我们要感谢台湾科技部 (104-2628-E-002-008-MY3; 105-2218-155-007; 105-2221-e-002-003-MY3; 105-2221-e-002-227-MY3; 105-2622-e-155-003-CC2) 与国立台湾顶尖大学项目的目标大学 (105R7706) 为资金支持。我们感谢世界银行通过一项高等教育质量提高项目 (HEQEP) 的分项目, #2071 的完整建议, 为这项工作提供部分资金。这项工作也得到了卧龙岗大学 AIIM (金基金) 的部分支持。

在呈现的工作中使用的几种化学物质是有毒和致癌的。在执行 IL 和生物量处理的合成时, 请使用所有适当的安全做法。
1. 酸性 IL 的制备
<ol><li>在50毫升的圆底烧瓶中加入7.625 毫摩尔 13-丙烷 sultone, 然后用橡胶隔膜关闭烧瓶。</li>
	<li>使用注射器 (10 毫升) 在0°c 添加7.625 毫摩尔 1-甲基咪唑到7.625 毫摩尔 13-propanesultone 缓慢 (1 分钟)。</li>
	<li>在完全添加 1-甲基咪唑和 13-propanesultone 后, 加入15毫升的干甲苯和回流的混合物 16 h 在120°c 得到固体两性离子。</li>
	<li>用过滤法将两性离子与甲苯分离, 然后用40毫升甲苯清洗两性离子。为烘干两性离子, 设置烤箱温度到80°c。一旦烤箱温度达到80摄氏度, 保持在烤箱中的样品为4小时, 然后使用干两性离子在下一步。</li>
	<li>用1000µL 微将硫酸加入含有两性离子 (两性离子和硫酸等摩尔) 的圆底烧瓶中。然后将圆底烧瓶连接到回流冷凝器。加热和搅拌的混合物在110°c 12 小时得到理想的 IL。 注: 硫酸与两性离子的反应不含任何溶剂。</li>
	<li>在酸性 IL 合成后, 使用1H 和13C 核磁共振波谱对其进行表征。</li>
</ol>2. 哈米特酸度的测定 (Ho)
<ol><li>在1升容积瓶中添加10毫克的p-硝基苯胺指示器, 然后添加蒸馏水, 使1升溶液。用手摇动溶液2分钟, 离开溶液1小时, 将p-硝基苯胺混合在水中 (空白溶液)。</li>
	<li>添加1.59 毫摩尔的 H + 离子的酸性催化剂 (HCl/H 2, 所以 4/酸性 IL) 到50毫升的 p-硝基苯胺指示剂溶液, 并用手摇动溶液搅拌 (样品溶液). 注意当前工作中使用的所有酸性催化剂 (HCl、H2所以4和酸性 IL) 分别添加在 50 mL 指示器解决方案 (表 1) 中, 用于确定哈米特酸度 (Ho)。</li>
	<li>执行空白溶液的 UV 测量 (p-硝基苯胺溶液) 和样品溶液 (含有p-硝基苯胺溶液的催化剂), 并确定p-硝基苯胺的安迈信。</li>
	<li>最后, 使用p-硝基苯胺的安迈信值和样例解决方案, 计算 unprotonated [I] 和质子 [.+] 指示器解决方案的摩尔浓度。然后使用2以下的公式计算Ho <img alt="Equation 1" src="/files/ftp_upload/57613/57613eq1.jpg">    等式1 其中 pk (I)蒽醌是水中p-硝基苯胺指示器的 pka (pKa = 0.99), [I] 和 [unprotonated+] 分别为摩尔浓度和质子指示器解决方案。</li>
</ol>3. 黄麻生物量分析
<ol><li>
戊聚糖分析 注: 黄麻生物量为烤箱干燥105摄氏度, 在烤箱16小时。<ol>
