CN103893216A - Method for extracting and separating antioxidant components from crude wood vinegar liquid - Google Patents
Method for extracting and separating antioxidant components from crude wood vinegar liquid Download PDFInfo
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- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 8
- 235000006708 antioxidants Nutrition 0.000 claims description 8
- 229930003427 Vitamin E Natural products 0.000 claims description 6
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 claims description 6
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Abstract
一种粗制木醋液中抗氧化组分的提取、分离方法，涉及木醋液组分提取、分离方法，该方法以粗制木醋液为原料，选用二氯甲烷作为萃取剂，其提取、分离过程包括：量取100～200ml粗制木醋液，与二氯甲烷按1:1～1：5体积比的比例萃取1～3次，将萃取液干燥，得到浸膏，对抗氧化活性进行跟踪；计算相应流分样品的清除率和IC50值，半抑制浓度，筛选得到抗氧化活性最佳的活性组分。本发明减少了粗木醋液常规的精制过程；二氯甲烷萃取率高，提取工艺简便。大孔树脂流分2分离率高。而且该馏分清除DPPH自由基能力比较强，抗氧化活性高于两个对照品，具有较好的抗氧化活性。A method for extracting and separating antioxidant components in crude wood vinegar relates to a method for extracting and separating components of wood vinegar. The method uses crude wood vinegar as a raw material and selects dichloromethane as an extractant. , The separation process includes: measure 100-200ml of crude wood vinegar, extract with methylene chloride at a volume ratio of 1:1-1:5 for 1-3 times, dry the extract to obtain an extract, which has antioxidant activity Carry out tracking; calculate the clearance rate and IC 50 value of the corresponding fraction samples, and the half-inhibitory concentration, and screen to obtain the active component with the best antioxidant activity. The invention reduces the conventional refining process of crude wood vinegar; the dichloromethane extraction rate is high, and the extraction process is simple and convenient. Macroporous resin fraction 2 had a high separation rate. Moreover, this fraction has a relatively strong ability to scavenge DPPH free radicals, and its antioxidant activity is higher than that of the two reference substances, and has better antioxidant activity.
Description
技术领域 technical field
本发明涉及木醋液组分提取、分离方法，特别是涉及一种粗制木醋液中抗氧化组分的提取、分离方法。 The invention relates to a method for extracting and separating components of wood vinegar, in particular to a method for extracting and separating antioxidant components in crude wood vinegar.
背景技术 Background technique
木材剩余物具有广泛的来源，从森林采伐剩余物、原木造材剩余物到木材加工剩余物，包含各种形式的废弃木质制品和木质纤维制品。据统计，各种废弃物可以占到原木材的50%。生产木炭是深度利用木材剩余物的有效途径，可获得具有较高附加值的木炭，并可收集木醋液，使木材剩余物得到最完全的利用。 Wood residues come from a wide range of sources, ranging from forest harvesting residues, log manufacturing residues, and wood processing residues, including various forms of waste wood products and wood fiber products. According to statistics, various wastes can account for 50% of the original wood. The production of charcoal is an effective way to deeply utilize wood residues. It can obtain charcoal with higher added value, and can collect wood vinegar to make the most complete use of wood residues.
作为一种天然林产品的副产物,木醋液起源于木材的干馏工业，是木材中的纤维素、半纤维素和木质素热分解的产物。从广义上讲，木醋液是指把树木炭化，将其能量转换成气体再自然冷却成浓缩液体。木醋液的组分和性质也随着不同的干馏原料和精制方法的同而异。其主要成分涉及多种类的化合物，大部分木醋液中含有酸、酯、酚、醇、呋喃类以及羟基类等上百种有机成分，是一种组份复杂、功能多样和相对稳定的系统物质。 As a by-product of natural forest products, wood vinegar originated from the dry distillation industry of wood, and is the product of thermal decomposition of cellulose, hemicellulose and lignin in wood. In a broad sense, wood vinegar refers to carbonizing trees, converting their energy into gas and then cooling naturally into concentrated liquid. The components and properties of wood vinegar also vary with different dry distillation raw materials and refining methods. Its main components involve many kinds of compounds. Most of wood vinegar contains hundreds of organic components such as acids, esters, phenols, alcohols, furans and hydroxyls. It is a system with complex components, diverse functions and relatively stable substance.
