CN102776063A - Method for extracting natural shrimp sauce from procambarus clarkii wastes - Google Patents
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- 241000238557 Decapoda Species 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000002699 waste material Substances 0.000 title claims abstract description 18
- 241000238030 Procambarus clarkii Species 0.000 title abstract description 13
- 235000015067 sauces Nutrition 0.000 title 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000605 extraction Methods 0.000 claims abstract description 24
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- 238000003756 stirring Methods 0.000 claims description 9
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Abstract
本发明公开了一种从克氏原鳌虾废弃物中提取天然虾油的方法，该方法主要步骤为：龙虾下脚料预处理；利用乙醇作为有机溶剂震荡提取；离心分离；回收有机溶剂；脱胶、脱酸、脱色、水洗以及干燥。本发明利用乙醇作为提取剂，进行振荡提取，对克氏原螯虾废弃物中的天然虾油进行有效提取，通过本方法，可获得11.04％的虾油，该虾油透明澄清、呈现出虾青素体现的浅酒红色、具有龙虾所特有香味，营养价值丰富，不饱和脂肪酸含量达到总脂肪酸的47.98％、顺式脂肪酸含量占不饱和脂肪酸含量的95.65％以及EPA和DHA含量占多不饱和脂肪酸含量的7.15％，同时乙醇作为有机溶剂提取安全可靠。如能工厂化，不但可以减少资源浪费，还可以减少环境污染，提高企业的经济效益。
The invention discloses a method for extracting natural shrimp oil from crayfish waste. The main steps of the method are: pretreatment of lobster leftovers; vibration extraction using ethanol as an organic solvent; centrifugal separation; recovery of organic solvent; degumming, Deacidification, decolorization, washing and drying. In the present invention, ethanol is used as an extractant to vibrate and extract the natural shrimp oil in the waste of Procambarus clarkii. By this method, 11.04% of the shrimp oil can be obtained, and the shrimp oil is transparent and clarified, showing shrimp green The light burgundy color reflected by the element, has the unique fragrance of lobster, and is rich in nutritional value. The content of unsaturated fatty acids reaches 47.98% of the total fatty acids, the content of cis fatty acids accounts for 95.65% of the content of unsaturated fatty acids, and the content of EPA and DHA accounts for 95.65% of the content of polyunsaturated fatty acids. content of 7.15%, and ethanol is safe and reliable as an organic solvent for extraction. If it can be factoryized, it can not only reduce the waste of resources, but also reduce environmental pollution and improve the economic benefits of enterprises.
Description
技术领域 technical field
本发明属于水产品加工技术领域，尤其涉及一种从克氏原鳌虾废弃物中提取天然虾油的方法。The invention belongs to the technical field of aquatic product processing, and in particular relates to a method for extracting natural shrimp oil from the waste of Procambarus clarkii.
背景技术 Background technique
克氏原螯虾(Procambarus clarkia)又称小龙虾，是淡水螯虾的一种，英文名Red Swamp Crayfish。克氏原螯虾是一种珍贵的水产经济动物，具有丰富的营养价值和保健功能，是一种真正的高蛋白、低脂肪、低胆固醇产品，其富含微量元素和维生素。克氏原螯虾肉味鲜美，风味独特，鲜味浓郁。克氏原螯虾出肉率在15％左右，因此有约85％的废弃物，如不加以利用，不但浪费资源，而且会造成环境污染。根据目前的市场来看，从龙虾下脚料中提取甲壳素、壳聚糖等已形成产业化，而且带来了很高的效益，但从国内外资料查阅，少见有从中提取天然虾油的研究。对于水产品油脂的提取从南极磷虾、中国对虾较多，很少从小龙虾下脚料中提取。Procambarus clarkia (Procambarus clarkia), also known as crayfish, is a kind of freshwater crayfish, and its English name is Red Swamp Crayfish. Procambarus clarkii is a precious aquatic economic animal with rich nutritional value and health care function. It is a real high-protein, low-fat, low-cholesterol product, which is rich in trace elements and vitamins. Procambarus clarkii has delicious meat, unique flavor and strong umami. The meat yield of Procambarus clarkii is about 15%, so there are about 85% of waste, if not utilized, it will not only waste resources, but also cause environmental pollution. According to the current market, the extraction of chitin and chitosan from lobster scraps has been industrialized and has brought high benefits. However, according to domestic and foreign data, there are few studies on extracting natural shrimp oil from them. . For the extraction of aquatic product oil, it is mostly extracted from Antarctic krill and Chinese prawn, and rarely extracted from crayfish leftovers.