<li>在1升圆底烧瓶中加入3克的烘箱干黄麻生物量, 然后在其中加入100毫升的 3.85 N HCl 溶液。</li>
		<li>将烧瓶连接到蒸馏装置, 开始搅拌和加热, 使溶液开始沸腾。</li>
		<li>在含有黄麻生物量和 HCl 溶液的圆底烧瓶中加入250毫升的 3.85 N HCl 滴状。</li>
		<li>在蒸馏过程中, 通过添加 3.85 N HCl 溶液滴状, 维持恒定体积 (100 毫升) 在圆底烧瓶中。</li>
		<li>当收集220毫升馏出物时, 停止实验。然后用蒸馏水将所收集的馏分稀释到500毫升。</li>
		<li>用紫外可见光光谱仪分析样品, 并记录 280 nm 的吸光度。</li>
		<li>使用吸光度和稀释值根据以下公式确定戊聚糖%: <img alt="Equation 2" src="/files/ftp_upload/57613/57613eq2.jpg">    等式2 注: 此方法称为纸浆和造纸工业 (TAPPI) 方法的技术协会, 用于戊聚糖分析9, 19.重复实验两到三次, 取戊聚糖的平均值。如有必要, 稀释所收集的馏出物, 使吸光度达到最佳极限。</li>
	</ol>
</li>
	<li>
木质素分析 注: 去除黄麻生物量中的水分, 然后用它进行木质素分析。将黄麻的生物量保持在105摄氏度的烤箱中, 以去除湿气。<ol>
<li>将1克的黄麻生物量添加到50毫升瓶中, 然后在含有黄麻生物量的小瓶中添加15毫升 72小波% H2,4 。搅拌的混合物使用热板与搅拌设施在30°c 2 小时。</li>
		<li>在1升圆底烧瓶中加入150毫升蒸馏水, 将所消化的生物质样品 (存在于瓶子中) 转移到烧瓶中。</li>
		<li>用195毫升水冲洗瓶子, 将洗涤过的液体转移到含有消化生物量的1升圆底烧瓶中。</li>
		<li>将溶液回流4小时, 然后将圆底烧瓶冷却至室温。等待12小时的不溶木质素和灰分定居下来。</li>
		<li>用 G2 坩埚过滤溶液, 得到不溶木素与灰分。然后用150毫升的热水清洗不溶解的固体, 使其无酸性。</li>
		<li>干燥固体 (木质素 + 灰) 在60°c 为16小时在烤箱和进一步烘干它105°c 为 1 h 在烤箱。</li>
		<li>将样品保存在干燥中, 并在样品冷却时取重量。在这个阶段获得的木质素含有灰分, 因此被称为未被修正的木质素。</li>
		<li>在空气存在的情况下, 将获得的样品加热650摄氏度, 在5小时内进行灰分校正。使用下面的公式确定灰分校正: <img alt="Equation 3" src="/files/ftp_upload/57613/57613eq3.jpg">    等式3
</li>
	</ol>
</li>
</ol>4. 将戊聚糖从黄麻生物量转化为糖
<ol><li>将2克的黄麻生物量添加到高压和高温间歇反应器 (160 毫升帕尔反应器)。加60毫升水和0.24 克酸性 IL, 将温度升高到160摄氏度。</li>
	<li>将搅拌速度设置为 200 rpm, 而反应器加热高达160摄氏度。一旦达到160摄氏度温度, 增加搅拌速度到 600 rpm。</li>
	<li>继续反应为 1 h。然后, 将搅拌速度降低到 200 rpm 并停止加热。</li>
	<li>让反应堆冷却到室温。停止搅拌, 打开反应器, 从反应混合物中分离出固体。采用高效液相色谱法对反应混合物进行分析。</li>
</ol>

