WO2014071736A1 - 一种提取蚕蛹油的方法 - Google Patents

一种提取蚕蛹油的方法 Download PDF

Info

Publication number
WO2014071736A1
WO2014071736A1 PCT/CN2013/077521 CN2013077521W WO2014071736A1 WO 2014071736 A1 WO2014071736 A1 WO 2014071736A1 CN 2013077521 W CN2013077521 W CN 2013077521W WO 2014071736 A1 WO2014071736 A1 WO 2014071736A1
Authority
WO
WIPO (PCT)
Prior art keywords
oil
silkworm
silkworm pupa
minutes
extraction
Prior art date
Application number
PCT/CN2013/077521
Other languages
English (en)
French (fr)
Inventor
张耀洲
王玉芳
陈剑清
舒特俊
Original Assignee
天津耀宇生物技术有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 天津耀宇生物技术有限公司 filed Critical 天津耀宇生物技术有限公司
Publication of WO2014071736A1 publication Critical patent/WO2014071736A1/zh

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00Refining fats or fatty oils

Definitions

  • the present invention relates to the field of food processing technology, and particularly relates to a method for extracting silkworm pupa oil by using a silkworm pupa as a raw material. Background technique
  • Natural oils and fats are widely found in animals and plants. They are contained in the body of animals, such as butter, lard, and sheep oil. Among the plants, there are perilla oil, linseed oil, and evening primrose oil. Grease is not only one of the main substances that human beings depend on, but also an important industrial raw material, and has a wide range of uses in the fields of food, medicine, cosmetics, leather industry and the like. China's oil and fat resources are seriously inadequate. China's three major edible oils, such as soybean oil, palm oil and rapeseed oil, rank first in the world, and total imports account for 18% of global trade. Therefore, experts have called for increased oil development, increased oil extraction rates, and increased oil production.
  • Silkworm cocoon is a kind of medicine and food. It is the main by-product of the silk industry. It can produce 1.5 tons of dried silkworm cocoons per ton of raw silk.
  • the silkworm cocoons are the most abundant stage of storage during the metamorphosis of silkworms.
  • a variety of natural active substances and pheromones are energy sources that support the emergence, flight, reproduction and embryonic development of silkworm moths, with very important nutritional value and health care functions.
  • China is a major producer of silkworm. Domestically, more than 200,000 tons of silkworm cocoons are available every year. However, due to the lack of deep processing technology, they are basically used as feed or fertilizer, and the resource utilization rate is low, resulting in great waste.
  • Silkworm pupa oil is a mixture of various high-grade fatty acid glycerides extracted from silkworm pupa. It has a yellow to red transparent oily liquid.
  • the content of unsaturated fatty acids in silkworm pupa oil is very high, about 75%, rich in essential linoleic acid and ⁇ -linolenic acid, etc., its content is about: oleic acid 33%, ⁇ -linolenic acid 35%, sub 8 % oleic acid, functional and nutritional studies at home and abroad have shown that alpha-linolenic acid has important protection Health function: Reduce blood lipids, cholesterol and blood pressure, prevent cardiovascular disease; inhibit platelet aggregation, prevent thrombosis and stroke; enhance retinal reflex ability, prevent vision deterioration; enhance memory. Therefore, silkworm cocoon oil products can be used to improve and prevent diseases such as hyperlipemia, hyperglycemia, and hypertension.
  • the extraction method of silkworm pupa oil mainly includes pressing method, including raw pressing method, hot pressing method, boiling pressing method and leaching method, also known as extraction method and Soxhlet fat extraction method and supercritical method, but the silkworm pupa is high protein. Highly lipid substances, the protein after extracting oil by pressing method has been denatured, and the content of crude fiber in silkworm cocoons is less, the texture is softer, the oil yield of pressing is very low, and the pressing method is not convenient.
  • the use of Soxhlet fat extraction is not only time-consuming and labor-intensive, but also requires the heating in the extraction process, which also affects the quality of the proposed grease.
  • the organic solvent extraction method has low cost and low energy consumption, but has the disadvantages of long extraction time and low extraction rate; supercritical carbon dioxide extraction has high extraction rate and short extraction time, but requires high equipment and high energy consumption, and homogenization.
  • the method-assisted extraction method has not been reported in the extraction of silkworm pupa oil, which effectively shortens the extraction time, and is easy to operate and easy to grasp. Homogenization enhances the rate and effect of the extraction process, which facilitates the extraction of oil. Summary of the invention
  • the present invention provides a method for extracting silkworm pupa oil from silkworm pupa by a homogenization method with simple operation, high extraction rate, short extraction time and low production cost.
  • the extract is filtered with 4 ⁇ 8 layers of gauze.
  • the filtrate is collected and centrifuged at 4000 ⁇ 8000 rpm/min for 10 ⁇ 30 minutes.
  • the supernatant is collected and the supernatant is placed in a vacuum filter at room temperature.
  • the filtrate was obtained by vacuum filtration at -0.08 MPa, and the filtrate was distilled under reduced pressure in a vacuum evaporator at 60-80 ° C and -0.08 MPa to recover the extraction solvent, and the residue was removed in an oven at 40 to 50 ° C. Extracting the solvent to obtain silkworm oil;
  • the super alkali content of the refining silkworm oil is determined. 74.4%, at this time the hardness of the soap angle is suitable, the oil soap is easy to separate, the acid value and the color are all required; when the initial temperature of the oil is 45 ° C; adding a mass fraction of 14% potassium hydroxide aqueous solution, mixing and stirring 30 ⁇ 40 In the minute and continue to heat up until the temperature of the silkworm cocoon oil is controlled at 60 ⁇ 65 °C, the oil soap is quickly centrifuged at 3000 ⁇ 4000rpm/min, the upper layer of oil is removed, and the washing is stirred at 120 rpm/min with 80 °C distilled water until the washing liquid The pH value is neutral and the purpose of deacidification is achieved.
  • the decolorized white clay which accounts for 4% of the silkworm pupa oil is added to the silkworm pupa oil after deacidification.
  • the temperature of the silkworm pupa oil is controlled at 40 ⁇ 42 °C, stirred for 30 minutes, and the bleached white clay is separated by filtration. Refined silkworm cocoon oil.
  • the mass ratio of the silkworm pupa powder to the extraction solvent in the above step (b) is 1:4-6. Further, the mass ratio of the silkworm meal to the extraction solvent in the above step (b) is 1:4.
  • the solvent extracted in the above step (b) is petroleum ether, ethyl acetate or absolute ethanol. Further, in the above step (b), the rotational speed of the homogenizer is 6000 to 8000 rpm/min.
  • the invention has the advantages that the invention has the advantages of simple process steps, high extraction rate, short extraction time and low production cost, and can be used for preparing silkworm pupa oil from silkworm pupa.
  • the prepared silkworm pupa oil has a yellow color and oily aroma.
  • the indexes meet the quality standards of silkworm pupa oil reported in the literature, and can be used as an edible oil or as a health food base. detailed description
  • Example 1 The present invention will be further described below in conjunction with the embodiments. However, the invention is not limited to these embodiments.
  • Example 1
  • the wet silkworm cocoons are placed in a blast drying oven at 120 ° C for 12 hours and dried until the water content is less than 8%.
  • the obtained homogenate was filtered through 4 to 8 layers of gauze, and the filtrate was collected and centrifuged at 4000 to 8000 rpm/min for 10 to 30 minutes. The supernatant was collected and the supernatant was placed in a vacuum filter. The filtrate was filtered under reduced pressure at -0.08 MPa at room temperature to obtain a filtrate; the filtrate was distilled under reduced pressure at 60-80 ° C, -0.08 MPa in a vacuum evaporator, and the extraction solvent was recovered in an oven at 40 to 50 ° C. The residue extraction solvent is removed to obtain silkworm oil.
  • citric acid crystals (C 6 H 8 0 7 -H 2 0 ) which are 0.05% of silkworm pupa oil to the silkworm pupa oil heated to 70 °C. After mixing, let stand for 5-6 minutes, which will remain in the silkworm pupa oil. Calcium, magnesium, iron and other divalent metal ions Ca 2+ , Mg 2+ , Fe 2+ become free, move to the aqueous phase, and then centrifuged at 3000 ⁇ 4000 rpm / min to remove, thereby achieving the purpose of degumming The acid value can not be higher than 0.2 mgKOH/g. Under the condition of considering the soap foot and color, the super alkali content of the refined silkworm oil is determined to be 74.4%.
  • the hardness of the soap angle is suitable, the oil soap is easy to separate, and the acid value is And the color is up to the requirement; when the initial temperature of the oil is 45 °C; add a potassium hydroxide aqueous solution with a mass fraction of 14%, mix and stir for 30 to 40 minutes and continue to heat up until the temperature of the silkworm cocoon is controlled at 60 ⁇ 65 °C.
