/或功能性连接的残留

Protein alignments are commonly used to evaluate the similarity of protein residues, and the derived consensus sequence used for identifying functional ...

Direct Imaging of Laser-driven Ultrafast Molecular Rotation

激光驱动的超快分子旋转直接成像

We present a method for visualizing laser-induced, ultrafast molecular rotational wave packet dynamics. We have developed a new 2-dimensional Coulomb ...

A Straightforward Method for Glucosinolate Extraction and Analysis with High-pressure Liquid Chromatography (HPLC)

A Straightforward Method for Glucosinolate Extraction and Analysis with High-pressure Liquid Chromatography HPLC

简捷方法对硫甙的提取与分析用高压液相色谱法（HPLC）

Glucosinolates are a well-studied and highly diverse class of natural plant compounds. They play important roles in plant resistance, rapeseed oil ...

Extraction and Purification of Polyphenols from Freeze-dried Berry Powder for the Treatment of Vascular Smooth Muscle Cells In Vitro

Extraction and Purification of Polyphenols from Freeze-dried Berry Powder for the Treatment of Vascular Smooth Muscle Cells In Vitro

从冷冻干燥的浆果粉中提取和纯化多酚用于治疗血管平滑肌细胞<em&gt;体外</em

Epidemiological studies indicate that increased flavonoid intake correlates with decreased mortality due to cardiovascular diseases (CVD) in the United ...

Fabrication and Testing of Catalytic Aerogels Prepared Via Rapid Supercritical Extraction

快速超临界萃取制备催化气凝胶的制备与试验研究

Protocols for preparing and testing catalytic aerogels by incorporating metal species into silica and alumina aerogel platforms are presented. Three ...

Microfluidic Chips for In Situ Crystal X-ray Diffraction and In Situ Dynamic Light Scattering for Serial Crystallography

Microfluidic Chips for In Situ Crystal X-ray Diffraction and In Situ Dynamic Light Scattering for Serial Crystallography

用于原位晶体 x 射线衍射和原位的微流控芯片系列晶体学的动态光散射

This protocol describes fabricating microfluidic devices with low X-ray background optimized for goniometer based fixed target serial crystallography. The ...

Separation of Aldehydes and Reactive Ketones from Mixtures Using a Bisulfite Extraction Protocol

用亚硫酸氢萃取协议分离混合物中的醛和反应性酮

The purification of organic compounds is an essential component of routine synthetic operations. The ability to remove contaminants into an aqueous layer ...

Measurement of Ultrafast Vibrational Coherences in Polyatomic Radical Cations with Strong-Field Adiabatic Ionization

强场绝热电离多原子自由基阳离子超快振动相干的测量

We present a pump-probe method for preparing vibrational coherences in polyatomic radical cations and probing their ultrafast dynamics. By shifting the ...