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我们没有什么可透露的。

将黄麻生物量转化为 C5 糖单体的戊聚糖表现为使用各种均质 Brønsted 酸性催化剂, 如H2,因此4、HCl 和酸性 IL。并将酸性 il 的催化效果与无酸度的 il (1-丁基 3-咪唑氯化氯) 进行了比较。所有反应都是在160摄氏度的巴里高压釜中进行的。酸性 IL 的使用表明, 与这项工作中使用的均质酸 (矿物酸 H2, 所以4和 HCl) 相比, 戊聚糖转化率最高。结果表明, 酸性 IL 具有较高的 C5 糖?...

生物量作为可再生能源和化学来源具有很大的潜力, 因为它是可持续的、廉价的、同样分布不像化石资源, 这使得它成为替代化石原料的最有希望的候选国之一。纤维素生物量的估计产量为每年1460亿公吨1。纤维素生物量主要由木质素、纤维素和半纤维素组成, 为其三主要成分。木质素是由 phenylpropanoid 单位制成的芳香聚合物;另一方面, 纤维素和半纤维素是纤维素生物量的多糖部分。纤维素由β (1→4) 糖苷链连接的葡萄糖单元组成, 而半纤维素由β (1→4)、β (1→3) 和β (1→6) 糖苷键2、3组成, 由 C5 糖、C6 糖和糖酸共同构成。与各种纤维素生物量 (蔗渣, 稻壳, 麦草,等), 黄麻木质纤维素的生物量也产生了很大数量 (ca. 98% 2014年) 在亚洲与世界黄麻总产量相比。印度生产 1.96 x 106公吨黄麻生物量, 而孟加拉国生产 1.34 x 106公吨的黄麻生物量, 与世界黄麻生物量总产量 (3.39 x 106公吨) 相比, 在 2014年4。这种非食用生物量的利用不会与粮食需求发生冲突。因此, 将其用作合成各种增值化学品 (木糖、阿拉伯糖、糠醛、5-hydroxymethylfurfural (HMF)、等) 的原料是有益的. 根据美国能源部的数据, 糠醛和 HMF 被认为是来自生物量5的前30块建筑化学物质中的一些。糠醛是从木糖或直接从半纤维素得到的, 可以转化为许多重要的化学物质。糠醇、甲基呋喃和四氢呋喃是从糠醛6中获得的重要化学物质。因此, 将纤维素生物量 (如黄麻生物量) 转化为 C5 糖和其他重要化学物质是一个重要的课题。
关于将纤维素生物量转化为增值化学品的各种催化方法, 可提供广泛的报告。矿物酸 (HCl 和 H2因此4) 和异质催化剂 (Amberlyst、HMOR、HUSY、SAPO-44、等) 被大量用于将半纤维素和纤维素生物量转化为糖 (戊和己糖依赖糖)和呋喃 (糠醛和 HMF)7,8。矿物酸的复用性和腐蚀是一个重要问题。然而, 随着固体酸催化剂的出现, 由于反应发生在催化剂表面, 因此需要较高的温度和压力。为了克服这些问题, 最近报告了测算的生物量作为催化剂或溶剂9,10,11,12,13,14。使用 IL 作为溶剂不是一个更好的方法, 因为它的成本较高, 并降低蒸汽压力的 ILs, 造成了困难的产品分离。因此, 必须在水溶剂系统中使用可回收 IL 作为催化剂 (少量), 以便将生物质转化为增值化学品。
在这里, 我们提出了使用 1-甲基 3-(3-磺丙基) 鎓硫酸氢酸性 IL 作为催化剂, 以直接转化为戊聚糖在黄麻生物量成糖单体, 没有任何预处理。通常, 纤维素生物量10、15、16、17的预处理报告了 ils, 而大量的 ils 用于生物量预处理。因此, 使用 IL 作为催化剂并将纤维素生物量转化为化学物质, 而无需任何额外的处理, 总是有利的。此外, 在目前的工作中, 用 Klason 方法计算了黄麻生物量中的木质素浓度, 可转化为各种芳香单体18。

<table><tbody><tr><td>1-Methylimidazole</td><td>Sigma Aldrich</td><td>M50834</td><td></td></tr><tr><td>1,3-Propanesultone</td><td>Sigma Aldrich</td><td>P50706</td><td>Moisture sensitive</td></tr><tr><td>p-nitroaniline</td><td>Sigma Aldrich</td><td>185310</td><td></td></tr><tr><td>Toluene</td><td>J. T. Baker</td><td>9460-03</td><td></td></tr><tr><td>Sulfuric acid</td><td>Honeywell-Fluka</td><td>30743</td><td>Highly corrosive</td></tr><tr><td>Hydrochloric acid</td><td>Honeywell-Fluka</td><td>30719</td><td>Highly corrosive</td></tr><tr><td>1-butyl-3-methylimidazolium chloride</td><td>Sigma Aldrich</td><td>900856</td><td>Highly hygroscopic</td></tr><tr><td>D(+)-Xylose</td><td>Acros Organics</td><td>141001000</td><td></td></tr><tr><td>L(+)-Arabinose</td><td>Acros Organics</td><td>104981000</td><td></td></tr><tr><td>UV-Spectrometer</td><td>JASCO</td><td>V-670</td><td></td></tr><tr><td>Parr reactor</td><td>Parr USA</td><td>Seriese 4560</td><td></td></tr><tr><td>Parr reactor controller</td><td>Parr USA</td><td>Seriese 4848</td><td></td></tr><tr><td>High pressure liquid chromatography (HPLC)</td><td>JASCO</td><td>Seriese LC-2000</td><td></td></tr><tr><td>Digital hot plate stirrer</td><td>Thermo Scientific</td><td>SP142020-33Q Cimarec</td><td></td></tr><tr><td>Oven furnace</td><td>Thermal Scientific</td><td>FB1400 Thermolyne blast oven furnace</td><td></td></tr></tbody></table>

a novel method for the pentosan analysis present in jute biomass and its conversion into sugar monomers using acidic ionic liquid

