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CN104974198A - Process of extracting tannin from pine bark - Google Patents

Process of extracting tannin from pine bark Download PDF

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Publication number
CN104974198A
CN104974198A CN201510329287.7A CN201510329287A CN104974198A CN 104974198 A CN104974198 A CN 104974198A CN 201510329287 A CN201510329287 A CN 201510329287A CN 104974198 A CN104974198 A CN 104974198A
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pine bark
tannin
extract
microwave
cortex pini
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王超群
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Guangxi University
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Guangxi University
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Abstract

本发明公开了一种从松树皮提取单宁的工艺,该方法包括以下步骤:一种从松树皮提取单宁的工艺,该工艺包括以下步骤:(1)预处理:将松树皮自然晾晒风干后粉碎过100目筛,得到松树皮粉末,备用;(2)微波提取:称取备用的松树皮粉末,置于带回流冷凝管的圆底烧瓶中,然后加入提取液,再将圆底烧瓶放入微波反应器中,在微波功率为80-85W,温度为45℃条件下进行微波提取1min,得到混合提取液;(3)纯化:将得到混合提取液冷却至常温后进行抽滤,将滤液40℃下真空浓缩后,在60℃下真空干燥至质量恒定,即可得白桦树单宁提取物。本发明的方法具有操作简便,提取效率高等优点,为松树皮的利用提供一种新的途径,提高松树皮的附加价值。The invention discloses a process for extracting tannin from pine bark, the method comprising the following steps: a process for extracting tannin from pine bark, the process comprising the following steps: (1) pretreatment: air-drying the pine bark naturally After crushing through a 100-mesh sieve, the pine bark powder is obtained, which is for subsequent use; (2) microwave extraction: take the standby pine bark powder, place it in a round-bottomed flask with a reflux condenser, then add the extract, and place the round-bottomed flask Put it into a microwave reactor, and carry out microwave extraction for 1 min at a microwave power of 80-85W and a temperature of 45°C to obtain a mixed extract; (3) Purification: After cooling the obtained mixed extract to room temperature, perform suction filtration, and After the filtrate is vacuum-concentrated at 40°C, it is vacuum-dried at 60°C until the quality is constant to obtain the birch tannin extract. The method of the invention has the advantages of simple and convenient operation, high extraction efficiency, etc., provides a new approach for the utilization of pine bark, and increases the added value of pine bark.

Description

从松树皮提取单宁的工艺Process of extracting tannin from pine bark

技术领域technical field

本发明涉及植物提取技术领域,尤其是涉及一种从松树皮提取单宁的工艺。The invention relates to the technical field of plant extraction, in particular to a process for extracting tannin from pine bark.

背景技术Background technique

松树皮中含有多种物质,从松树皮中提取物质屡见不鲜,目前国内对松树皮提取物的研究着重于松树皮提取物中的抗氧化能力的物质花青素(原花青素低聚体)(OPCs),该物质抗氧化能力为维他命C的20倍,维他命E的50倍。OPCs作为著名抗氧化剂可有效压制自由基作用,而自由基在变性性疾病,心血管疾病,视力模糊,晒伤和早衰等方面发挥着重要的作用。Pine bark contains a variety of substances, and it is not uncommon to extract substances from pine bark. At present, the research on pine bark extract in China focuses on the anti-oxidant substances in pine bark extract, anthocyanins (proanthocyanidin oligomers) (OPCs) , the antioxidant capacity of this substance is 20 times that of vitamin C and 50 times that of vitamin E. As well-known antioxidants, OPCs can effectively suppress the action of free radicals, which play an important role in degenerative diseases, cardiovascular diseases, blurred vision, sunburn and premature aging.

