塔拉单宁水解废液回收奎尼酸的工艺试验

从塔拉单宁水解制备没食子酸的废液着手,用真空蒸发法分离去除盐酸,用不同的溶剂萃取法分离去除没食子酸,用活性炭吸附法和强碱阴离子交换法分离去除色素和糖类物质。从而提出了从塔拉单宁水解废液中回收目标产品奎尼酸的方法,产品得率约为理论值的78％。     

五倍子制备没食子酸的研究进展

没食子单宁是没食子酸与多元醇制成的酯,易在酸、碱、酶的催化作用下水解,由此可制备多种与没食子酸相关的衍生物.以五倍子为原料提取没食子酸的方法有化学法和生物法两种,与化学水解法相比,生物法最显著的特点是水解完全,水解副产物葡萄糖可作为能源与碳源被生物催化剂代谢,不仅提高了资源的有效利用率,而且发酵废液易于处理,有利于环境保护.     

紫外法和皮粉法测定塔拉单宁含量的对比研究

分别采用紫外法和皮粉法对5种不同含量的塔拉单宁进行对比研究,并利用SPSS软件对单宁含量测定结果进行显著性检验,结果表明：高纯度塔拉单宁(93%)分别用紫外法和皮粉法测定单宁含量时实验结果并未显著差异(P>0.05),而4种纯度为60%左右塔拉单宁的实验结果均具有显著性差异(P<0.05),皮粉法测得的单宁含量均比用紫外法测得的结果高,差值约为1.5%～2.0%,并由此计算出紫外法测定塔拉单宁含量计算公式中的矫正常数p为1.03。紫外-可见吸收光谱与HPLC分析结果表明：塔拉单宁与五倍子单宁的最大吸收峰均为276 nm,同质量浓度下塔拉单宁的吸收峰强度高于五倍子单宁,塔拉单宁成分出峰时间主要在20～40 min,五倍子单宁主要在30～45 min。     

从没食子酸结晶母液中回收没食子酸的萃取工艺

引言没食子酸又名五倍子酸,是一种应用很广泛的化工原料[1],可用作食品抗氧化剂、着色剂、净化剂、防腐剂等[2],且具有抗肿瘤、抗炎、抗突变等多种生物学作用[3]。没食子酸是单宁酸的水解产物,国内厂家大多数以含水解单宁的植物五倍子、塔拉为原料生产没     

没食子酸生产技术(中)

二、五倍子单宁的水解水解是没食子酸生产的主要工序,也是决定产品收率、成本高低的关键。 1.水解的原理及其影响因素五倍子单宁由没食子酰基与β-D-葡萄糖以酯键连接而成。在酸或酶的作用下,酯键很容易断裂分解成没食子酸和葡萄糖。     

单宁酸水解制取没食子酸的研究

研究了单宁酸用硫酸水解成没食子酸的条件和有关因素的影响 ,得出的最佳工艺条件是 :n(15°B单宁液 ) :n(硫酸 ) =12∶1,反应温度 110℃ ,反应时间 4h ;单宁转化率达到 10 0 % ,没食子酸水解粗晶色泽浅淡     

高转化率生物法制没食子酸研究

本文介绍由倍花上分离的１株黑曲霉（Ａｓｐｅｒｇｉｌｌｕｓｎｉｇｅｒ－３１）酶解五倍子单宁生物转化制没食子酸试验结果。倍花料通常的实际产品没食子酸的单宁转化率的６３．５％，角倍料约７４．５％；如适当改变条件，产品的单宁转化率可分别增至７８．５％与８９．５％左右，迄今中外有关文献现尚未见超过本研究单宁转化率的报告。     

塔拉粉直接合成3,4,5—三甲氧基苯甲醛

直接以塔拉粉为起始原料,通过甲基化、水解、酯化、肼化、氧化制得3,4,5-三甲氧基苯甲醛,经波谱测定确证其结构与用五倍子合成的3,4,5-三甲氧基苯甲醛一致。产品成本比用五倍子单宁为原料每吨降低1.5万元。     

五倍子单宁的发酵水解

天然植物单宁是指分子量为500～3000,在制革过程中能与动物生皮胶原结合的多酚化合物。植物单宁分水解和凝缩两大类。桔单宁不仅在制革方面具有商用价值,还可以作为生产没食子酸的原料。化学工业和制药工业以没食子酸作合成中间体。人们最为熟知的桔单宁是土耳其倍子单宁,这是山毛榉科染色栎(Quercus infectoria)上获得的一种病理赘瘤,可作药用单     