近年来, 离子液体 (ILs) 被用于生物质测算, 因为它们具有热稳定性、较低的蒸气压、不可燃性、较高的热容量、可调谐的溶解度和酸度等显著特性。通过利用 Brønsted 酸性 1-甲基-3-(3-磺丙基)-鎓硫酸氢的催化量, 我们演示了在一锅工艺中从黄麻生物量的戊聚糖中合成 C5 糖 (木糖和阿拉伯糖) 的方法。酸性 IL 是在实验室合成的, 其特点是使用核磁共振光谱技术来了解其纯度。测定了不同的保水性能, 如酸强度、热、热液稳定性等, 表明催化剂在较高温度下稳定 (250 摄氏度), 具有很高的耐酸强度 (Ho 1.57)。酸性 IL 将超过90% 的戊聚糖转化为糖和糠醛。因此, 本研究提出的方法也可用于其他纤维素生物量戊聚糖浓度的评价。

从生物量中回收的戊聚糖和木质素的确切数量取决于纤维素生物量的类型。从不同的地方收集的纤维素生物量的相似类型可以有不同浓度的戊聚糖和木质素。本研究中使用的黄麻生物量包含20个戊聚糖% 和 14 个小波% 木质素。
图 1显示了矿物酸 (H2、4和 HCl) 和酸性 IL 对黄麻生?...

Watch this Scientific Journal Video about A Novel Method for the Pentosan Analysis Present in Jute Biomass and Its Conversion into Sugar Monomers Using Acidic Ionic Liquid at JoVE.com

A Novel Method for the Pentosan Analysis Present in Jute Biomass and Its Conversion into Sugar Monomers Using Acidic Ionic Liquid

我们提出了一个协议, 以合成 C5 糖 (木糖和阿拉伯糖) 从可再生的不可食用的纤维素生物量 (即, 黄麻) 与存在 Brønsted 酸性离子液体 (捞) 作为催化剂在水中.该催化剂比传统的矿物酸催化剂具有更好的催化性能 (H2, 因此4和 HCl)。

利用酸性离子液体戊聚糖分析黄麻生物量及其转化为糖单体的新方法

Recently, ionic liquids (ILs) are used for biomass valorization into valuable chemicals because of their remarkable properties such as thermal stability, ...

a-novel-method-for-pentosan-analysis-present-jute-biomass-its

Research

JoVE Journal

Environment

7.2K 次观看.  National Taiwan University. 我们提出了一个协议, 以合成 C5 糖 (木糖和阿拉伯糖) 从可再生的不可食用的纤维素生物量 (即, 黄麻) 与存在 Brønsted 酸性离子液体 (捞) 作为催化剂在水中.该催化剂比传统的矿物酸催化剂具有更好的催化性能 (H2, 因此4和 HCl)。

视频: A Novel Method for the Pentosan Analysis Present in Jute Biomass and Its Conversion into Sugar Monomers Using Acidic Ionic Liquid

Methods for Facilitating Microbial Growth on Pulp Mill Waste Streams and Characterization of the Biodegradation Potential of Cultured Microbes

The kraft process is applied to wood chips for separation of lignin from the polysaccharides within lignocellulose for pulp that will produce a high quality paper. Black liquor is a pulping waste generated by the kraft process that has potential for downstream bioconversion. However, the recalcitrant nature of the lignocellulose resources, its chemical derivatives that constitute the majority of available organic carbon within black liquor, and its basic pH present challenges to microbial biodegradation of this waste material. Methods for the collection and modification of black liquor for microbial growth are aimed at utilization of this pulp waste to convert the lignin, organic acids, and polysaccharide degradation byproducts into valuable chemicals. The lignocellulose extraction techniques presented provide a reproducible method for preparation of lignocellulose growth substrates for understanding metabolic capacities of cultured microorganisms. Use of gas chromatography-mass spectrometry enables the identification and quantification of the fermentation products resulting from the growth of microorganisms on pulping waste. These methods when used together can facilitate the determination of the metabolic activity of microorganisms with potential to produce fermentation products that would provide greater value to the pulping system and reduce effluent waste, thereby increasing potential paper milling profits and offering additional uses for black liquor.