  • the oil soap is quickly centrifuged by 3,000-4000 rpm/min, the upper layer of oil is removed, and the mixture is washed with 120 ° C distilled water at 120 rpm/min until the pH of the washing liquid is neutral, and the purpose of deacidification is achieved;
  • the silkworm pupa oil Controlled at 40 ⁇ 42 ° C, stirred for 30 minutes, bleaching clay was separated by filtration to obtain refined oils pupa.
  • the wet silkworm cocoons are placed in a blast drying oven at 120 ° C for 12 hours and dried until the water content is less than 8%.
  • the obtained homogenate is filtered with 4 ⁇ 8 layers of gauze, the filtrate is collected, centrifuged at 4000 ⁇ 8000 rpm / min for 10 ⁇ 30 minutes, the supernatant is collected, and the supernatant is placed in a vacuum filter at room temperature.
  • the filtrate was filtered under reduced pressure at -0.08 MPa to obtain a filtrate; the filtrate was distilled under reduced pressure at 60-80 ° C and -0.08 MPa in a vacuum evaporator to recover the extraction solvent, and the residue was removed in an oven at 40 to 50 ° C.
  • the solvent is extracted and the silkworm oil is obtained.
  • the citric acid crystal ( C 6 H 8 0 7 -H 2 0 ) which accounts for 0.08 % of the silkworm pupa oil is added, and after mixing, it is allowed to stand for 5-6 minutes, which will remain in the silkworm pupa oil.
  • the acid value can not be higher than 0.2 mg KOH / g as the standard, in the case of comprehensive consideration of soap feet and color, the determination of the super alkali content of the refining silkworm pupa oil is 74.4%, at this time the hardness of the saponin angle is suitable, the oil soap is easy to separate, The acid value and color are all required.
  • the wet silkworm cocoons are placed in a blast drying oven at 120 ° C for 12 hours and dried until the water content is less than 8%.
  • the obtained homogenate is filtered with 4 ⁇ 8 layers of gauze, the filtrate is collected, centrifuged at 4000 ⁇ 8000 rpm / min for 10 ⁇ 30 minutes, the supernatant is collected, and the supernatant is placed in a vacuum filter at room temperature.
  • the filtrate was filtered under reduced pressure at -0.08 MPa to obtain a filtrate; the filtrate was distilled under reduced pressure at 60-80 ° C and -0.08 MPa in a vacuum evaporator to recover the extraction solvent, and the residue was removed in an oven at 40 to 50 ° C.
  • the solvent is extracted and the silkworm oil is obtained.
  • the citric acid crystal ( C 6 H 8 0 7 -H 2 0 ) which accounts for 0.12% of the silkworm pupa oil is added, and after mixing, it is allowed to stand for 5-6 minutes, which will remain in the silkworm pupa oil.
  • Calcium, magnesium, iron and other divalent metal ions Ca 2+ , Mg 2+ , Fe 2+ become free, move to the aqueous phase, and then centrifuged at 3000 ⁇ 4000 rpm / min to remove, thereby achieving the purpose of degumming
  • the acid value can not be higher than 0.2 mgKOH/g.
  • the super alkali content of the refined silkworm oil is determined to be 74.4%.
  • the hardness of the soap angle is suitable, the oil soap is easy to separate, and the acid value is And the color is up to the requirements;
  • the initial temperature of the oil is 45 °C; add a mass fraction of 14% potassium hydroxide aqueous solution, mix and stir for 30 ⁇ 40 minutes and continue to heat up until the silkworm oil temperature is controlled at 60 ⁇ 65 °C,
  • the oil soap is quickly centrifuged by centrifugation at 3000 ⁇ 4000 rpm/min, the upper layer of grease is removed, and the mixture is stirred and washed at 120 rpm/min with distilled water at 80 ° C until the pH of the washing liquid is neutral to achieve the purpose of deacidification;
  • the extraction method is as follows: In the homogenization extraction step (b) of the above examples 1-3, the silkworm pupa powder is weighed and placed 100g. In the pulverizer, petroleum ether (extraction solvent) added was replaced with ethyl acetate, and the amount to be added was the same as that of the corresponding examples, and other steps were also prepared in the same manner as in the corresponding examples to prepare refining silkworm pupa oil.
  • the extraction method is as follows: In the homogenization extraction step (b) of the above Examples 1-3, 100 g of silkworm pupa powder was weighed and placed in a homogenizer, added The petroleum ether (extraction solvent) is replaced with absolute ethanol, and the amount to be added is the same as that of the corresponding examples, and other steps should be the same as in the corresponding examples to prepare refined silkworm oil.
  • the extraction method is as follows: In the homogenization extraction step (b) of the above Examples 1 to 6, 100 g of silkworm pupa powder is weighed and placed in a homogenizer. The extraction solvent to be added and the amount to be added should be the same as in the corresponding examples, and the homogenizer was rotated at 1000 rpm/min, and the homogenate was collected. The other steps should be the same as in the corresponding examples to prepare refined silkworm pupa oil.
  • the extraction method is as follows: In the homogenization extraction step (b) of the above Examples 1 to 6, 100 g of silkworm pupa powder is weighed and placed in a homogenizer. The extraction solvent to be added and the amount to be added should be the same as in the corresponding examples, the homogenizer was rotated at 6000 rpm/min, and the homogenate was collected. The other steps should be the same as in the corresponding examples to prepare refined silkworm cocoon oil.
  • Silkworm Cocoon Provided by Zhejiang Zhongqi Biomedical Co., Ltd.
  • Reagents Petroleum ether, glacial acetic acid and other chromatographic reagents are chromatographically pure, other reagents are of analytical grade, and all reagents are sold.
  • Experimental equipment Gas chromatograph, Sakamoto Shimazu production; 1 W400A high-speed universal pulverizer, Beijing Kewei Yongxing Instrument Co., Ltd.; Thermo-RC 6+ centrifuge; Shanghai medical instrument analysis factory production; Pulping machine, Shanghai Youjie Electromechanical Equipment Development Co., Ltd.; RE-2000 rotary evaporator, produced by Shanghai Yarong Biochemical Instrument Factory; GZX-9146MB: digital display blast drying oven,
  • the supernatant was collected, and the supernatant was filtered under reduced pressure at -0.08 MPa in a vacuum filter to obtain a filtrate; the filtrate was reduced in a reduced pressure evaporator at 60 to 80 ° C, -0.08 MPa.
  • the distillation solvent is recovered, the extraction solvent is recovered, and the residual extraction solvent is removed in an oven at 40 to 50 ° C to obtain silkworm pupa oil.
  • the formula for calculating the yield of silkworm pupa oil is as follows:
  • the treatment time of the present invention is selected to be 30 to 40 minutes, preferably 30 minutes.
  • the above optimization conditions were used in the experiment. Three times of repetition, that is, the extraction solvent was petroleum ether, the mass ratio of the silkworm pupa powder to the extraction solvent was 1:4, the homogenate rotation speed was 8000 rpm/min, and the homogenization treatment time was 30 minutes.
  • the yield of silkworm cocoon oil is calculated according to formula (1), and the extraction rate is calculated as follows: yield (%) xlOO
  • the yield of the silkworm pupa oil of the present invention is increased from 24.1% to 26.9%, the extraction rate is increased from 80.3% to 89.7%, and the extraction time is shortened from 2 hours to 30%. minute.
  • the silkworm pupa oil prepared by the method provided by the present invention was tested as follows:
  • Odour Normal and no odor.
  • the silkworm pupa oil prepared by the present invention is close to the quality indexes of the silkworm pupa oil standard reported in the literature.
  • the silkworm pupa oil prepared by the present invention was analyzed for its fatty acid composition by GC-MS.
  • Chromatographic conditions VF-1701ms (30m * 0.25mm * 0.25um); Carrier gas: high purity helium; Flow rate: l.OmL / min; Inlet temperature: 250 degrees; Split ratio 20: 1; Injection volume : lul; column temperature: 80 degrees for 5 minutes, 30 degrees per minute to 200 degrees, for 1 minute, 3 degrees per minute to 230 degrees, for 10 minutes.
  • Mass spectrometry conditions EI source: 70 ev; ion source temperature 250 degrees, transmission line temperature: 260 degrees; quadrupole temperature: 40 degrees; scanning range: 35-500;
  • the present invention is compared with the existing silkworm pupa oil extraction method, the silkworm pupa oil extraction
  • the take rate is obviously improved, the extraction time is greatly shortened, the process is simple and stable, and it is suitable for industrial production.
  • the silkworm pupa oil product extracted by the invention has a yellow color and has the unique oil flavor of the silkworm pupa oil. Since the silkworm pupa oil has no national quality standard, compared with the edible oil such as rapeseed oil, the indicators meet the requirements.
  • GB1536-2004 "Rapeseed oil” quality standard fatty acid composition analysis shows that rich in polyunsaturated fatty acids, especially ⁇ -linolenic acid rich in content, is a nutritional nutrient oil with high nutritional value.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Microbiology (AREA)
  • Medicines Containing Material From Animals Or Micro-Organisms (AREA)
  • Fats And Perfumes (AREA)
  • Cosmetics (AREA)