目前，从天然植物和海洋资源中提取、分离有效成分作为各种用途的产品开发已经成为研究热点。木醋液做作为一种天然植物资源和天然化工原料，含有数量可观的有机物，其功能逐渐被人们所挖掘，可广泛的应用于各行各业。在农业上，木醋液能减农药、减化学肥料用量，杀菌驱虫、保护生态环境。在稻田中施用木醋液，由于木醋液能提高水和土壤微生物的活性，可防治立枯病。在畜牧业，木醋液能消除养猪养鸡场的臭味，作为饲料添加剂能改善肉质。在医药上，木醋液对脚气病、皮肤病、肝脏病和糖尿病有效。在轻工业中，由于木醋液具有防腐、抗氧化等功效，用于化装品、沐浴液和食品饮料等的添加剂。（Doran W.L.，1932； 宫本雄一，1962；Rodolfo，et al.，1975； Ohta，et al. ， 1994；朴哲等，2003；马建义，2013）。 At present, the extraction and separation of active ingredients from natural plants and marine resources as products for various purposes has become a research hotspot. As a natural plant resource and natural chemical raw material, wood vinegar contains a considerable amount of organic matter. Its function has been gradually discovered by people and can be widely used in various industries. In agriculture, wood vinegar can reduce the amount of pesticides and chemical fertilizers, sterilize and repel insects, and protect the ecological environment. Apply wood vinegar in paddy fields, because wood vinegar can increase the activity of water and soil microorganisms, it can prevent damping-off. In animal husbandry, wood vinegar can eliminate the odor in pig and chicken farms, and as a feed additive, it can improve meat quality. In medicine, wood vinegar is effective for beriberi, skin diseases, liver diseases and diabetes. In light industry, wood vinegar is used as an additive in cosmetics, bath liquids, food and beverages due to its anti-corrosion and anti-oxidation effects. (Doran W.L., 1932; Miyamoto Yuichi, 1962; Rodolfo, et al., 1975; Ohta, et al., 1994; Park Chul et al., 2003; Ma Jianyi, 2013).
发明内容 Contents of the invention
本发明的目的在于提供一种粗制木醋液中抗氧化组分的提取、分离方法。该方法以树种的枝桠条、边角料等采伐剩余物为原料，经在木炭窑焖烧产生的烟气使其自然气冷凝结成为液体，陈化后为粗制木醋液（颜色黑褐色），然后将定量的粗制木醋液用二氯甲烷进行萃取，得到浸膏，再筛选出最佳的抗氧化活性组分。减少了粗木醋液常规的精制过程，二氯甲烷萃取率高，提取工艺简便。 The object of the present invention is to provide a method for extracting and separating antioxidant components in crude wood vinegar. This method uses tree species branches, leftovers and other harvesting residues as raw materials, and the flue gas produced by simmering in a charcoal kiln makes it condensed into a liquid by natural gas condensation, and after aging, it becomes crude wood vinegar (color dark brown). Then the quantitative crude wood vinegar was extracted with dichloromethane to obtain the extract, and then the best antioxidant active components were screened out. The conventional refining process of crude wood vinegar is reduced, the dichloromethane extraction rate is high, and the extraction process is simple and convenient.