目前，小龙虾出口很大一部分是以虾仁的形式，因此会产生大量的废弃物，目前的对克氏原螯虾废弃物中天然虾油的提取很少。对油脂的提取现在通常采用相似相溶原理，有机溶剂主要有四种，酯、酮、醚、醇。极性从小到大排列是：烷、烯、醚、酯、酮、醛、胺、醇和酚、酸。从对人体健康上来说：苯类毒性太大；烷烃类腐蚀性强；酮类对人的呼吸道有影响；酯类有强烈的脂溶性，会被皮肤毛细孔吸收，进入微细血管，影响肝脏功能，甲醇对眼睛有影响。所以本方法采用乙醇作为提取剂，从极性和毒性上都具有一定的优势，而其容易获得，价格相对较便宜。并且选用乙醇作为提取剂的另一个理由是虾油也是极性油脂，利用极性乙醇，同为极性的复合更好，溶解性也更好，所以使用极性溶剂，希望达到较高的提取率。并且此方法也是最便捷，经济(有机溶剂可回收利用)，可工厂化利用的油脂提取方法。At present, a large part of the crayfish export is in the form of shelled shrimp, so a large amount of waste will be generated, and the natural shrimp oil in the current Procambarus clarkii waste is rarely extracted. The extraction of oils and fats is now usually based on the principle of similar miscibility. There are mainly four types of organic solvents, esters, ketones, ethers, and alcohols. The order of polarity from small to large is: alkanes, alkenes, ethers, esters, ketones, aldehydes, amines, alcohols and phenols, acids. From the perspective of human health: benzene is too toxic; alkanes are highly corrosive; ketones have an impact on the human respiratory tract; esters are strongly fat-soluble and will be absorbed by skin pores and enter tiny blood vessels, affecting liver function , Methanol is harmful to the eyes. Therefore, this method uses ethanol as the extractant, which has certain advantages in terms of polarity and toxicity, and it is easy to obtain and relatively cheap. And another reason for choosing ethanol as the extractant is that shrimp oil is also a polar oil. Using polar ethanol, the compound of the same polarity is better and the solubility is better, so using a polar solvent hopes to achieve a higher extraction. Rate. And this method is also the most convenient, economical (the organic solvent can be recycled), and the oil extraction method that can be industrially utilized.
发明内容 Contents of the invention
本发明提供了一种采用低毒性有机溶剂(乙醇)振荡浸提法提取克氏原螯虾废弃物中的天然虾油的方法。The invention provides a method for extracting natural shrimp oil in Procambarus clarkii waste by adopting a low-toxicity organic solvent (ethanol) shaking extraction method.
本发明实施例是这样实现的，一种从克氏原鳌虾废弃物中提取天然虾油的方法，该方法主要步骤为：The embodiment of the present invention is achieved in this way, a method for extracting natural shrimp oil from the waste of Crayfish clarkii, the main steps of the method are:
龙虾下脚料预处理；利用乙醇作为有机溶剂震荡提取；离心分离；回收有机溶剂；脱胶、脱酸、脱色、水洗以及干燥。Lobster leftovers are pretreated; ethanol is used as an organic solvent for vibration extraction; centrifugation; organic solvent recovery; degumming, deacidification, decolorization, washing and drying.
进一步，龙虾下脚料预处理的处理方法为：Further, the processing method for the pretreatment of lobster scraps is:
水煮后，剔除肉，收集所有下脚料，在鼓风干燥箱中干燥，条件40～60℃，10h左右，使龙虾的含水量保持在20％左右，利用多功能粉碎机粉碎40目，备用。After boiling, remove the meat, collect all leftovers, and dry in a blast drying oven at 40-60°C for about 10 hours to keep the water content of the lobster at about 20%. Use a multi-functional pulverizer to crush 40 meshes and set aside .
进一步，利用乙醇作为有机溶剂震荡提取方法为：Further, utilizing ethanol as the organic solvent vibration extraction method is:
将1∶5～1∶7(g∶ml)虾粉和70％～90％的乙醇装入样品瓶，密封，放入台式恒温震荡箱中，30～60℃，转速100rpm/min，浸提1～2h，浸提2次，此时提取率可达到11.04％。Put 1:5～1:7 (g:ml) shrimp powder and 70%～90% ethanol into the sample bottle, seal it, put it into a desktop constant temperature shaking box, 30～60°C, rotating speed 100rpm/min, extract 1 to 2 hours, leaching twice, and the extraction rate can reach 11.04%.
进一步，离心分离的方法为：Further, the method of centrifugal separation is:
将浸提液转移到离心管中，在5000rpm下离心10min，取上清液为粗虾油。The extract was transferred to a centrifuge tube, centrifuged at 5000rpm for 10min, and the supernatant was taken as crude shrimp oil.