Abstract

一种用匀浆法从蚕蛹中提取蚕蛹油的方法,包括蚕蛹预处理、匀浆法提取、制备蚕蛹油、精炼蚕蛹油等步骤。

Description

一种提取蚕蛹油的方法 技术领域 本发明属于食品加工技术领域, 具体涉及到一种以蚕蛹为原料釆用匀 浆法提取蚕蛹油的方法。 背景技术
天然油脂广泛存在于动植物体内, 含在动物体内的有牛油、 猪油、 羊 油等, 含在植物体内的有紫苏油、 亚麻油、 月见草油等。 油脂不但是人类 赖以生存的主要物质之一, 而且也是重要的工业原料, 在食品、 药品、 化 妆品、 皮革工业等技术领域具有广泛的用途。 我国油脂资源严重不足, 国 内豆油、 棕榈油、 菜籽油三大食用油脂进口量均位列世界第一, 进口总量 占全球贸易量的 18 %。 因此专家呼吁加大油脂开发、 提高油脂提取率, 加 大油脂产量。
蚕蛹是一种药食两用的资源, 是缫丝业的主要副产物, 每生产 1吨生丝 即可生产 1.5吨干蚕蛹, 蚕蛹是蚕***过程中贮藏营养最为丰富的阶段, 体 内富含的多种天然活性物质和信息素是支持蚕蛾羽化、 飞翔、 生殖和胚胎 发育的能源, 具有非常重要的营养价值和保健功能。 我国是桑蚕的主要生 产国, 国内每年有 20万吨以上蚕蛹可供利用, 但是由于缺乏深加工技术, 基本都用做饲料或肥料, 资源利用率低, 造成极大的浪费。 鉴于蚕蛹重要 的营养价值和保健功能, 国家***认定其为新资源营养食品, 蚕蛹油是 从蚕蛹中提炼出来的含有多种高级脂肪酸甘油脂的混合物, 外观呈黄至红 色的透明的油状液体, 蚕蛹油中不饱和脂肪酸的含量很高, 约为 75 % , 富 含人体必需的亚油酸及 α-亚麻酸等, 其含量约为: 油酸 33 % , α-亚麻酸 35 % , 亚油酸 8 % , 国内外的功能学及营养学研究表明 α-亚麻酸具有重要的保 健功能: 降低血脂、 胆固醇和血压, 预防心血管疾病; 抑制血小板凝集, 防止血栓形成与中风; 增强视网膜的反射能力, 预防视力退化; 增强记忆 等。 因此, 蚕蛹油脂制品可以用来改善和预防高血脂、 高血糖、 高血压等 疾病。 经国家食品药品监督局核准认定, 医药界以蚕蛹为原料已开发出了 具有降压、 降脂和护肝功能的新药。 世界卫生组织的专家试验证明, 蚕蛹 中富含的 α-亚麻酸是人体必需奇数碳脂肪酸, 在人体内代谢产生 ΕΡΑ、 DHA和***环素等。
蚕蛹油的提取方法主要有压榨法, 包括生榨法、 热榨法、 煮沸压榨法 和浸出法又称萃取法和索氏脂肪抽提法和超临界等新型提取方法, 但由于 蚕蛹是高蛋白、 高脂质物质, 使用压榨法提取油后的蛋白质多己变性, 而 且蚕蛹中粗纤维含量较少, 质地较软, 压榨出油率很低, 压榨法已不便利 用。 使用索氏脂肪抽提法, 不但费时费力, 由于抽提过程中需要加热, 还 会影响提出油脂的品质。 有机溶剂萃取法成本低、 耗能小, 但存在萃取时 间长及提取率不高的缺点; 超临界二氧化碳萃取法提取率高、 提取时间短, 但对设备要求高、 耗能大, 而匀浆法辅助萃取法在蚕蛹油提取方面还未见 报道, 其有效缩短了提取时间, 且操作简单, 易于掌握。 匀浆可强化萃取 分离过程的速率和效果, 从而有利于油脂的提取。 发明内容
为了克服现有提取蚕蛹油技术中的不足, 本发明提供一种操作简便、 提取率高、 提取时间短、 生产成本低的用匀浆法从蚕蛹中提取蚕蛹油的方 法。
为了解决问题, 本发明所釆用的具体技术方案如下:
(a)蚕蛹预处理:
将湿蚕蛹放入 120°C 鼓风干燥箱内 12h进行干燥至含水量小于 8%时, (b)匀浆法提取:
称取一定量的蚕蛹粉置于匀浆机内, 加入相应比例的提取溶剂, 蚕蛹 粉与提取溶剂的质量比为 1: 3~6, 启动匀浆机匀浆 6次, 每次 5分钟, 总共 30分钟, 转速在 6000 ~ 18000rpm/min, 收集匀浆液;
(c)制备蚕蛹油:
提取液用 4~8层纱布过滤, 收集滤液, 用离心机在 4000 ~ 8000 rpm/min 的转速下离心 10~30分钟, 收集上清液, 将上清液在减压抽滤器内于室温 下、 -0.08MPa下减压抽滤, 得到滤液, 滤液在减压蒸发器内于 60~80°C、 -0.08MPa减压蒸馏, 回收提取溶剂, 在 40~50°C的烘箱中去除残佘提取溶 剂, 得蚕蛹油;
(d)精炼蚕蛹油:
将步骤 (c)所得蚕蛹油加热到 70 °C后加入占蚕蛹油质量 0.05 % -0.12 % 的柠檬酸晶体(C6H807¾0), 经混合后, 静置 5-6分钟, 会使蚕蛹油中残 存的钙、 镁、 铁等的二价金属离子 Ca2+、 Mg2+、 Fe2+变为游离态, 移动到水 相中。 再通过 3000~4000rpm/min离心后去除掉, 从而达到脱胶的目的; 以 酸值不能高于 0.2 mgKOH/g为标准, 在综合考虑皂脚和色泽情况下, 确定 精炼蚕蛹油的超碱量为 74.4%, 此时皂角硬度合适, 油皂易于分离, 酸值以 及色泽均达到要求; 当毛油初温 45°C时; 加入质量分数为 14%的氢氧化钾 水溶液, 混合搅拌 30 ~ 40分钟并持续升温至蚕蛹油温度控制在 60 ~65°C时, 通过 3000~4000rpm/min迅速离心分离油皂, 去掉上层油脂, 用 80°C蒸馏水 以 120 rpm/min搅拌洗涤, 直至洗液的 pH值为中性, 达到脱酸的目的; 脱 酸后的蚕蛹油中加入占蚕蛹油质量 4 %的脱色白土, 蚕蛹油温度控制在 40 ~ 42 °C, 搅拌 30分钟, 过滤分离脱色白土, 得精炼蚕蛹油。
进一步地, 上述步骤 (b)中蚕蛹粉与提取溶剂的质量比为 1 : 4~6。 进一步地, 上述步骤 (b)中蚕蛹粉与提取溶剂的质量比为 1 : 4。
进一步地, 上述步骤 (b)中提取溶剂为石油醚、 乙酸乙酯或无水乙醇。 进一步地, 上述步骤 (b)中匀浆机的转速为 6000 ~ 8000rpm/min。