本发明可通过以下技术方案实现： The present invention can be realized through the following technical solutions:
一种粗制木醋液中抗氧化成分的提取、分离方法，该方法以粗制木醋液为原料，选用二氯甲烷作为萃取剂，其提取、分离过程包括：量取100～200 ml粗制木醋液，与二氯甲烷按1:1～1：5体积比的比例萃取1～3次，将萃取液干燥，得到浸膏，称取1～3 g浸膏，用乙醇95%，体积百分比，进行溶解；采用湿法装柱法进行大孔树脂上样，选取甲醇-水体系10% ～100 %；体积比，作为洗脱液进行洗脱，将洗脱下来的样液点硅胶板、暗箱式紫外分析仪进行检测分析，得到大孔树脂不同流份样品；同时，配置浓度维生素E和维生素C0.2～10.0 μg/ml及浓度粗制木醋液、二氯甲烷萃取液、大孔树脂流分样品，均为0.5～30.0 μg/ml和0.1～0.5 mmol的DPPH（1，1-二苯基-2-三硝基苯肼）溶液；移取50~100 μl的DPPH溶液和50~100 μl浓度的粗制木醋液、二氯甲烷萃取液、大孔树脂流分样品，分别置于96孔板中，避光反应20～40 min，在500~520 nm下测其吸光度值，对上述样品的抗氧化活性进行跟踪；计算相应流分样品的清除率和IC50值，半抑制浓度，筛选得到抗氧化活性最佳的活性组分。
A method for extracting and separating antioxidant components in crude wood vinegar. The method uses crude wood vinegar as a raw material and selects dichloromethane as an extraction agent. The extraction and separation process includes: measuring 100 to 200 ml of crude Prepare wood vinegar, extract 1-3 times with dichloromethane at a volume ratio of 1:1-1:5, dry the extract to obtain extract, weigh 1-3 g of extract, and use 95% ethanol, Volume percentage, for dissolution; wet column packing method for macroporous resin sample loading, select methanol-
所述的一种粗制木醋液中抗氧化成分的提取、分离方法，该方法大孔树脂流2的IC50值低于8.0 μg/ml，低于维生素E和维生素C的IC50值。
In the method for extracting and separating antioxidant components in crude wood vinegar, the IC 50 value of the
本发明的优点与效果是： Advantage and effect of the present invention are:
1．本发明以粗制木醋液为原料，可充分利用木醋液资源。同时，选用二氯甲烷作为萃取剂，萃取液颜色清澈，金黄色，减少了粗木醋液常规的精制过程；二氯甲烷萃取率高，提取工艺简便。 1. The invention uses crude wood vinegar as a raw material, and can make full use of wood vinegar resources. At the same time, dichloromethane is selected as the extraction agent, and the color of the extract is clear and golden yellow, which reduces the conventional refining process of crude wood vinegar; the dichloromethane extraction rate is high, and the extraction process is simple.
2. 本发明提取、分离过程中采用活性跟踪手段，对粗制木醋液、二氯甲烷萃取液和经大孔树脂分离得到的不同流分样品进行实时监测，活性筛选和分离工艺简便，大孔树脂流分2分离率高。而且该馏分清除DPPH自由基能力比较强，抗氧化活性高于两个对照品，具有较好的抗氧化活性。
2. In the extraction and separation process of the present invention, the activity tracking method is used to monitor the crude wood vinegar, the dichloromethane extract and the different fraction samples separated by the macroporous resin in real time. The activity screening and separation process is simple and large.