Industrial wastes can be collected and modified to analyze microbial growth. Lignocellulose extraction techniques provide components to analyze specific biodegradation ability. Gas chromatography-mass spectrometry identifies fermentation products of microorganisms grown on pulping waste. These methods determine the metabolic capacity of microorganisms to degrade pulping waste.

方法对纸浆厂污水流和培养微生物的生物降解能力的表征促进微生物生长

The kraft process is applied to wood chips for separation of lignin from the polysaccharides within lignocellulose for pulp that will produce a high ...

科研

环境科学

High-throughput Screening of Recalcitrance Variations in Lignocellulosic Biomass: Total Lignin, Lignin Monomers, and Enzymatic Sugar Release

The conversion of lignocellulosic biomass to fuels, chemicals, and other commodities has been explored as one possible pathway toward reductions in the use of non-renewable energy sources. In order to identify which plants, out of a diverse pool, have the desired chemical traits for downstream applications, attributes, such as cellulose and lignin content, or monomeric sugar release following an enzymatic saccharification, must be compared. The experimental and data analysis protocols of the standard methods of analysis can be time-consuming, thereby limiting the number of samples that can be measured. High-throughput (HTP) methods alleviate the shortcomings of the standard methods, and permit the rapid screening of available samples to isolate those possessing the desired traits. This study illustrates the HTP sugar release and pyrolysis-molecular beam mass spectrometry pipelines employed at the National Renewable Energy Lab. These pipelines have enabled the efficient assessment of thousands of plants while decreasing experimental time and costs through reductions in labor and consumables.

Plant cell wall structure and chemistry traits are evaluated to identify ideal feedstocks for biofuels and bio-materials. Standard methods have limitations when applied to large data sets. These high-throughput pretreatment, enzyme saccharification, and pyrolysis-molecular beam mass spectrometry methods compare large numbers of biomass samples with decreased experimental time and cost.

总木质素，木质素单体，和酶促糖推出:顽拗变奏曲在木质纤维素生物质的高通量筛选

The conversion of lignocellulosic biomass to fuels, chemicals, and other commodities has been explored as one possible pathway toward reductions in the ...

Pretreatment of Lignocellulosic Biomass with Low-cost Ionic Liquids

A number of ionic liquids (ILs) with economically attractive production costs have recently received growing interest as media for the delignification of a variety of lignocellulosic feedstocks. Here we demonstrate the use of these low-cost protic ILs in the deconstruction of lignocellulosic biomass (Ionosolv pretreatment), yielding cellulose and a purified lignin. In the most generic process, the protic ionic liquid is synthesized by accurate combination of aqueous acid and amine base. The water content is adjusted subsequently. For the delignification, the biomass is placed into a vessel with IL solution at elevated temperatures to dissolve the lignin and hemicellulose, leaving a cellulose-rich pulp ready for saccharification (hydrolysis to fermentable sugars). The lignin is later precipitated from the IL by the addition of water and recovered as a solid. The removal of the added water regenerates the ionic liquid, which can be reused multiple times. This protocol is useful to investigate the significant potential of protic ILs for use in commercial biomass pretreatment/lignin fractionation for producing biofuels or renewable chemicals and materials.

The pretreatment of lignocellulosic biomass with protic low-cost ionic liquids is shown, resulting in a delignified cellulose-rich pulp and a purified lignin. The pulp gives rise to high glucose yields after enzymatic saccharification.

木质纤维素生物质预处理低成本离子液体

A number of ionic liquids (ILs) with economically attractive production costs have recently received growing interest as media for the delignification of ...

Lignin Down-regulation of Zea mays via dsRNAi and Klason Lignin Analysis

To facilitate the use of lignocellulosic biomass as an alternative bioenergy resource, during biological conversion processes, a pretreatment step is needed to open up the structure of the plant cell wall, increasing the accessibility of the cell wall carbohydrates. Lignin, a polyphenolic material present in many cell wall types, is known to be a significant hindrance to enzyme access. Reduction in lignin content to a level that does not interfere with the structural integrity and defense system of the plant might be a valuable step to reduce the costs of bioethanol production. In this study, we have genetically down-regulated one of the lignin biosynthesis-related genes, cinnamoyl-CoA reductase (ZmCCR1) via a double stranded RNA interference technique. The ZmCCR1_RNAi construct was integrated into the maize genome using the particle bombardment method. Transgenic maize plants grew normally as compared to the wild-type control plants without interfering with biomass growth or defense mechanisms, with the exception of displaying of brown-coloration in transgenic plants leaf mid-ribs, husks, and stems. The microscopic analyses, in conjunction with the histological assay, revealed that the leaf sclerenchyma fibers were thinned but the structure and size of other major vascular system components was not altered. The lignin content in the transgenic maize was reduced by 7-8.7%, the crystalline cellulose content was increased in response to lignin reduction, and hemicelluloses remained unchanged. The analyses may indicate that carbon flow might have been shifted from lignin biosynthesis to cellulose biosynthesis. This article delineates the procedures used to down-regulate the lignin content in maize via RNAi technology, and the cell wall compositional analyses used to verify the effect of the modifications on the cell wall structure.