本发明的有益效果是: 本发明具有工艺步骤简单、 提取率高、 提取时 间短、 生产成本低等优点, 可用于从蚕蛹中制备蚕蛹油。 所制备的蚕蛹油 呈现黄色, 有油香味, 各项指标符合文献报道的蚕蛹油质量标准, 可作为 食用油, 也可作为保健食品基料。 具体实施方式
应该指出, 以下具体说明都是例示性的, 皆在对本发明提供进一步的 发明。 除非另有说明, 本文使用的所有科学和技术术语具有与本发明所属 技术领域人员通常理解的相同含义。
下面结合实施例对本发明做进一步说明。 但本发明不限于这些实施例。 实施例 1
以蚕蛹粉 100g为所用原料提取蚕蛹油为例, 其提取方法如下:
(a)蚕蛹预处理
将湿蚕蛹放入 120°C鼓风干燥箱内 12h进行干燥至含水量小于 8%时, 用
(b)匀浆法提取
称取 100g的蚕蛹粉置于匀浆机内, 加入 400g石油醚 (提取溶剂), 蚕蛹 粉与石油醚的质量比为 1: 4, 启动匀浆机匀浆 6次, 每次 5分钟, 总共 30分 钟, 转速为 8000rpm/min, 收集匀浆液。
(c)制备蚕蛹油
所得匀浆液用 4 ~ 8层纱布过滤, 收集滤液, 用离心机在 4000 ~ 8000 rpm/min的转速下离心 10 ~ 30分钟, 收集上清液, 将上清液在减压抽滤器内 于室温下、 -0.08MPa下减压抽滤, 得到滤液; 滤液在减压蒸发器内于 60 ~ 80°C、 -0.08MPa减压蒸馏, 回收提取溶剂, 在 40 ~ 50°C的烘箱中去除残佘 提取溶剂, 得蚕蛹油。
(d)精炼蚕蛹油
加热到 70°C的蚕蛹油中加入占蚕蛹油质量 0.05 %的柠檬酸晶体 ( C6H807-H20 ), 经混合后, 静置 5-6分钟, 会使蚕蛹油中残存的钙、 镁、 铁等二价的金属离子 Ca2+、 Mg2+、 Fe2+变为游离态, 移动到水相中, 再通过 3000 ~ 4000rpm/min离心后去除掉, 从而达到脱胶的目的; 以酸值不能高于 0.2 mgKOH/g为标准, 在综合考虑皂脚和色泽情况下, 确定精炼蚕蛹油的 超碱量为 74.4%, 此时皂角硬度合适, 油皂易于分离, 酸值以及色泽均达到 要求; 当毛油初温 45°C时; 加入质量分数为 14 %的氢氧化钾水溶液, 混合 搅拌 30 ~ 40分钟并持续升温至蚕蛹油温度控制在 60 ~ 65°C时, 再通过 3000 ~ 4000rpm/min趁热迅速离心分离油皂, 去掉上层油脂, 用 80°C蒸馏水 以 120 rpm/min搅拌洗涤, 直至洗液的 pH值为中性, 达到脱酸的目的; 脱 酸后的蚕蛹油中加入占蚕蛹油质量 4 %的脱色白土, 蚕蛹油温度控制在 40 ~ 42 °C , 搅拌 30分钟, 过滤分离脱色白土, 得精炼蚕蛹油。
实施例 2
以蚕蛹粉 100g为所用原料提取蚕蛹油为例, 其提取方法如下:
(a)蚕蛹预处理
将湿蚕蛹放入 120°C鼓风干燥箱内 12h进行干燥至含水量小于 8%时, 用
(b)匀浆法提取
称取 100g的蚕蛹粉置于匀浆机内, 加入 500g石油醚 (提取溶剂), 蚕蛹 粉与石油醚的质量比为 1: 5 , 启动匀浆机匀浆 6次, 每次 5分钟, 总共 30分 钟, 转速为 8000rpm/min, 收集匀浆液。 (C)制备蚕蛹油
所得匀浆液用 4 ~ 8层纱布过滤, 收集滤液, 用离心机在 4000 ~ 8000 rpm/min的转速下离心 10 ~ 30分钟, 收集上清液, 将上清液在减压抽滤器内 于室温下、 -0.08MPa下减压抽滤, 得到滤液; 滤液在减压蒸发器内于 60 ~ 80°C、 -0.08MPa减压蒸馏, 回收提取溶剂, 在 40 ~ 50°C的烘箱中去除残佘 提取溶剂, 得蚕蛹油。
(d)精炼蚕蛹油
所得蚕蛹油加热到 70°C后加入占蚕蛹油质量 0.08 %的柠檬酸晶体 ( C6H807-H20 ), 经混合后, 静置 5-6分钟, 会使蚕蛹油中残存的钙、 镁、 铁等二价的金属离子 Ca2+、 Mg2+、 Fe2+变为游离态, 移动到水相中, 再通过 3000 ~ 4000rpm/min离心后去除掉, 从而达到脱胶的目的; 以酸值不能高于 0.2 mgKOH/g为标准, 在综合考虑皂脚和色泽情况下, 确定精炼蚕蛹油的 超碱量为 74. 4%, 此时皂角硬度合适, 油皂易于分离, 酸值以及色泽均达到 要求; 当毛油初温 45°C时, 加入质量分数为 14 %的氢氧化钾水溶液, 混合 搅拌 30 ~ 40分钟并持续升温至蚕蛹油温度控制在 60 ~ 65°C时, 再通过 3000 ~ 4000rpm/min趁热迅速离心分离油皂, 去掉上层油脂, 用 80°C蒸馏水 以 120 rpm/min搅拌洗涤, 直至洗液的 pH值为中性, 达到脱酸的目的; 脱 酸后的蚕蛹油中加入占蚕蛹油质量 4 %的脱色白土, 蚕蛹油温度控制在 40 ~ 42 °C , 搅拌 30分钟, 过滤分离脱色白土, 得精炼蚕蛹油。
实施例 3
以蚕蛹粉 100g为所用原料提取蚕蛹油为例, 其提取方法如下:
(a)蚕蛹预处理
将湿蚕蛹放入 120°C鼓风干燥箱内 12h进行干燥至含水量小于 8%时, 用
(b)匀浆法提取 称取 lOOg的蚕蛹粉置于匀浆机内, 加入 600g石油醚 (提取溶剂), 蚕蛹 粉与石油醚的质量比为 1: 6, 启动匀浆机匀浆 6次, 每次 5分钟, 总共 30分 钟, 转速为 8000rpm/min, 收集匀浆液。
(c)制备蚕蛹油
所得匀浆液用 4 ~ 8层纱布过滤, 收集滤液, 用离心机在 4000 ~ 8000 rpm/min的转速下离心 10 ~ 30分钟, 收集上清液, 将上清液在减压抽滤器内 于室温下、 -0.08MPa下减压抽滤, 得到滤液; 滤液在减压蒸发器内于 60 ~ 80°C、 -0.08MPa减压蒸馏, 回收提取溶剂, 在 40 ~ 50°C的烘箱中去除残佘 提取溶剂, 得蚕蛹油。
(d)精炼蚕蛹油