但松树皮中还含有多种物质可以提取,在松树皮中就含有较多的单宁,单宁(Tannins)又称单宁酸、鞣质、鞣酸。它广泛存在于植物的叶、果实、根及皮等部位,也是树木受昆虫侵袭而生成的虫瘿的主要成分;主要应用于医药、食品、制革、日用化学品、水处理等领域。单宁是多酚中高度聚合的化合物,为黄色或棕黄色无定形松散粉末,在空气中颜色逐渐变深,有较强的吸湿性;不溶于乙醚、苯、氯仿,易溶于水、乙醇、丙酮,水溶液有涩味。单宁的化学成分比较复杂,大致分为两种:一种是水解类单宁,是多元酚酸与糖主要以酯键形成的化合物,如没食子酸单宁和鞣花酸单宁;一种是缩合类单宁,重要组成成分为黄烷醇及其衍生物,如坚木单宁、荆树皮单宁和落叶松单宁。特定分子结构的单宁具有生理活性,能与生物体内的蛋白质、多糖、核酸等发生作用。单宁对人体的作用具有双重性,食物中的单宁过量会产生抗营养的作用,如降低蛋白质的营养价值、影响VA和Vb12的有效利用。单宁在传统医药上内服可治胃肠道出血和止痢,外用于局部止血和创面保护防止感染发炎;近年研究发现单宁还具有抑菌抗病毒、抗过敏、抗氧化和延缓衰老、预防心血管疾病、抗肿瘤和促进免疫等作用。单宁在食品行业中可作为功能性成分用于制作保健品,生产食品添加剂、风味剂等;在化妆品中主要起收敛、防晒、美白、抗皱、保湿、防腐等作用;在制革工业中,单宁是栲胶的主要成分。因此,利用松树皮提取单宁物质可以增加松树皮的附加价值,具有重要的经济效益和社会效益。However, pine bark also contains a variety of substances that can be extracted. Pine bark contains more tannins. Tannins are also known as tannic acid, tannins, and tannins. It widely exists in the leaves, fruits, roots and bark of plants, and is also the main component of galls produced by trees attacked by insects; it is mainly used in medicine, food, tanning, daily chemicals, water treatment and other fields. Tannin is a highly polymerized compound among polyphenols. It is a yellow or brownish yellow amorphous loose powder. The color gradually becomes darker in the air and has strong hygroscopicity. It is insoluble in ether, benzene, and chloroform, and easily soluble in water and ethanol. , Acetone, the aqueous solution has astringent taste. The chemical composition of tannin is relatively complicated, and it can be roughly divided into two types: one is hydrolyzed tannin, which is a compound formed by polyphenolic acid and sugar mainly through ester bonds, such as gallic acid tannin and ellagic acid tannin; It is a condensed tannin, and its important components are flavanols and their derivatives, such as quebracho tannin, wattle bark tannin and larch tannin. Tannins with a specific molecular structure have physiological activity and can interact with proteins, polysaccharides, nucleic acids, etc. in organisms. The effect of tannin on the human body is dual. Excessive tannin in food will produce anti-nutritional effects, such as reducing the nutritional value of protein and affecting the effective utilization of VA and Vb12. In traditional medicine, tannin can be used internally to treat gastrointestinal bleeding and dysentery, and externally used for local hemostasis and wound protection to prevent infection and inflammation; recent studies have found that tannin also has antibacterial, anti-viral, anti-allergic, anti-oxidative, anti-aging, and preventive effects. Cardiovascular disease, anti-tumor and immune-stimulating effects. Tannin can be used as a functional ingredient in the food industry to make health care products, food additives, flavors, etc.; in cosmetics, it mainly plays the role of astringent, sunscreen, whitening, anti-wrinkle, moisturizing, and antiseptic; in the leather industry, Tannin is the main component of extract. Therefore, using pine bark to extract tannins can increase the added value of pine bark, which has important economic and social benefits.

发明内容Contents of the invention

为了实现本发明的目的,本发明提供一种从松树皮提取单宁的工艺,本发明的方法具有操作简便,提取效率高等优点,为松树皮的利用提供一种新的途径,提高松树皮的附加价值。In order to realize the purpose of the present invention, the present invention provides a kind of technique that extracts tannin from pine bark, and the method of the present invention has advantages such as easy and simple operation, high extraction efficiency, provides a kind of new approach for the utilization of pine bark, improves the tannin of pine bark additional value.

为了实现上述目的,本发明采用的技术方案如下:In order to achieve the above object, the technical scheme adopted in the present invention is as follows:

一种从松树皮提取单宁的工艺,该工艺包括以下步骤:A process for extracting tannin from pine bark, the process comprises the following steps:

(1)预处理:将松树皮自然晾晒风干后粉碎过100目筛,得到松树皮粉末,备用;(1) pretreatment: the pine bark is naturally air-dried and then pulverized through a 100-mesh sieve to obtain pine bark powder for subsequent use;

