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CN1263139A - Wet extraction method of flax glue from flax seed - Google Patents

Wet extraction method of flax glue from flax seed Download PDF

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CN1263139A
CN1263139A CN 99100664 CN99100664A CN1263139A CN 1263139 A CN1263139 A CN 1263139A CN 99100664 CN99100664 CN 99100664 CN 99100664 A CN99100664 A CN 99100664A CN 1263139 A CN1263139 A CN 1263139A
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leaching
semen lini
flax
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shell
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CN1075540C (en
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胡鑫尧
刘崇义
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Tsinghua University
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Abstract

本发明涉及一种从亚麻子中湿法提取亚麻胶的方法,该方法是首先将亚麻子粉碎,并使壳、仁分离,对壳皮筛分后用温水浸取二次,对浸取混合物进行过滤,将滤液干燥后即为产品亚麻胶;或用温水浸取一次,再用盐酸及18碳烯酸混合液浸取一次,将浸取液烘干,即为产品;或用卫生醇浸取二次,对浸取混合物进行过滤,将滤液减压蒸馏后即得产品。本发明方法具有工艺简单,易操作,产品提取率高,纯度高,无毒性等优点。The invention relates to a method for wet extraction of linseed gum from linseed. The method is firstly to crush the linseed, separate the husk and the kernel, leaching the husk and skin twice with warm water after sieving the leaching mixture. After filtering, drying the filtrate is the product flax glue; or leaching once with warm water, then leaching once with a mixture of hydrochloric acid and 18-decenyl acid, and drying the leaching solution, which is the product; or leaching with sanitary alcohol Take it twice, filter the leaching mixture, and distill the filtrate under reduced pressure to obtain the product. The method of the invention has the advantages of simple process, easy operation, high product extraction rate, high purity, non-toxicity and the like.

Description

一种从亚麻子中湿法提取亚麻胶的方法A method for wet extraction of linseed gum from linseed

本发明涉及一种从亚麻(俗称胡麻)子中湿法提取亚麻胶的方法,属化学工艺技术领域。The invention relates to a method for wet extraction of flax gum from flax (commonly known as flax) seeds, which belongs to the technical field of chemical technology.

亚麻胶(英文名Flaxseed mucilage;拉丁文名为:Linseed mucilage),是生物、食品、制药等工业中应用甚广的天然(绿色)植物胶。中国专利CN1072184A,公开了一种将亚麻子直接用水浸取(50℃~95℃)并加入亚硫酸和柠檬酸作为助浸剂而浸出胶体的方法。上述方法的缺点是,一、亚麻子被浸取提胶后,还要将被浸取的亚麻子重新干燥,再去榨油,这种再重新干燥工艺必然要大量消耗能源,这在工业化生产及经济上均不可取;二、上述方法均为实验室试验,尚未进行工业化生产,从其过程看,难于自动化生产,多由单机或人工操作;三、其干燥方法可能使胶变性;四、缺少综合利用考虑,而仅仅考虑提胶;五、加入的助浸取剂亚硫酸,对食用产品,特别对作为“绿色”食品是不利的,因为带入不应有的亚硫酸根。Flaxseed mucilage (English name: Flaxseed mucilage; Latin name: Linseed mucilage) is a natural (green) vegetable glue widely used in biology, food, pharmaceutical and other industries. Chinese patent CN1072184A discloses a method of leaching linseed directly with water (50° C. to 95° C.) and adding sulfurous acid and citric acid as leaching aids to extract the colloid. The shortcoming of above-mentioned method is, one, after the linseed is leached to extract gum, also will be leached linseed to dry again, go to oil again, this re-drying process must consume a large amount of energy again, this is in industrialized production and economically are all undesirable; two, the above-mentioned methods are all laboratory experiments, and industrialized production has not yet been carried out. From the perspective of its process, it is difficult to automate production, and it is mostly operated by a stand-alone or manual operation; three, its drying method may make the glue denature; four, Lack of comprehensive utilization considerations, but only consider gel extraction; five, the added sulfurous acid leaching aid is unfavorable to edible products, especially as "green" food, because undue sulfites are brought in.