所得蚕蛹油加热到 70°C后加入占蚕蛹油质量 0.12 %的柠檬酸晶体 ( C6H807-H20 ), 经混合后, 静置 5-6分钟, 会使蚕蛹油中残存的钙、 镁、 铁等二价的金属离子 Ca2+、 Mg2+、 Fe2+变为游离态, 移动到水相中, 再通过 3000 ~ 4000rpm/min离心后去除掉, 从而达到脱胶的目的; 以酸值不能高于 0.2 mgKOH/g为标准, 在综合考虑皂脚和色泽情况下, 确定精炼蚕蛹油的 超碱量为 74.4%, 此时皂角硬度合适, 油皂易于分离, 酸值以及色泽均达到 要求; 当毛油初温 45 °C时; 加入质量分数为 14 %的氢氧化钾水溶液, 混合 搅拌 30 ~ 40分钟并持续升温至蚕蛹油温度控制在 60 ~ 65 °C时, 通过 3000 ~ 4000rpm/min趁热迅速离心分离油皂, 去掉上层油脂, 用 80°C蒸馏水以 120 rpm/min搅拌洗涤, 直至洗液的 pH值为中性, 达到脱酸的目的; 脱酸后的 蚕蛹油中加入占蚕蛹油质量 4 %的脱色白土, 蚕蛹油温度控制在 40 ~ 42 °C , 搅拌 30分钟, 过滤分离脱色白土, 得精炼蚕蛹油。
实施例 4
以蚕蛹粉 100g为所用原料提取蚕蛹油为例, 其提取方法如下: 在以上的实施例 1 ~ 3的匀浆法提取步骤 (b)中, 称取蚕蛹粉 100g置于匀 浆机内, 加入的石油醚 (提取溶剂)用乙酸乙酯替换, 所加入的量应与相应的 实施例相同, 其他步骤也应与相应的实施例相同, 制备成精炼蚕蛹油。
实施例 5
以蚕蛹粉 100g为所用原料提取蚕蛹油为例, 其提取方法如下: 在以上的实施例 1 ~ 3的匀浆法提取步骤 (b)中, 称取蚕蛹粉 100g置于匀 浆机内, 加入的石油醚 (提取溶剂)用无水乙醇替换, 所加入的量应与相应的 实施例相同, 其他步骤也应与相应的实施例相同, 制备成精炼蚕蛹油。
实施例 6
以蚕蛹粉 100g为所用原料提取蚕蛹油为例, 其提取方法如下: 在以上的实施例 1 ~ 6的匀浆法提取步骤 (b)中, 称取蚕蛹粉 100g置于匀 浆机内, 所加入的提取溶剂和所加入的量应与相应的实施例相同, 匀浆机 的转速为 lOOOOrpm/min, 收集匀浆液。 其他步骤应与相应的实施例相同, 制备成精炼蚕蛹油。
实施例 7
以蚕蛹粉 100g为所用原料提取蚕蛹油为例, 其提取方法如下: 在以上的实施例 1 ~ 6的匀浆法提取步骤 (b)中, 称取蚕蛹粉 100g置于匀 浆机内, 所加入的提取溶剂和所加入的量应与相应的实施例相同, 匀浆机 的转速为 6000rpm/min, 收集匀浆液。 其他步骤应与相应的实施例相同, 制 备成精炼蚕蛹油。
为了确定本发明所用原料的最佳配比和工艺步骤, 发明人进行了大量 的实验室研究试验, 每种试验重复三次, 实验结果为三次重复试验的平均 值, 各种试验情况如下:
材料: 蚕蛹: 由浙江中奇生物医药股份有限公司提供。
试剂: 石油醚、 冰乙酸等色谱用试剂为色谱纯, 其他试剂均为分析纯, 且所有试剂均为巿售。 实验仪器: 气相色谱仪, 曰本岛津生产; 1 W400A型高速万能粉碎机, 北京科伟永兴仪器有限公司生产; Thermo-RC 6+型离心机; 上海医用仪器 分析厂生产; 可调高速匀浆机, 上海尤释机电设备发展有限公司; RE-2000 型旋转蒸发仪,上海亚荣生化仪器厂生产; GZX-9146MB :数显鼓风干燥箱,
称取粉碎过的蚕蛹粉 3份, 每份为 100g, 分别置于匀浆机内, 称取提取 溶剂石油醚、 乙酸乙酯、 无水乙醇各 400g加入到匀浆机里, 启动匀浆机用 转速为 8000rpm/min处理 6次, 每次 5分钟, 总共 30分钟, 收集匀浆液, 用 4 ~ 8层纱布过滤, 收集滤液, 用离心机 4000 ~ 8000rpm/min 的转速下离心 10 ~ 30分钟, 收集上清液, 将上清液在减压抽滤器内于室温下、 -0.08MPa 下减 压抽滤, 得到滤液; 滤液在减压蒸发器内于 60 ~ 80°C、 -0.08MPa减压蒸馏, 回收提取溶剂, 在 40 ~ 50°C的烘箱中去除残余提取溶剂, 得蚕蛹油。 蚕蛹 油得率的计算公式如下:
) 蚕蛹粉的质量 (g)
Figure imgf000010_0001
实验和计算结果见表 1。
表 1 不同溶剂对出油率及油品质的影响
Figure imgf000010_0002
由表 1可见, 乙酸乙酯提取的出油率最高, 但得到的蚕蛹油颜色深不透 明, 蚕蛹油的腥臭味较重。 表明乙酸乙酯极性大, 除浸提出油脂物质外还 提出了非脂类的物质。 而石油醚提出的蛹油澄清透明, 呈淡黄色, 气味最 油醚作为提取溶剂。
替换页 (细则第 26条) 2、 蚕蛹粉与提取溶剂的质量比对蚕蛹油得率的影响
准确称取粉碎过的蚕蛹粉 5份, 每份为 100g, 分别置于匀浆机内, 称取 提取溶剂石油醚 200g、 300g、 400g、 500g、 600g分别加入到相应的匀浆机 内, 启动匀浆机用转速为 8000rpm/min处理 6次, 每次 5分钟, 总共 30分钟, 收集匀浆液, 用 4 ~ 8层纱布过滤, 收集滤液, 用离心机 4000~8000rpm/min 的转速下离心 10~30分钟, 收集上清液, 将上清液在减压抽滤器内于室温 下、 -0.08MPa下减压抽滤, 得到滤液; 滤液在减压蒸发器内于 60~80°C、 -0.08MPa减压蒸馏, 回收提取溶剂, 在 40~50°C的烘箱中去除残佘提取溶 表 2 蚕蛹粉与提取溶剂的质量比对蚕蛹油得率的影响
Figure imgf000011_0001
由表 2可见, 随着蚕蛹粉与提取溶剂的质量比的提高, 蚕蛹油得率也提 高, 当质量比大于 1 : 4后, 蚕蛹油得率增加缓慢, 考虑到成本及各种因素, 本发明选择蚕蛹粉与提取溶剂的质量比 1 : 4~6, 最佳质量为 1 : 4。
3、 匀浆机转速对蚕蛹油得率的影响