Lignin Down-regulation of Zea mays via dsRNAi and Klason Lignin Analysis

A double stranded RNA interference (dsRNAi) technique is employed to down-regulate the maize cinnamoyl coenzyme A reductase (ZmCCR1) gene to lower plant lignin content. Lignin down-regulation from the cell wall is visualized by microscopic analyses and quantified by the Klason method. Compositional changes in hemicellulose and crystalline cellulose are analyzed.

木质素下调<em&gt;玉米</em&gt;通过dsRNAi和Klason木质素分析

To facilitate the use of lignocellulosic biomass as an alternative bioenergy resource, during biological conversion processes, a pretreatment step is ...

生物工程

Extraction of Lignin with High &#946;-O-4 Content by Mild Ethanol Extraction and Its Effect on the Depolymerization Yield

Lignin valorization strategies are a key factor for achieving more economically competitive biorefineries based on lignocellulosic biomass. Most of the emerging elegant procedures to obtain specific aromatic products rely on the lignin substrate having a high content of the readily cleavable &#946;-O-4 linkage as present in the native lignin structure. This provides a miss-match with typical technical lignins that are highly degraded and therefore are low in &#946;-O-4 linkages. Therefore, the extraction yields, and the quality of the obtained lignin are of utmost importance to access new lignin valorization pathways. In this manuscript, a simple protocol is presented to obtain lignins with high &#946;-O-4 content by relatively mild ethanol extraction that can be applied to different lignocellulose sources. Furthermore, analysis procedures to determine the quality of the lignins are presented together with a depolymerization protocol that yields specific phenolic 2-arylmethyl-1,3-dioxolanes, which can be used to evaluate the obtained lignins. The presented results demonstrate the link between lignin quality and potential for the lignins to be depolymerized into specific monomeric aromatic chemicals. Overall, the extraction and depolymerization demonstrates a trade-off between the lignin extraction yield and the retention of the native aryl-ether structure and thus the potential of the lignin to be used as the substrate for the production of chemicals for higher-value applications.

Here, we present a protocol to perform ethanol extraction of lignin from several biomass sources. The effect of the extraction conditions on the lignin yield and &#946;-O-4 content are presented. Selective depolymerization is performed on the obtained lignins to obtain high aromatic monomer products.

轻度乙醇萃取高β-o-4 的木质素及其对解聚产率的影响

Lignin valorization strategies are a key factor for achieving more economically competitive biorefineries based on lignocellulosic biomass. Most of the ...

化学

Comprehensive Compositional Analysis of Plant Cell Walls (Lignocellulosic biomass) Part I: Lignin

The need for renewable, carbon neutral, and sustainable raw materials for industry and society has become one of the most pressing issues for the 21st century. This has rekindled interest in the use of plant products as industrial raw materials for the production of liquid fuels for transportation1 and other products such as biocomposite materials7. Plant biomass remains one of the greatest untapped reserves on the planet4. It is mostly comprised of cell walls that are composed of energy rich polymers including cellulose, various hemicelluloses (matrix polysaccharides, and the polyphenol lignin6 and thus sometimes termed lignocellulosics. However, plant cell walls have evolved to be recalcitrant to degradation as walls provide tensile strength to cells and the entire plants, ward off pathogens, and allow water to be transported throughout the plant; in the case of trees up to more the 100 m above ground level. Due to the various functions of walls, there is an immense structural diversity within the walls of different plant species and cell types within a single plant4. Hence, depending of what crop species, crop variety, or plant tissue is used for a biorefinery, the processing steps for depolymerization by chemical/enzymatic processes and subsequent fermentation of the various sugars to liquid biofuels need to be adjusted and optimized. This fact underpins the need for a thorough characterization of plant biomass feedstocks. Here we describe a comprehensive analytical methodology that enables the determination of the composition of lignocellulosics and is amenable to a medium to high-throughput analysis. In this first part we focus on the analysis of the polyphenol lignin (Figure 1). The method starts of with preparing destarched cell wall material. The resulting lignocellulosics are then split up to determine its lignin content by acetylbromide solubilization3, and its lignin composition in terms of its syringyl, guaiacyl- and p-hydroxyphenyl units5. The protocol for analyzing the carbohydrates in lignocellulosic biomass including cellulose content and matrix polysaccharide composition is discussed in Part II2.