本发明的目的是研究一种从亚麻子壳中湿法提取亚麻胶的方法,对亚麻子进行综合利用,亚麻油可用于提取亚麻酸,残油可改制工业润滑油,果仁榨饼可用于混合饲料,使亚麻子有更广泛的用途,提高亚麻子的附加值。The purpose of the present invention is to study a method for wet extraction of linseed gum from linseed husks, comprehensive utilization of linseed, linseed oil can be used to extract linolenic acid, residual oil can be transformed into industrial lubricating oil, and nut cake can be used for The mixed feed makes the linseed more widely used and increases the added value of the linseed.

本发明设计的从亚麻子壳中湿法提取亚麻胶的方法,包括下列各步骤:The method for the wet extraction of flax glue designed by the present invention comprises the following steps:

(1)对亚麻子进行子壳和果仁分离,以得到亚麻子壳;(1) Separating the linseed from the husks and kernels to obtain the linseed husks;

(2)从亚麻子壳中提取亚麻胶,提取的方法为:用30~50℃的温水浸取亚麻子壳0.5~2小时,对浸取物压滤,将滤出的渣,再用50~85℃的温水浸取0.5~1小时,对浸取物过滤,将上述压滤和过滤所得到的滤液在40~60℃下干燥2~5小时,即得产品亚麻胶;(2) Extract linseed gum from linseed husks, the extraction method is: leaching linseed husks with warm water at 30-50°C for 0.5-2 hours, press-filtering the leached material, and using 50 Leak in warm water at ~85°C for 0.5-1 hour, filter the extract, and dry the filtrate obtained by the above-mentioned pressure filtration and filtration at 40-60°C for 2-5 hours to obtain the product flax glue;

或用30~50℃的温水浸取亚麻子壳0.5~2小时,对浸取物压滤,将滤出的渣用浓度为0.1的盐酸和1M18碳烯酸浸取0.5~1小时,使其PH值为2.5~4,对浸取物进行过滤,将上述压滤和过滤所得的滤液烘干,即得产品亚麻胶;Or use warm water at 30-50°C to extract linseed shells for 0.5-2 hours, press-filter the extract, and leaching the filtered residue with hydrochloric acid and 1M18 carbenic acid at a concentration of 0.1 for 0.5-1 hour to make it The pH value is 2.5 to 4, the extract is filtered, and the filtrate obtained by the above-mentioned pressure filtration and filtration is dried to obtain the product flax glue;

或用亚麻子壳与醇的体积比为1∶1~3,浓度为80%的卫生醇,在15~25℃下浸取亚麻子壳2~4小时,对浸取物过滤,将滤出的渣再以体积比为1∶1~3、浓度为80%的卫生醇,在20~45℃下浸取1~2小时,对浸取物进行过滤,将上述二次过滤液在0.5个大气压下进行减压蒸馏,除去其中的所含的醇,剩下粉状物即为产品亚麻胶。Or use the volume ratio of linseed husk and alcohol as 1:1-3, the concentration is 80% hygienic alcohol, leaching linseed husk at 15-25 ℃ for 2-4 hours, filtering the extract, and filtering out The slag is then leached for 1 to 2 hours at 20 to 45°C with a volume ratio of 1:1 to 3 and a concentration of 80% sanitation alcohol, and the leachate is filtered. Carry out vacuum distillation under atmospheric pressure to remove the alcohol contained therein, and the remaining powder is the product flax gum.

上述工艺中的亚麻子的子壳和果仁的分离可用旋转磨、锥形磨或平板沙盘气流磨中的任何一种,磨的转速为50~180转/分,气流速度为30~90升/分。The separation of the linseed husks and nuts in the above process can be done by any one of rotary mill, conical mill or flat sand table airflow mill, the rotating speed of the mill is 50-180 rpm, and the air velocity is 30-90 liters /point.

上述三种不同的浸取方法,根据所需产品的要求而定,即若制备低蛋白胶,则用温水浸取,若制备高蛋白胶,则用盐酸与18碳烯酸高温浸取,若制备混合胶,则用醇浸取。The above three different leaching methods are determined according to the requirements of the desired product, that is, if the low-protein glue is prepared, it is leached with warm water; To prepare the mixed glue, use alcohol leaching.

上述干燥工艺可用干燥方法可用已工业化的常温喷雾干燥、减压蒸馏和红外线干燥等方法。The available drying methods for the above-mentioned drying process can be industrialized methods such as normal temperature spray drying, vacuum distillation and infrared drying.