称取粉碎过的蚕蛹粉 6份, 每份为 100g, 分别置于匀浆机内, 称取提取溶剂 石油醚 6份, 每份为 400g, 分别加入到相应的匀浆机内, 启动匀浆机用转速 为 8000rpm/min 处理 6次, 每次 5分钟, 总共 30分钟, 收集匀浆液, 用 4~8 层纱布过滤, 收集滤液, 用离心机在 4000~8000rpm/min的转速下离心 10~ 30分钟, 收集上清液, 将上清液在减压抽滤器内于室温下、 -0.08MPa下减 压抽滤, 得到滤液; 滤液在减压蒸发器内于 60~80°C、 -0.08MPa减压蒸馏, 回收提取溶剂, 在 40 ~50°C的烘箱中去除残佘提取溶剂, 得蚕蛹油。 按公 表 3 匀浆转速对蚕蛹油得率的影响
Figure imgf000012_0001
由表 3可见, 当匀浆转速由 6000rpm/min增加到 8000rpm/min时,蚕蛹油 提取率增加显著, 当转速由 8000rpm/min增加到 12000rpm/min时,蚕蛹油提 取率增加不显著, 当转速由 12000rpm/min增加到 16000rpm/min时, 提取率 反而降低, 这可能是由于匀浆转速过大会造成溶剂的损失, 综合考虑可以 把 8000rpm/min作为最佳的匀浆转速。
4、 匀浆时间对蚕蛹油得率的影响
称取粉碎过的蚕蛹粉 4份, 每份为 100g, 分别置于匀浆机内, 称取提取 溶剂石油醚 4份, 每份为 400g, 分别加入到相应的匀浆机内, 启动匀浆机用 转速为 8000rpm/min处理 2次, 4次, 6次, 8次, 每次 5分钟, 总共各自为 10 分钟, 20分钟, 30分钟, 40分钟, 收集匀浆液, 用 4 ~ 8层纱布过滤, 收集 滤液, 用离心机 4000 ~ 8000转 /分钟离心 10 ~ 30分钟, 收集上清液, 将上清 液在减压抽滤器内于室温下、 -0.08MPa下减压抽滤, 得到滤液; 滤液在减 压蒸发器内于 60 ~ 80°C、 -0.08MPa减压蒸馏, 回收提取溶剂, 在 40 ~ 50°C 的烘箱中去除残佘提取溶剂, 得蚕蛹油。 按公式 (1)计算蚕蛹油的得率, 其 结果见表 4。
表 4 匀浆处理时间对蚕蛹油得率的影响
Figure imgf000012_0002
由表 4可见, 随着匀浆时间的增加, 蚕蛹油提取率也增加, 当匀浆处理 30 ~ 40分钟, 蚕蛹油的得率较高, 而匀浆处理 30分钟时, 蚕蛹油的得率最 高。 本发明选择匀浆处理时间为 30 ~ 40分钟, 最佳为 30分钟。
5、 匀浆法与溶剂浸提法两种方法提取蚕蛹油的提取率与得率的比较
为了验证本发明提取蚕蛹油的可靠性, 实验釆用了上述优化条件进行 了三次重复, 即提取溶剂为石油醚, 蚕蛹粉与提取溶剂的质量比为 1 :4, 匀 浆转速为 8000rpm/min、 匀浆处理时间为 30分钟。 其蚕蛹油的得率按公式(1) 计算, 提取率的计算公式如下: 得率 (%) xlOO
吞 i:粉 ® ί % ) 实验和计算结果见表 5。
表 5 溶剂浸提法与匀浆法提取蚕蛹油的比较
Figure imgf000013_0001
由表 5可见,本发明与溶剂浸提法相比,本发明提取蚕蛹油的得率由 24.1 %提高到 26.9 % ,提取率由 80.3 %提高到 89.7 % , 而提取时间由 2小时缩短到 30分钟。
为了验证本发明的有益效果, 因此对本发明提供的方法制备的蚕蛹油进 行了测试, 其测试如下:
1)感官检验
色泽: 淡黄色。
气味: 正常无异味。
外观: 均匀、 无异物及沉淀物。
2)匀浆法制备的蚕蛹油理化指标
参照 GB/T 5009.37— 2003 《食用植物油卫生标准的分析方法》, GB/T 5534— 1995《动植物油脂皂化值的测定》, GB/T 5530-2005《动植物油脂 酸 值和酸度测定》、 GB/T 5532-2008《动植物油脂碘值的测定》、 GB/T5527-1985 《植物油脂检验折光指数测定法》、 GB5526-1985《植物油脂检验比重测定 法》、 进行了蚕蛹油理化指标分析, 其测定结果见表 6。 表 6 蚕蛹油质量与菜籽油国家标准比较
Figure imgf000014_0002
由表 6可见, 釆用本发明制备的蚕蛹油与文献报道的蚕蛹油标准的各项 质量指标接近。
Figure imgf000014_0001
釆用本发明制备的蚕蛹油用 GC-MS对脂肪酸组成进行了分析。
色谱条件: VF-1701ms(30m*0.25mm*0.25um); 载气: 高纯氦气; 流速: l.OmL/min; 进样口温度: 250度; 分流比为 20: 1 ; 进样量: lul; 柱温: 80度 保持 5分钟, 30度每分钟升温到 200度,保持 1分钟, 3度每分钟升温到 230度, 保持 10min。
质谱条件: EI 源: 70ev; 离子源温度 250度, 传输线温度: 260度; 四 级杆温度: 40度; 扫描范围: 35-500;
试验结果见表 7。
表 7 蚕蛹油脂肪酸组成
Figure imgf000014_0003
由表 7可见, 不饱和脂肪酸相对含量为 75.34 % , 可见蚕蛹油含有大量多 不饱和脂肪酸, 营养价值丰富。
由以上试验研究表明, 本发明与现有蚕蛹油提取方法相比, 蚕蛹油提 取率明显提高, 提取时间大大缩短, 工艺过程简单、 稳定, 适于工业化生 产。 釆用本发明所提取蚕蛹油产品呈现黄色, 具有蚕蛹油特有油香味, 由 于蚕蛹油目前无国家质量标准, 与菜籽油等食用油对比, 各项指标符合
GB1536-2004《菜籽油》质量标准, 脂肪酸组成分析显示富含多不饱和脂肪 酸, 尤其是 α-亚麻酸含量丰富, 是一种具有较高营养价值的营养保健油脂。
以上所述, 仅为本发明的实施例, 应当指出, 对于本技术中的普通技 术人员来说, 在不脱离本发明的核心技术特征的前提下, 还可以做若干的 改进和润饰, 这些润饰和改进也应属于本发明的专利保护范围。