(2)微波提取:称取备用的松树皮粉末,置于带回流冷凝管的圆底烧瓶中,然后加入提取液,再将圆底烧瓶放入微波反应器中,在微波功率为80-85W,温度为45℃条件下进行微波提取1min,得到混合提取液;(2) Microwave extraction: take the standby pine bark powder, place it in a round-bottomed flask with a reflux condenser, then add the extract, then put the round-bottomed flask into a microwave reactor, and the microwave power is 80-85W , and the temperature was 45°C for microwave extraction for 1 min to obtain a mixed extract;

(3)纯化:将得到混合提取液冷却至常温后进行抽滤,将滤液40℃下真空浓缩后,在60℃下真空干燥至质量恒定,即可得白桦树单宁提取物。(3) Purification: the obtained mixed extract was cooled to normal temperature, then suction filtered, the filtrate was concentrated in vacuum at 40°C, and then vacuum-dried at 60°C until the quality was constant to obtain the birch tannin extract.

在本发明中,作为进一步说明,所述步骤(2)中所述提取液与松树粉末按照质量比为1:20-30。In the present invention, as a further illustration, the mass ratio of the extraction liquid and the pine tree powder in the step (2) is 1:20-30.

在本发明中,作为进一步说明,所述提取液是按照乙醇:丙酮:水质量比为10-15:8-10:0.3-0.5的混合液。In the present invention, as a further illustration, the extract is a mixed solution with a mass ratio of ethanol: acetone: water of 10-15:8-10:0.3-0.5.

在本发明中,作为进一步说明,所述圆底烧瓶的规格为250mL。In the present invention, as a further illustration, the specification of the round bottom flask is 250mL.

本发明的有益效果是:The beneficial effects of the present invention are:

1.本发明以乙醇、丙酮、水混合液位提取溶剂进行微波提取松树皮中的单宁物质,通过调配最佳的料液比、提取温度、微波功率、提取时间等因素,缩短浸提时间,增加有效成分的提取率,并且与传统热提取相比,微波辅助提取具有时间短、提取效率高。1. The present invention carries out microwave extraction of tannin substance in pine bark with ethanol, acetone, water mixed liquid level extraction solvent, shortens extraction time by allocating optimal material-liquid ratio, extraction temperature, microwave power, extraction time and other factors , increase the extraction rate of active ingredients, and compared with traditional thermal extraction, microwave-assisted extraction has a shorter time and higher extraction efficiency.

2.本发明具有工艺简单,易于操作、提取率高等优点。2. The present invention has the advantages of simple process, easy operation and high extraction rate.

3.单宁单宁有止血、抑制微生物、抗过敏、抗突变、抗癌、抗肿瘤、抗衰老等作用,本发明提供的方法提取单宁能够充分发挥挖掘松树皮采伐和加工剩余物潜在的经济价值,为农民增收提供了一种新的途径。3. Tannin Tannin has effects such as hemostasis, inhibition of microorganisms, anti-allergic, anti-mutation, anti-cancer, anti-tumor, anti-aging, and the method provided by the present invention extracts tannin and can fully exert the potential potential of excavating pine bark harvesting and processing residues. Economic value provides a new way for farmers to increase their income.

具体实施方式Detailed ways

下面通过具体实施例进一步说明本发明,以使本发明的优点和特征更易于被理解,应该理解的是,本发明的实施例仅仅是用于本发明,而不是对本发明的限制。The present invention will be further described below through specific examples, so that the advantages and features of the present invention can be more easily understood. It should be understood that the examples of the present invention are only used for the present invention, rather than limiting the present invention.

实施例1Example 1

一种从松树皮提取单宁的工艺,该工艺包括以下步骤:A process for extracting tannin from pine bark, the process comprises the following steps:

(1)预处理:将松树皮自然晾晒风干后粉碎过100目筛,得到松树皮粉末,备用;(1) pretreatment: the pine bark is naturally air-dried and then pulverized through a 100-mesh sieve to obtain pine bark powder for subsequent use;

(2)微波提取:称取备用的松树皮粉末,置于带回流冷凝管的250mL圆底烧瓶中,然后加入按照乙醇:丙酮:水质量比为10:8:0.3的混合液为提取液,其中,提取液与松树粉末按照质量比为1:20,再将圆底烧瓶放入微波反应器中,在微波功率为80W,温度为45℃条件下进行微波提取1min,得到混合提取液;(2) Microwave extraction: take the standby pine bark powder, place it in a 250mL round-bottomed flask with a reflux condenser, then add the mixed solution according to ethanol: acetone: water mass ratio of 10:8:0.3 as the extract, Among them, the mass ratio of the extract to the pine tree powder is 1:20, and then the round bottom flask is put into a microwave reactor, and the microwave power is 80W, and the temperature is 45°C, and the microwave extraction is carried out for 1min to obtain the mixed extract;