从野桐提炼新的水解单宁野桐精酸和野桐亭酸

在日本,富含单宁的野桐(Mallotus japonicus)(大戟科植物)的皮和叶,被用来治疗胃溃疡病。本报告作者已从中分离出一种新的称之为野桐精酸(mallotusinic acid)(1)的水解类单宁,以及野桐宁(geraniin)(2)作为叶子的主要成份,另外也发现了一种新的水解类单宁,称之为野桐亭酸(mallotinic acid)(3)。其方法是:将叶子在丙酮和水的混合物中搅匀,再用醋酸乙酯提取浓溶液。用上行滴入逆流色层法,并用正丁醇-醋酸-水(4:1:5)展开剂来分离醋酸乙酯提出物。夹杂有野桐宁的野桐精酸是继芸香甙和野桐宁之后的组份中分离得到的。用醋酸乙酯提取,调     

响应曲面法优化木薯酒精污泥基活性炭制备及对没食子酸的吸附性能

以木薯酒精厂生产过程中产生的脱水污泥为原料,采用响应曲面法Box-Behnken模型优化了木薯酒精污泥基活性炭的制备工艺,同时对最优成品进行一系列表征分析,并将其应用于没食子酸废水的处理研究.活性炭的最优制备条件为活化温度489℃,浸渍时间14h,活化时间51 min,氯化锌浓度21.53％,该条件下样品的碘吸附值达5...     

Novel hyperbranched glycomimetics recognized by the human mannose receptor: quinic or shikimic acid derivatives as mannose bioisosteres

The mannose receptor mediates the internalization of a wide range of molecules or microorganisms in a pattern recognition manner. Therefore, it represents an attractive entry for specific drug, gene, or antigen delivery to macrophages and dendritic cells. In an attempt to design novel effective synthetic mannose receptor ligands, quinic and shikimic acid were selected as putative mannose mimics on the basis of X-ray crystallographic data from the related rat mannose-binding lectin. As the mannose receptor preferentially binds to molecules displaying several sugar residues, fluorescein-labeled cluster quinic and shikimic acid derivatives with valencies of two to eight were synthesized. Their mannose receptor mediated uptake was assayed on monocyte-derived human dendritic cells by cytofluorimetric analysis. Mannose-receptor specificity was further assessed by competitive inhibition assays with mannan, by confocal microscopy analysis, and by expression of the mannose receptor in transfected Cos-1 cells. Constructs derived from both quinic and shikimic acid were efficiently recognized by the mannose receptor with an optimum affinity for the molecules with a valency of four. As a result, commercially available quinic and shikimic acids appear as stable mannose bioisosteres, which should prove valuable tools for specific cell delivery.     

烟用香精香料中奎尼酸的测定

建立以高效液相色谱测定烟用香精香料中奎尼酸含量的方法。以质量分数50%的乙醇为萃取剂,样品经振荡提取后,采用C18色谱柱分离和二极管阵列检测器测定。结果表明,奎尼酸在1.0～250.0 mg/L范围内线性关系良好,相关系数为0.999,检出限为3.12μg/g,加标回收率为92.6%～105.1%,相对标准偏差（RSD）〈5%（n=5）。所建立的方法具有灵敏度高、准确性好、操作简便等优点,适合于烟用香精香料中奎尼酸的批量测定。     

The Effect of Temperature on Forward/Back Extraction Using an Amine Extractant for the Recovery of Cyclic Hydroxy Carboxylic Acids

ABSTRACT

Forward extraction of shikimic and quinic acids with tridodecylamine (TDA)/1-heptanol is favored at low temperature. In back extraction, higher temperatures and the addition of oleic acid as a competitive displacer provided 80% recovery for shikimic acid and 70% recovery for quinic acid. Higher recoveries are possible since these valuesare limited by the forward extraction step. The effect of temperature swing on carboxylic acid extraction by amines is primarily due to the change in amine basicity with temperature. The addition of a displacer lowers the energy cost by lowering the temperature required in back extraction.     

EXTRACTION OF SHIKIMIC AND QUINIC ACIDS

Solvent extraction using an extractant/diluent system was evaluated for the recovery of shikimic and quinic acids. Tridodecylamine (TDA) was used as the extractant, and 1-heptanol as the diluent. TDA complexes with the acid resulting in an acid-amine complex, which is solvated by the alcohol diluent. In back extraction, oleic acid was added to the organic phase as a displacer. Oleic acid competitively displaces the carboxylic acid in the acid-amine complex, thus forming a displacer-amine complex. The distribution coefficient for back extraction by competitive displacement increased by at least an order of magnitude depending on the mole to mole ratio of oleic acid to TDA

Based on results from batch extraction experiments, a mass-action analysis was introduced for modeling forward and back extraction. The mass-action analysis served as a tool for understanding the mechanism of the extraction process.     