Claims

权利要求书
1.一种提取蚕蛹油的方法, 其特征在于, 所述方法包括以下步骤:
(a)蚕蛹预处理;
(b)匀浆法提取;
(c)制备蚕蛹油;
(d)精炼蚕蛹油。
2.如权利要求 1所述的方法,其特征在于,步骤 (a)中所述蚕蛹预处理为: 将湿蚕蛹放入 120°C鼓风干燥箱内 12h进行干燥至含水量小于 8%时,用粉
3.如权利要求 1 所述的方法, 其特征在于, 步骤 (b)中所述匀浆法提取 为: 将蚕蛹粉置于匀浆机内, 加入提取溶剂, 其中蚕蛹粉与提取溶剂的质 量比为 1: 3 ~ 6, 启动匀浆机, 在 6000 ~ 18000rpm/min的转速下匀浆 6次, 每次 5分钟, 总共 30分钟, 收集匀浆液。
4. 如权利要求 3所述的方法, 其特征在于, 步骤 (b)中所述蚕蛹粉与提 取溶剂的质量比为 1: 4 ~ 6。
5. 如权利要求 3所述的方法, 其特征在于, 步骤 (b)中所述蚕蛹粉与提 取溶剂的质量比为 1: 4。
6. 如权利要求 3至 5任一所述的方法, 其特征在于, 步骤 (b)中所述提 取溶剂为石油醚、 乙酸乙酯或无水乙醇。
7. 如权利要求 3至 5任一所述的方法, 其特征在于, 步骤 (b)中所述匀 浆机的转速为 6000 ~ 8000rpm/min。
8.如权利要求 1所述的方法,其特征在于,步骤 (c)中所述制备蚕蛹油具 体包括: 将步骤 (b)所得匀浆液用 4 ~ 8层纱布过滤, 收集滤液, 在 4000 ~ 8000rpm/min的转速下离心 10 ~ 30分钟, 收集上清液, 将上清液在减压抽 滤器内于室温下、 -0.08MPa下减压抽滤,滤液在减压蒸发器内于 60 ~ 80°C、 -0.08MPa减压蒸馏, 回收提取溶剂, 在 40~50°C的烘箱中去除残佘提取溶 剂, 得蚕蛹油。
9.如权利要求 1 所述的方法, 其特征在于, 步骤 (d)中所述精炼蚕蛹油 具体包括:
2)蚕蛹油的脱酸;
3)蚕蛹油的精炼。
10.如权利要求 9所述的方法, 其特征在于,
步骤 1)中所述蚕蛹油的脱胶为: 将步骤 (c)所得蚕蛹油加热到 70°C后加 入占蚕蛹油质量 0.05% ~0.12%的柠檬酸晶体 C6H807H20, 经混合后, 静 置 5-6分钟, 再通过 3000~4000rpm/min离心, 从而达到脱胶的目的;
步骤 2)中所述蚕蛹油的脱酸为:以酸值不能高于 0.2 mgKOH/g为标准 , 在综合考虑皂脚和色泽情况下,确定精炼蚕蛹油的超碱量为 74.4%, 当毛油 初温为 45°C时; 加入质量分数为 14%的氢氧化钾水溶液, 混合搅拌 30~40 分钟并持续升温至蚕蛹油温度控制在 60 ~ 65°C时,通过 3000 ~ 4000rpm/min 迅速离心分离油皂, 去掉上层油脂, 用 80°C蒸馏水以 120 rpm/min搅拌洗 涤, 直至洗液的 pH值为中性, 从而达到脱酸的目的;
步骤 2)中所述蚕蛹油的精炼为:脱酸后的蚕蛹油中加入占蚕蛹油质量 4 %的脱色白土, 蚕蛹油温度控制在 40~42°C, 搅拌 30分钟, 过滤分离脱色 白土, 得精炼蚕蛹油。
PCT/CN2013/077521 2012-11-09 2013-06-20 一种提取蚕蛹油的方法 WO2014071736A1 (zh)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN2012104463041A CN102965189A (zh) 2012-11-09 2012-11-09 一种提取蚕蛹油的方法
CN201210446304.1 2012-11-09