使用本发明研究的提取亚麻胶的方法,亚麻胶的提取率可以高达82~95%,使亚麻子应用的经济附加值提高10~20倍,而且提取的亚麻胶无毒性,纯度高,可广泛用于生物、食品、医药等领域,因而本发明的方法具有明显的工业生产性和经济效益。Using the method for extracting flax gum researched by the present invention, the extraction rate of flax gum can be as high as 82-95%, which increases the economic added value of flaxseed application by 10-20 times, and the extracted flax gum is non-toxic, high in purity, and can be widely used It is used in the fields of biology, food, medicine, etc., so the method of the present invention has obvious industrial productivity and economic benefits.

下面介绍本发明的实施例:Introduce the embodiment of the present invention below:

实施例1:Example 1:

取亚麻种子为原料,精选,筛分出直径为0.8mm以上的亚麻子,用旋转磨将其粉碎,并用气流使壳皮和果仁分离,旋转磨转速为100转/分,气流速度为45升/分。分出的核仁榨油。将得到的壳皮进行筛分,取20~100目之间的壳皮,用40℃温水浸取1小时,对浸取物压滤,将滤出的渣再用60℃温水浸取0.5小时,对浸取物过滤,将上述二次滤液在50℃下干燥3小时,即得粉末状产品亚麻胶,亚麻胶的提取率为90%。Take flax seeds as raw materials, select and screen flax seeds with a diameter of 0.8 mm or more, crush them with a rotary mill, and separate the shells and nuts with airflow. The rotational speed of the rotary mill is 100 rpm, and the airflow speed is 45 l/min. Extract oil from the separated kernels. Sieve the obtained shells, take the shells between 20 and 100 mesh, soak them in warm water at 40°C for 1 hour, press filter the extracts, and soak the filtered residue in warm water at 60°C for 0.5 hours , filter the extract, and dry the above secondary filtrate at 50° C. for 3 hours to obtain the powdered product flax gum, the extraction rate of flax gum is 90%.

实施例2:Example 2:

取亚麻种子为原料,精选,筛分出直径为0.8mm以上的亚麻子,用平板沙盘气流磨将其粉碎,并用气流使壳皮和果仁分离,旋转磨转速为150转/分,气流速度为60升/分。分出的核仁榨油。将得到的壳皮进行筛分,取20~100目之间的壳皮,用50℃温水浸取1小时,对浸取物压滤,将滤出的渣再用60℃温水浸取1小时,将上述二次滤液在40℃下干燥5小时,即得粉末状产品亚麻胶,亚麻胶的提取率为90%。Take flax seeds as raw material, select and screen flax seeds with a diameter of 0.8mm or more, crush them with a flat sand table airflow mill, and separate the shell and nuts with an airflow. The rotational speed of the rotary mill is 150 rpm, and the airflow The speed is 60 l/min. Extract oil from the separated kernels. Sieve the obtained shells, take shells between 20 and 100 mesh, soak them in warm water at 50°C for 1 hour, press filter the extract, and soak the filtered residue in warm water at 60°C for 1 hour , the above-mentioned secondary filtrate was dried at 40°C for 5 hours to obtain the powdered product flax gum, and the extraction rate of flax gum was 90%.

实施例3:Example 3:

取亚麻种子为原料,精选,筛分出直径为0.8mm以下的亚麻子,用旋转磨将其粉碎,然后用冷法榨取其中亚麻油,将压榨饼搅碎后,用40℃温水浸取1小时,对浸取物压滤,将滤出的渣再用浓度为0.1的盐酸和1M18碳烯酸浸取1小时,使其PH值为3,对浸取物过滤,将上述二次滤液用减压蒸馏法使其干燥,即得粉末状产品亚麻胶,亚麻胶的提取率为93%。Take linseed as raw material, select, sieve out the linseed with a diameter of less than 0.8mm, crush it with a rotary mill, and then extract the linseed oil in the cold method, crush the pressed cake, and soak it in warm water at 40°C For 1 hour, press filter the extract, and leaching the filtered residue with hydrochloric acid and 1M18 olefinic acid with a concentration of 0.1 for 1 hour to make the pH value 3, filter the extract, and filter the above secondary filtrate Dry it by vacuum distillation to obtain the powdered product flax gum, the extraction rate of flax gum is 93%.