Comprehensive Compositional Analysis of Plant Cell Walls Lignocellulosic biomass Part I: Lignin

Plant biomass is a major carbon-neutral renewable resource that could be used for the production of biofuels. Plant biomass consists mainly of cell walls, a structurally complex composite material termed lignocellulosics. Here we describe a protocol for a comprehensive analysis of the content and composition of the polyphenolic lignin.

综合植物细胞壁成分分析（木质纤维素生物质）第一部分：木质素

The need for renewable, carbon neutral, and sustainable raw materials for industry and society has become one of the most pressing issues for the 21st ...

生物学

Comprehensive Compositional Analysis of Plant Cell Walls (Lignocellulosic biomass) Part II: Carbohydrates

The need for renewable, carbon neutral, and sustainable raw materials for industry and society has become one of the most pressing issues for the 21st century. This has rekindled interest in the use of plant products as industrial raw materials for the production of liquid fuels for transportation2 and other products such as biocomposite materials6. Plant biomass remains one of the greatest untapped reserves on the planet4. It is mostly comprised of cell walls that are composed of energy rich polymers including cellulose, various hemicelluloses, and the polyphenol lignin5 and thus sometimes termed lignocellulosics. However, plant cell walls have evolved to be recalcitrant to degradation as walls contribute extensively to the strength and structural integrity of the entire plant. Despite its necessary rigidity, the cell wall is a highly dynamic entity that is metabolically active and plays crucial roles in numerous cell activities such as plant growth and differentiation5. Due to the various functions of walls, there is an immense structural diversity within the walls of different plant species and cell types within a single plant4. Hence, depending of what crop species, crop variety, or plant tissue is used for a biorefinery, the processing steps for depolymerisation by chemical/enzymatic processes and subsequent fermentation of the various sugars to liquid biofuels need to be adjusted and optimized. This fact underpins the need for a thorough characterization of plant biomass feedstocks. Here we describe a comprehensive analytical methodology that enables the determination of the composition of lignocellulosics and is amenable to a medium to high-throughput analysis (Figure 1). The method starts of with preparing destarched cell wall material. The resulting lignocellulosics are then split up to determine its monosaccharide composition of the hemicelluloses and other matrix polysaccharides1, and its content of crystalline cellulose7. The protocol for analyzing the lignin components in lignocellulosic biomass is discussed in Part I3.

Comprehensive Compositional Analysis of Plant Cell Walls Lignocellulosic biomass Part II: Carbohydrates

Plant biomass is a major carbon-neutral renewable resource that could be used for the production of biofuels. Plant biomass consists mainly of cell walls, a structurally complex composite material termed lignocellulosics. Here we describe a protocol for a comprehensive analysis of the content and composition of wall derived carbohydrates.

综合植物细胞壁成分分析（木质纤维素生物质）第二部分：碳水化合物

Fractionation of Lignocellulosic Biomass using the OrganoCat Process

The shift from a petroleum-based to a more sustainable and bio-based economy requires the development of new refinery concepts to maintain the supply of raw materials and energy. For these novel and sustainable biorefinery concepts, it is important to use catalysts and solvents that are aligned with the principles of Green Chemistry. Therefore, the implementation of biogenic alternatives can be a promising solution. The lignocellulose pretreatment and fractionation process presented herein-OrganoCat-is an integrated fractionation of lignocellulose into its main components using biogenic acids such as 2,5-furandicarboxylic acid as catalyst. Hemicelluloses and other non-cellulosic polysaccharides are selectively depolymerized by the diluted acid and dissolved, while the crystalline cellulose remains in the solid pulp. In the presence of a second organic phase consisting of biogenic 2-methyltetrahydrofuran, disentangled lignin is extracted in situ. The process allows for the efficient fractionation of the three main components-lignin, cellulose, and non-cellulosic sugars. This helps to focus on the quality of the lignin, the improvement of enzymatic hydrolysis of the cellulose-enriched pulp, and the mild non-cellulosic sugar extraction with low degradation.