Publications (1)

Publication Number Publication Date
WO2014071736A1 true WO2014071736A1 (zh) 2014-05-15

Family

ID=47795625

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2013/077521 WO2014071736A1 (zh) 2012-11-09 2013-06-20 一种提取蚕蛹油的方法

Country Status (2)

Country Link
CN (1) CN102965189A (zh)
WO (1) WO2014071736A1 (zh)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106974253A (zh) * 2017-05-04 2017-07-25 广西壮族自治区蚕业技术推广总站 一种蚕蛹综合利用的方法
CN107699359A (zh) * 2017-11-24 2018-02-16 黑龙江美丽石岛科技开发有限公司 一种海参肠卵油的提取工艺及利用海参肠卵油制备海参肠卵油软胶囊的方法

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104178333A (zh) * 2013-05-22 2014-12-03 武汉蜀泰科技有限公司 一种复合酶法处理大麦虫提取生物油脂的方法
CN104250582B (zh) * 2014-09-04 2017-12-26 湖南省中医药研究院中药研究所 一种从蚕蛹下脚料中提取无臭白色蚕蛹油的方法
CN105754716B (zh) * 2016-02-25 2020-02-07 湖南科技学院 一种低温提取蛇油以及对蛇油进行去腥、脱色的方法
CN105995886A (zh) * 2016-05-24 2016-10-12 广东汇香源生物科技股份有限公司 一种蚕蛹风味膏及其制备方法与应用
CN106675773A (zh) * 2016-12-28 2017-05-17 武汉工程大学 一种常温匀浆原位提取能源昆虫油脂的方法
CN106644651A (zh) * 2017-01-25 2017-05-10 湖州出入境检验检疫局综合技术服务中心 一种测定冻蚕蛹酸价和过氧化值的样品前处理方法
CN108641816A (zh) * 2018-05-09 2018-10-12 大连理工大学 一种提取米糠油的方法
CN109233994A (zh) * 2018-10-16 2019-01-18 山东省蚕业研究所 一种柞蚕蛾油的提取方法
CN110484357A (zh) * 2019-08-22 2019-11-22 浙江省农业科学院 一种冷榨鲜蚕蛹油的生产方法
CN110655972A (zh) * 2019-09-11 2020-01-07 苏州嘉缌韵生物科技有限公司 一种食用级蚕蛹油的生产工艺
CN112920895A (zh) * 2021-02-08 2021-06-08 辽宁大学 一种超声辅助萃取蚕蛹油的生产工艺

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101781601A (zh) * 2010-02-24 2010-07-21 陕西师范大学 用超声波从蚕蛹中提取蚕蛹油的方法

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2517964B1 (fr) * 1981-12-10 1985-08-30 Moreau Lavaud Reine Nouveau procede de preparation d'huile de chrysalide
CN101100627A (zh) * 2007-07-13 2008-01-09 江苏科技大学 一种蚕蛹油的萃取方法
CN101463289A (zh) * 2009-01-16 2009-06-24 戴永昌 一种萃取蚕蛹油的生产工艺

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101781601A (zh) * 2010-02-24 2010-07-21 陕西师范大学 用超声波从蚕蛹中提取蚕蛹油的方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
LIU, GUO ET AL.: "Can2 yong3 zi1 yuan2 kai1 fal del yan2 jiu1 jin4 zhan3.", FEED INDUSTRY., vol. 33, no. 8, August 2012 (2012-08-01), pages 40 - 42 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106974253A (zh) * 2017-05-04 2017-07-25 广西壮族自治区蚕业技术推广总站 一种蚕蛹综合利用的方法
CN107699359A (zh) * 2017-11-24 2018-02-16 黑龙江美丽石岛科技开发有限公司 一种海参肠卵油的提取工艺及利用海参肠卵油制备海参肠卵油软胶囊的方法

Also Published As

Publication number Publication date
CN102965189A (zh) 2013-03-13

Similar Documents

Publication Publication Date Title
WO2014071736A1 (zh) 一种提取蚕蛹油的方法
CN104711118B (zh) 一种降低反式脂肪酸的方法
CN103859067B (zh) 一种营养稻米油及其生产方法
TW201032724A (en) Palm oil, deodorized distillates and manufacturing methods therefor
CN105331438B (zh) 一种半固态水酶法制备菜籽油的方法
CN103666750A (zh) 一种牡丹籽油的精炼方法及制皂工艺
CN104212629A (zh) 盐水润湿冷榨提取亚麻油的方法
CN111000760A (zh) 一种利用牡丹花精油和籽油制备化妆品基础油的方法
CN103013653B (zh) 一种精制蛋黄油的制备方法
CN101519626A (zh) 蚕蛹毛油提取α-亚麻酸的工艺
CN107586593A (zh) 一种从牡丹籽中提取牡丹籽精油的方法
WO2015021631A1 (zh) 一种黄芪籽粗油、精制油及制备方法与应用
CN103467432B (zh) 一种从毛叶山桐子油脱臭馏出物中提取维生素e的方法
JP2014518926A (ja) オイルケーキに対する直接的な反応性粉砕プロセス
CN107954969B (zh) 高质量维生素e的提取工艺
CN104862068A (zh) 一种压榨法制备大豆油的工艺
CN109666533A (zh) 精制马油及其精炼提取方法和应用
Srivastava et al. Hypocholesterimic effects of cold and hot extracted virgin coconut oil (VCO) in comparison to commercial coconut oil: evidence from a male wistar albino rat model
CN109438227A (zh) 一种ω-3多烯脂肪酸乙酯的生产方法
CN108085132A (zh) 一种薏苡仁油精炼工艺
CN102199487A (zh) 生产原生态冷榨栝楼籽油的方法
CN108283221A (zh) 一种富含dha的油茶籽滋养调味油及其制备方法
BR112019012765A2 (pt) óleo de palma com teor reduzido de hidrocarbonetos saturados
CN105154223A (zh) 一种米糠油
CN109536270A (zh) 藜麦麸皮中油脂的提取方法及其在食品方面的应用

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 13853890

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 13853890

Country of ref document: EP

Kind code of ref document: A1