实施例4:Example 4:

取亚麻种子为原料,精选,筛分出直径为0.8mm以上的亚麻子,用旋转磨将其粉碎,并用气流使壳片和果仁分离,旋转磨转速为100转/分,气流速度为45升/分。分出的核仁榨油。将得到的壳皮进行筛分,取20~100目之间的壳皮,用40℃温水浸取1小时,对浸取物压滤,将滤出的渣再用浓度为0.1的盐酸和1M18碳烯酸浸取1小时,使其PH值为3,对浸取物过滤,将上述二次滤液用喷雾干燥法使其干燥,在50℃下干燥3小时,即得粉末状产品亚麻胶,亚麻胶的提取率为90%。Take flax seeds as raw material, select, screen out flaxseeds with a diameter of 0.8mm or more, pulverize them with a rotary mill, and separate the shells and nuts with an airflow. The rotational speed of the rotary mill is 100 rpm, and the airflow speed is 45 l/min. Extract oil from the separated kernels. Sieve the obtained shells, take shells between 20 and 100 meshes, soak them in warm water at 40°C for 1 hour, filter the extracts, and filter the filtered residue with hydrochloric acid with a concentration of 0.1 and 1M18 Carbenic acid was leached for 1 hour to make the pH value 3, and the leached material was filtered, and the above-mentioned secondary filtrate was dried by spray drying method, and dried for 3 hours at 50 ° C to obtain the powdered product flax gum. The extraction rate of flax gum is 90%.

实施例5:Example 5:

取亚麻种子为原料,精选,筛分出直径为0.8mm以上的亚麻子,用锥齿磨将其粉碎,并用气流使壳皮和果仁分离,锥齿磨转速为100转/分,气流速度为45升/分。分出的核仁榨油。将得到的壳皮进行筛分,取20~100目之间的壳皮,以壳皮与乙醇体积为1∶1的比例,用乙醇浸取亚麻子壳,温度为15℃,浸取时间为3小时,对浸取物过滤,对滤渣再用1∶2的乙醇浸取,温度为25℃,时间为1.5小时,最后在0.5个大气压下进行减压蒸馏,除去其中的乙醇,即得粉末状产品亚麻胶,亚麻胶的提取率为85%。Take flax seeds as raw material, select and screen flax seeds with a diameter of 0.8mm or more, crush them with a bevel tooth mill, and use airflow to separate the shell from the nut. The speed is 45 l/min. Extract oil from the separated kernels. Sieve the obtained husks, take the husks between 20 and 100 meshes, and use ethanol to extract the linseed husks with the volume ratio of the husks and ethanol at a ratio of 1:1. The temperature is 15° C., and the leaching time is After 3 hours, filter the extract, then extract the filter residue with 1:2 ethanol at a temperature of 25°C for 1.5 hours, and finally carry out vacuum distillation at 0.5 atmospheric pressure to remove the ethanol and obtain the powder The flax gum is a product with the extraction rate of 85%.

实施例6:Embodiment 6:

取亚麻种子为原料,精选,筛分出直径为0.8mm以上的亚麻子,用旋转磨将其粉碎,并用气流使壳皮和果仁分离,旋转磨转速为100转/分,气流速度为45升/分。分出的核仁榨油。将得到的壳皮进行筛分,取20~100目之间的壳皮,用丙醇浸取亚麻子壳,其比例为丙醇∶亚麻子壳=2∶1,丙醇浓度为80%,浸取温度为40℃,浸取1小时,对浸取物过滤,对滤渣再用2∶1的丙醇浸取,温度为40℃,浸取0.5小时,最后在0.5个大气压下减压蒸馏,即得粉末状产品亚麻胶,亚麻胶的提取率为90%。Take flax seeds as raw materials, select and screen flax seeds with a diameter of 0.8 mm or more, crush them with a rotary mill, and separate the shells and nuts with airflow. The rotational speed of the rotary mill is 100 rpm, and the airflow speed is 45 l/min. Extract oil from the separated kernels. The obtained shells are screened, and the shells between 20 and 100 meshes are taken, and the linseed shells are extracted with propanol, the ratio is propanol: linseed shells=2: 1, and the concentration of propanol is 80%. The leaching temperature is 40°C, leaching for 1 hour, filtering the leaching material, and leaching the filter residue with 2:1 propanol at a temperature of 40°C, leaching for 0.5 hours, and finally distilling under reduced pressure at 0.5 atmospheres , to obtain the powdered product flax glue, the extraction rate of flax glue is 90%.