OrganoCat is a method for the pretreatment and fractionation of lignocellulose under mild conditions into lignin, fermentable sugars, and cellulose pulp. In a biogenic, biphasic solvent system of water and 2-methyltetrahydrofuran with 2,5-furancarboxylic acid as catalyst, the OrganoCat products are separated in situ for straightforward product recovery.

使用有机催化工艺分馏木质纤维素生物质

The shift from a petroleum-based to a more sustainable and bio-based economy requires the development of new refinery concepts to maintain the supply of ...

Ultrafast Lignin Extraction from Unusual Mediterranean Lignocellulosic Residues

Pretreatment is still the most expensive step in lignocellulosic biorefinery processes. It must be made cost-effective by minimizing chemical requirements as well as power and heat consumption and by using environment-friendly solvents. Deep eutectic solvents (DESs) are key, green, and low-cost solvents in sustainable biorefineries. They are transparent mixtures characterized by low freezing points resulting from at least one hydrogen bond donor and one hydrogen bond acceptor. Although DESs are promising solvents, it is necessary to combine them with an economic heating technology, such as microwave irradiation, for competitive profitability. Microwave irradiation is a promising strategy to shorten the heating time and boost fractionation because it can rapidly attain the appropriate temperature. The aim of this study was to develop a one-step, rapid method for biomass fractionation and lignin extraction using a low-cost and biodegradable solvent. 
In this study, a microwave-assisted DES pretreatment was conducted for 60 s at 800 W, using three kinds of DESs. The DES mixtures were facilely prepared from choline chloride (ChCl) and three hydrogen-bond donors (HBDs): a monocarboxylic acid (lactic acid), a dicarboxylic acid (oxalic acid), and urea. This pretreatment was used for biomass fractionation and lignin recovery from marine residues (Posidonia leaves and aegagropile), agri-food byproducts (almond shells and olive pomace), forest residues (pinecones), and perennial lignocellulosic grasses (Stipa tenacissima). Further analyses were conducted to determine the yield, purity, and molecular weight distribution of the recovered lignin. In addition, the effect of DESs on the chemical functional groups in the extracted lignin was determined by Fourier-transform infrared (FTIR) spectroscopy. The results indicate that the ChCl-oxalic acid mixture affords the highest lignin purity and the lowest yield. The present study demonstrates that the DES-microwave process is an ultrafast, efficient, and cost-competitive technology for lignocellulosic biomass fractionation.

Deep eutectic solvent-based, microwave-assisted pretreatment is a green, fast, and efficient process for lignocellulosic fractionation and high-purity lignin recovery.

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 ...

Quantitative 31P NMR Analysis of Lignins and Tannins

The development of sustainable biorefinery products is confronted, among others, with the challenge of lignin and tannin valorization. These abundant, renewable aromatic biopolymers have not been widely exploited due to their inherent structural complexity and high degrees of variability and species diversity. The lack of a defined primary structure for these polyphenols is further compounded with complex chemical alterations induced during processing, eventually imparting a large variety of structural features of extreme significance for any further utilization efforts.
Consequently, a protocol for the rapid, simple, and unequivocal identification and quantification of the various functional groups present in natural polyphenols, is a fundamental prerequisite for understanding and accordingly tailor their reactivity and eventual utility.
Quantitative 31P NMR offers the opportunity to rapidly and reliably identify unsubstituted, o-mono substituted, and o-disubstituted phenols, aliphatic OHs, and carboxylic acid moieties in lignins and tannins with broad application potential.
The methodology consists of an in situ quantitative lignin or tannin labeling procedure using a suitable 31P containing probe, followed by the acquisition of a quantitative 31P NMR spectrum in the presence of an internal standard. The high natural abundance of the 31P nucleus allows for small amounts of the sample (~30 mg) and short NMR acquisition times (~30-120 min) with well-resolved 31P signals that are highly dependent on the surrounding chemical environment of the labeled OH groups.

Quantitative 31P NMR Analysis of Lignins and Tannins

31P NMR is a powerful tool for the structural elucidation of polyphenols. This fast, easy, precise, quantitative, and highly reproducible analytical procedure, that allows for the quantification and differentiation of the different types of hydroxy, phenolic, and carboxylic groups in lignins and tannins has now become a routine analytical tool.

利格宁和单宁的定量 31P NMR 分析

The development of sustainable biorefinery products is confronted, among others, with the challenge of lignin and tannin valorization. These abundant, ...

利用酸性离子液体戊聚糖分析黄麻生物量及其转化为糖单体的新方法

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