附图说明 Description of drawings
图1 为粗木醋液、二氯甲烷萃取液、大孔树脂流分2以及两种抗氧化活性对照品（VE,VC）的活性测试图 。
Figure 1 is the activity test chart of crude wood vinegar, dichloromethane extract,
具体实施方式 Detailed ways
实施例1： Example 1:
本发明一种粗制木醋液中抗氧化组分的提取、分离方法。主要通过以下步骤实现： 量取约100～200 ml粗制木醋液，与二氯甲烷按1:1～1：5（体积比）的比例萃取1～3次，将萃取液干燥，得到浸膏，称取约1～3 g浸膏，用乙醇（95%，体积百分比）进行溶解；分别采用湿法装柱法进行大孔树脂上样，选取甲醇-水体系（10% ～100 %；体积比）作为洗脱液进行洗脱，将洗脱下来的样液点硅胶板、暗箱式紫外分析仪进行检测分析，得到大孔树脂不同流份分样品。同时，采用活性追踪手段，即配置不同浓度的维生素E和维生素C（0.2～10.0 μg/ml）及不同浓度粗制木醋液、二氯甲烷萃取液、大孔树脂流分样品（均为0.5～30.0 μg/ml）和0.1～0.5 mmol的DPPH（1，1-二苯基-2-三硝基苯肼）溶液。移取50~100 μl的DPPH溶液和50~100 μl不同浓度的粗制木醋液、二氯甲烷萃取液、大孔树脂流分样品，分别置于96孔板中，避光反应20～40 min，在500~520 nm下测其吸光度值，对上述样品的抗氧化活性进行跟踪。计算相应流分样品的清除率和IC50值，筛选得到抗氧化活性最佳的活性组分。 The invention discloses a method for extracting and separating antioxidant components in crude wood vinegar. It is mainly achieved through the following steps: Measure about 100-200 ml of crude wood vinegar, extract it with dichloromethane at a ratio of 1:1-1:5 (volume ratio) for 1-3 times, dry the extract, and obtain Extraction, weigh about 1-3 g of extract, and dissolve it with ethanol (95%, volume percentage); use wet column packing method to load macroporous resin, select methanol-water system (10%-100%; Volume ratio) is used as the eluent for elution, and the eluted sample liquid is spotted on a silica gel plate and a dark box ultraviolet analyzer for detection and analysis, and samples of different fractions of the macroporous resin are obtained. At the same time, the activity tracking method was adopted, that is, different concentrations of vitamin E and vitamin C (0.2-10.0 μg/ml) and different concentrations of crude wood vinegar, dichloromethane extract, and macroporous resin fraction samples (both 0.5 μg/ml) were prepared. ～30.0 μg/ml) and 0.1～0.5 mmol of DPPH (1,1-diphenyl-2-trinitrophenylhydrazine) solution. Pipette 50-100 μl of DPPH solution and 50-100 μl of different concentrations of crude wood vinegar, dichloromethane extract, and macroporous resin fraction samples, place them in a 96-well plate, and react in the dark for 20-40 min, the absorbance value was measured at 500-520 nm, and the antioxidant activity of the above samples was tracked. The clearance rate and IC 50 value of the corresponding fraction samples were calculated, and the active components with the best antioxidant activity were screened.
本发明以粗制木醋液为原料，选用二氯甲烷作为萃取剂，萃取液颜色清澈，金黄色，减少了粗木醋液常规的精制过程；每1000 mL粗木醋液蒸干可得到约20~30g粗木醋液干膏，经萃取干燥可得到10 ~15g二氯甲烷萃取物。二氯甲烷萃取率大于50 %，提取工艺简便。本方法的提取、分离过程中采用活性跟踪手段，对粗制木醋液、二氯甲烷萃取液和经大孔树脂分离得到的不同流分样品进行实时监测，活性筛选和分离工艺简便。每1000 mL粗木醋液经蒸干，萃取干燥，过大孔树脂柱得到流分2约为0.5~1.0 g，大孔树脂流分2分离率大于20 %。而且该流分清除DPPH自由基能力比较强，由附图1的清除率，经计算大孔树脂流2的IC50值低于8.0 μg/ml，低于维生素E和维生素C的IC50值，说明其具有较好的抗氧化活性。
The present invention uses crude wood vinegar as a raw material, selects methylene chloride as an extractant, and the color of the extract is clear and golden yellow, which reduces the conventional refining process of crude wood vinegar; every 1000 mL of crude wood vinegar can be evaporated to dryness to obtain about 20~30g of crude wood vinegar dry paste can be extracted and dried to obtain 10~15g of dichloromethane extract. The dichloromethane extraction rate is greater than 50%, and the extraction process is simple. In the extraction and separation process of the method, an activity tracking means is adopted to monitor the crude wood vinegar, dichloromethane extract and different fraction samples separated by macroporous resin in real time, and the activity screening and separation process is simple and convenient. Each 1000 mL of crude wood vinegar was evaporated to dryness, extracted and dried, and about 0.5-1.0 g of
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