Claims (2)

1, a kind of from Semen Lini wet method extract the method for flax glue, it is characterized in that this method comprises following each step:
(1) Semen Lini is carried out sub-shell and separate, to obtain the Semen Lini shell with kernel;
(2) from the Semen Lini shell, extract flax glue, the method of extracting is: leached the Semen Lini shells 0.5~2 hour with 30~50 ℃ warm water, to the press filtration of leaching thing, with the slag that leaches, again with 50~85 ℃ warm water leaching 0.5~1 hour, the leaching thing is filtered, with above-mentioned press filtration and filter resulting filtrate 40~60 ℃ dry 2~5 hours down, promptly get the product flax glue;
Or with 30~50 ℃ warm water leaching Semen Lini shell 0.5~2 hour, to the press filtration of leaching thing, with the slag concentration that leaches is 0.1 hydrochloric acid and the leaching of 1M18 carbon enoic acid 0.5~1 hour, making its pH value is 2.5~4, the leaching thing is filtered, filtrate oven dry with above-mentioned press filtration and filtration gained promptly gets the product flax glue;
Or with the Semen Lini shell with alcohol volume ratio be 1: 1~3, concentration is 80% health alcohol, leached the Semen Lini shell 2~4 hours down at 15~25 ℃, the leaching thing is filtered, with the slag that leaches again with volume ratio be 1: 1~3, concentration is 80% health alcohol, 20~45 ℃ of leachings 1~2 hour down, the leaching thing is filtered, above-mentioned secondary filtration liquid is carried out underpressure distillation under 0.5 normal atmosphere, remove wherein contained alcohol, remaining meal is the product flax glue.
2, the method for claim 1 is characterized in that, wherein Semen Lini is pulverized and used any in rotation mill, conoidal mill or the dull and stereotyped sand table airflow milling, and the rotating speed of mill is 50~180 rev/mins, and gas velocity is 30~90 liters/minute.
CN99100664A 1999-02-12 1999-02-12 Wet extraction method of flax glue from flax seed Expired - Fee Related CN1075540C (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002038690A1 (en) * 2000-11-09 2002-05-16 Xinjiang Lvqi Biological Products Company Limited A method of extracting flax gum from flax seed
CN1112416C (en) * 2000-02-01 2003-06-25 新疆昌吉市绿旗生物制品有限责任公司 Technology for producing flaxseed gum
CN100344719C (en) * 2006-01-19 2007-10-24 中国科学院山西煤炭化学研究所 Method for producing linen glue
CN108359021A (en) * 2018-02-24 2018-08-03 广州利众生物科技有限公司 A kind of method that quick preparation has antiviral and immunoregulatory activity Linseed pigment
US10835552B2 (en) 2015-07-03 2020-11-17 Jinan University Method for preparing linseed polysaccharide having antiviral activity and immunological activity, and use of the linseed polysaccharide
CN115162041A (en) * 2022-06-22 2022-10-11 中国农业科学院油料作物研究所 A method for extracting high-purity cellulose from flaxseed husks

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1031715C (en) * 1991-11-14 1996-05-01 巴勇舸 Method for flax glue extracted from flax seeds

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1112416C (en) * 2000-02-01 2003-06-25 新疆昌吉市绿旗生物制品有限责任公司 Technology for producing flaxseed gum
WO2002038690A1 (en) * 2000-11-09 2002-05-16 Xinjiang Lvqi Biological Products Company Limited A method of extracting flax gum from flax seed
CN100344719C (en) * 2006-01-19 2007-10-24 中国科学院山西煤炭化学研究所 Method for producing linen glue
US10835552B2 (en) 2015-07-03 2020-11-17 Jinan University Method for preparing linseed polysaccharide having antiviral activity and immunological activity, and use of the linseed polysaccharide
CN108359021A (en) * 2018-02-24 2018-08-03 广州利众生物科技有限公司 A kind of method that quick preparation has antiviral and immunoregulatory activity Linseed pigment
CN108359021B (en) * 2018-02-24 2020-08-21 广州利众生物科技有限公司 A method for rapidly preparing flaxseed polysaccharide with antiviral and immunomodulatory activities
CN115162041A (en) * 2022-06-22 2022-10-11 中国农业科学院油料作物研究所 A method for extracting high-purity cellulose from flaxseed husks
CN115162041B (en) * 2022-06-22 2024-09-17 中国农业科学院油料作物研究所 Method for extracting high-purity cellulose from flaxseed shells

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