(3)纯化:将得到混合提取液冷却至常温后进行抽滤,将滤液40℃下真空浓缩后,在60℃下真空干燥至质量恒定,即可得白桦树单宁提取物。(3) Purification: the obtained mixed extract was cooled to normal temperature, then suction filtered, the filtrate was concentrated in vacuum at 40°C, and then vacuum-dried at 60°C until the quality was constant to obtain the birch tannin extract.

经过计算,本实施例最后所得单宁总量为110.05mg/100g。After calculation, the final total amount of tannins obtained in this embodiment is 110.05mg/100g.

实施例2Example 2

一种从松树皮提取单宁的工艺,该工艺包括以下步骤:A process for extracting tannin from pine bark, the process comprises the following steps:

(1)预处理:将松树皮自然晾晒风干后粉碎过100目筛,得到松树皮粉末,备用;(1) pretreatment: the pine bark is naturally air-dried and then pulverized through a 100-mesh sieve to obtain pine bark powder for subsequent use;

(2)微波提取:称取备用的松树皮粉末,置于带回流冷凝管的250mL圆底烧瓶中,然后加入按照乙醇:丙酮:水质量比为3:2:0.1的混合液为提取液,其中,提取液与松树粉末按照质量比为1:30,再将圆底烧瓶放入微波反应器中,在微波功率为85W,温度为45℃条件下进行微波提取1min,得到混合提取液;(2) Microwave extraction: take by weighing the spare pine bark powder, place in the 250mL round-bottomed flask with reflux condenser, then add according to ethanol: acetone: the mixed solution that water mass ratio is 3:2:0.1 is extraction liquid, Among them, the mass ratio of the extract to the pine tree powder is 1:30, and then the round bottom flask is put into a microwave reactor, and the microwave power is 85W, and the temperature is 45°C, and the microwave extraction is carried out for 1min to obtain the mixed extract;

(3)纯化:将得到混合提取液冷却至常温后进行抽滤,将滤液40℃下真空浓缩后,在60℃下真空干燥至质量恒定,即可得白桦树单宁提取物。(3) Purification: the obtained mixed extract was cooled to normal temperature, then suction filtered, the filtrate was concentrated in vacuum at 40°C, and then vacuum-dried at 60°C until the quality was constant to obtain the birch tannin extract.

经过计算,本实施例最后所得单宁总量为112.35mg/100g。After calculation, the total amount of tannins obtained in this embodiment is 112.35mg/100g.

实施例3Example 3

一种从松树皮提取单宁的工艺,该工艺包括以下步骤:A process for extracting tannin from pine bark, the process comprises the following steps:

(1)预处理:将松树皮自然晾晒风干后粉碎过100目筛,得到松树皮粉末,备用;(1) pretreatment: the pine bark is naturally air-dried and then pulverized through a 100-mesh sieve to obtain pine bark powder for subsequent use;

(2)微波提取:称取备用的松树皮粉末,置于带回流冷凝管的250mL圆底烧瓶中,然后加入按照乙醇:丙酮:水质量比为13:9:0.4的混合液为提取液,其中,提取液与松树粉末按照质量比为1:25,再将圆底烧瓶放入微波反应器中,在微波功率为81W,温度为45℃条件下进行微波提取1min,得到混合提取液;(2) Microwave extraction: take by weighing the spare pine bark powder, place in the 250mL round-bottomed flask with reflux condenser, then add according to ethanol: acetone: the mixed solution that water mass ratio is 13:9:0.4 is extracting liquid, Among them, the mass ratio of the extract to the pine tree powder is 1:25, and then the round bottom flask is put into a microwave reactor, and the microwave power is 81W, and the temperature is 45°C, and the microwave extraction is carried out for 1min to obtain the mixed extract;

(3)纯化:将得到混合提取液冷却至常温后进行抽滤,将滤液40℃下真空浓缩后,在60℃下真空干燥至质量恒定,即可得白桦树单宁提取物。(3) Purification: the obtained mixed extract was cooled to normal temperature, then suction filtered, the filtrate was concentrated in vacuum at 40°C, and then vacuum-dried at 60°C until the quality was constant to obtain the birch tannin extract.