没食子酸正辛酯合成工艺研究

研究了以没食子酸和正辛醇为原料合成没食子酸正辛酯的新工艺 ,讨论了正辛醇的用量、夹水剂的种类和过量正辛醇的循环使用次数对酯化反应的影响。正辛醇循环使用 4～ 8次时 ,没食子酸正辛酯的总得率为 79.53% 95.32 %。     

没食子酸标准样品的制备与定值研究

研究了没食子酸标准样品的制备、均匀性和稳定性检验及其定值方法。用五倍子单宁酸水解得到的没食子酸为原料,经精制得到高纯度的没食子酸标准样品。通过红外光谱、核磁共振、热重分析证实该标准样品的化学结构式。标准样品含量测定采用高效液相色谱面积归一化法,并通过了均匀性检验和稳定性检验(15个月)。经6个实验室的联合定值,没食子酸标准样品的含量值为99.96%±0.10%。     

QUANTIFICATION OF GALLIC ACID AND ELLAGIC ACID FROM THE SEED OF CORNUS OFFICINALIS BY UHPLC METHOD AND THEIR ANTIOXIDANT ACTIVITY

Gallic acid and ellagic acid have been identified in the seed of Cornus officinalis by the use of an ultrahigh performance liquid chromatography (UHPLC) method coupled with a diode array detector (DAD). The water extract of C. officinalis seed contained the highest gallic acid content (3.03 ± 0.10 mg/g seed), which was followed by aqueous methanol extract (2.43 ± 0.10 mg/g seed) and aqueous ethanol extract (1.53 ± 0.25 mg/g seed). But a higher concentration (12.32 ± 0.45 mg/g seed) of ellagic acid was obtained from extraction with aqueous methanol than with aqueous ethanol (11.03 ± 0.42 mg/g seed) and water (7.28 ± 0.16 mg/g seed). After heat treatment and acid hydrolysis, C. officinalis seed had higher concentrations of gallic acid and ellagic acid, contributing to more potent antioxidant activity. The results demonstrated a rich source of gallic acid and ellagic acid in C. officinalis seed, which might provide a novel source of these natural antioxidants.     

白兰地中没食子酸的测定

在橡木桶中陈酿的白兰地随着贮存的时间增长,没食子酸的含量会有明显的增加。文章运用高效液相色谱仪建立一种测定白兰地中没食子酸含量的方法,该方法简单快速、准确性和稳定性高、环保、检测成本低。通过研究不同档次白兰地中没食子酸的含量,有助于提高鉴别白兰地的品质。     

A comparison between catalytic ozonation and activated carbon adsorption/ozone-regeneration processes for wastewater treatment

Two methods based on the use of granular activated carbon (GAC) and ozone to remove organic compounds from water have been investigated. Both methods have been applied to degrade an aqueous solution of gallic acid and a secondary effluent from a wastewater treatment plant (WWTP). One of the methods, namely catalytic ozonation, implies simultaneous ozonation and adsorption onto GAC. This process takes advantage of the oxidizing power of ozone and the adsorption capacity of GAC but also of the catalytic transformation of ozone into secondary oxidants on the GAC surface. The efficiency of catalytic ozonation was compared to those of single adsorption and single ozonation. It was found that the catalytic process highly improves the conversion of total organic carbon (TOC) and makes a more efficient use of ozone than the single ozonation process. To illustrate the reusability of the catalyst, the GAC was reused four times through a series of consecutive experiments. No loss of catalytic activity was observed when treating the WWTP effluent but some deactivation could be appreciated when treating the aqueous solution of gallic acid. This deactivation could be attributed to some porosity destruction and surface oxidation produced as a result of reactions of aqueous ozone on the GAC surface. The other method investigated is an adsorption-regeneration process (namely GAC/O₃-regeneration) that comprises two steps: dynamic adsorption onto GAC and further regeneration of the spent GAC with gaseous ozone. The adsorption stage of the GAC/O₃-regeneration experiments was carried out in a continuous flow adsorption column and breakthrough curves were obtained. It was observed that the GAC used in this work adsorbed gallic acid very efficiently but exhibited limited capacity to remove chemical oxygen demand (COD) from the WWTP effluent. The optimum ozone dose to regenerate the spent GAC after gallic acid adsorption was found to be about 0.4 g O₃/g GAC, with results showing around 90% regeneration efficiency. As a result of incomplete regeneration, the GAC adsorption capacity progressively decreased with the number of adsorption–regeneration cycles. The GAC/O₃-regeneration method was not successful at treating the WWTP effluent as low adsorption uptake was observed. Moreover, the GAC became damaged after regeneration because of excessive oxidation of its surface.