经过计算,本实施例最后所得单宁总量为119.52mg/100g。After calculation, the final total amount of tannins obtained in this embodiment is 119.52mg/100g.

实施例4Example 4

一种从松树皮提取单宁的工艺,该工艺包括以下步骤:A process for extracting tannin from pine bark, the process comprises the following steps:

(1)预处理:将松树皮自然晾晒风干后粉碎过100目筛,得到松树皮粉末,备用;(1) pretreatment: the pine bark is naturally air-dried and then pulverized through a 100-mesh sieve to obtain pine bark powder for subsequent use;

(2)微波提取:称取备用的松树皮粉末,置于带回流冷凝管的250mL圆底烧瓶中,然后加入按照乙醇:丙酮:水质量比为14:9:0.3的混合液为提取液,其中,提取液与松树粉末按照质量比为1:29,再将圆底烧瓶放入微波反应器中,在微波功率为84W,温度为45℃条件下进行微波提取1min,得到混合提取液;(2) Microwave extraction: take the standby pine bark powder, place it in a 250mL round-bottomed flask with a reflux condenser, then add the mixed solution according to ethanol: acetone: water mass ratio of 14:9:0.3 as the extract, Among them, the mass ratio of the extract to the pine tree powder is 1:29, and then the round bottom flask is put into a microwave reactor, and the microwave power is 84W, and the temperature is 45°C, and the microwave extraction is carried out for 1min to obtain the mixed extract;

(3)纯化:将得到混合提取液冷却至常温后进行抽滤,将滤液40℃下真空浓缩后,在60℃下真空干燥至质量恒定,即可得白桦树单宁提取物。(3) Purification: the obtained mixed extract was cooled to normal temperature, then suction filtered, the filtrate was concentrated in vacuum at 40°C, and then vacuum-dried at 60°C until the quality was constant to obtain the birch tannin extract.

经过计算,本实施例最后所得单宁总量为120.11mg/100g。After calculation, the total amount of tannins obtained in this embodiment is 120.11mg/100g.

本发明所提供的松树皮提取单宁提取工艺简单、成本低、提取率高,经高效液相色谱分析表明该成品的单宁含量高,纯度高,且具有较高的生物活性,具有很高的应用价值。The pine bark extraction tannin provided by the present invention has simple extraction process, low cost, and high extraction rate. Analysis by high-performance liquid chromatography shows that the finished product has high tannin content, high purity, and high biological activity. application value.

Claims (4)

1. extract a technique for tannin from Cortex Pini, it is characterized in that, this technique comprises the following steps:
(1) pre-treatment: pulverized 100 mesh sieves after air-dry for Cortex Pini natural drying, obtain Cortex Pini powder, for subsequent use;
(2) microwave extraction: take Cortex Pini powder for subsequent use, be placed in the round-bottomed flask of band reflux condensing tube, then extracting solution is added, again round bottom flask is entered in microwave reactor, be 80-85W at microwave power, temperature is carry out microwave extraction 1min under 45 DEG C of conditions, obtains mixed extract;
(3) purifying: will obtain carrying out suction filtration after mixed extract is cooled to normal temperature, after vacuum concentration at filtrate 40 DEG C, vacuum-drying is to constant mass at 60 DEG C, white birch tanning extract.
2. a kind of technique extracting tannin from Cortex Pini according to claim 1, is characterized in that: extracting solution described in described step (2) and pine tree powder are 1:20-30 according to mass ratio.
3. a kind of technique extracting tannin from Cortex Pini according to claim 1, is characterized in that: described extracting solution is according to ethanol: acetone: quality is than the mixed solution for 10-15:8-10:0.3-0.5.
4. a kind of technique extracting tannin from Cortex Pini according to claim 3, is characterized in that: the specification of described round-bottomed flask is 250mL.
CN201510329287.7A 2015-06-15 2015-06-15 Process of extracting tannin from pine bark Pending CN104974198A (en)

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CN112458132A (en) * 2020-11-17 2021-03-09 汕头大学 Method for preparing multi-element antibacterial probiotic by using single raw material

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CN109403025A (en) * 2018-10-22 2019-03-01 太和县瑞丝源发制品有限公司 A kind of production method of wig nursing Essence
CN112458132A (en) * 2020-11-17 2021-03-09 汕头大学 Method for preparing multi-element antibacterial probiotic by using single raw material

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