进一步，回收有机溶剂的方法为：Further, the method of reclaiming organic solvent is:
将粗虾油在旋转蒸发仪上进行回收有机溶剂，温度为50℃，真空度为-0.1Mpa。The crude shrimp oil is recovered the organic solvent on a rotary evaporator, the temperature is 50°C, and the vacuum degree is -0.1Mpa.
进一步，脱胶的方法为：Further, the method of degumming is:
称取一定质量的粗虾油，用水浴锅加热至50～70℃，按质量比磷酸∶油加入0.1～0.3％浓度为85％的磷酸，加热搅拌30min，静置冷却。将虾油转移到离心管中，5000rpm/min离心10min，转移上层油层。Weigh a certain quality of crude shrimp oil, heat it to 50-70°C with a water bath, add 0.1-0.3% phosphoric acid with a concentration of 85% according to the mass ratio of phosphoric acid: oil, heat and stir for 30 minutes, and let it stand for cooling. Transfer the shrimp oil to a centrifuge tube, centrifuge at 5000rpm/min for 10min, and transfer the upper oil layer.
进一步，脱酸的方法为：Further, the method of deacidification is:
称取一定质量的脱胶得到的虾油，用水浴锅加热至40～60℃，按质量比NaOH∶油加入0.2～0.4％浓度为15％～20％的NaOH，加热搅拌30min，静置冷却；将虾油转移到离心管中，5000rpm/min离心10min，转移上层油层。Weigh a certain amount of degummed shrimp oil, heat it to 40-60°C with a water bath, add 0.2-0.4% NaOH with a concentration of 15%-20% according to the mass ratio NaOH:oil, heat and stir for 30 minutes, and let it stand for cooling; Transfer the shrimp oil to a centrifuge tube, centrifuge at 5000rpm/min for 10min, and transfer the upper oil layer.
进一步，脱色的方法为：Further, the method of decolorization is:
称取一定质量的脱酸得到的虾油，用水浴锅加热至60～80℃，按质量比凹土∶油加入1～3％的凹土，加热搅拌15min，静置冷却。将虾油转移到离心管中，5000rpm/min离心10min，转移上层油层。Weigh a certain amount of deacidified shrimp oil, heat it to 60-80°C in a water bath, add 1-3% attapulgite according to the mass ratio of attapulgite: oil, heat and stir for 15 minutes, and let stand to cool. Transfer the shrimp oil to a centrifuge tube, centrifuge at 5000rpm/min for 10min, and transfer the upper oil layer.
进一步，水洗，干燥的方法为：将经过脱胶，脱酸，脱色的虾油，放入10～20％的水，5000rpm/min离心10min，分离；重复2次。最后置于冷冻干燥箱中-40℃，-0.05～-0.1MPa干燥12h得精制虾油。Further, the method of washing and drying is as follows: put the degummed, deacidified and decolored shrimp oil into 10-20% water, centrifuge at 5000rpm/min for 10min, and separate; repeat twice. Finally, place it in a freeze-drying oven at -40°C and dry at -0.05 to -0.1 MPa for 12 hours to obtain refined shrimp oil.
本发明利用乙醇作为提取剂，进行振荡提取，对克氏原螯虾废弃物中的天然虾油进行有效提取，通过本方法，可获得11.04％的虾油，该虾油透明澄清、呈现出虾青素体现的浅酒红色、具有龙虾所特有香味，营养价值丰富，不饱和脂肪酸含量达到总脂肪酸的47.98％、顺式脂肪酸含量占不饱和脂肪酸含量的95.65％以及EPA和DHA含量占多不饱和脂肪酸含量的7.15％，同时乙醇作为有机溶剂提取安全可靠。如能工厂化，不但可以减少资源浪费，还可以减少环境污染，提高企业的经济效益。The present invention uses ethanol as the extractant to carry out vibratory extraction to effectively extract the natural shrimp oil in the waste of Procambarus clarkii. Through this method, 11.04% of the shrimp oil can be obtained, and the shrimp oil is transparent and clear, showing shrimp green The light burgundy color reflected by the element, has the unique fragrance of lobster, and is rich in nutritional value. The content of unsaturated fatty acids reaches 47.98% of the total fatty acids, the content of cis fatty acids accounts for 95.65% of the content of unsaturated fatty acids, and the content of EPA and DHA accounts for 95.65% of the content of polyunsaturated fatty acids. content of 7.15%, and ethanol is safe and reliable as an organic solvent for extraction. If it can be factoryized, it can not only reduce the waste of resources, but also reduce environmental pollution and improve the economic benefits of enterprises.
附图说明 Description of drawings
图1是本发明实施例提供的从克氏原鳌虾废弃物中提取天然虾油的方法的实现流程图。Fig. 1 is the implementation flowchart of the method for extracting natural shrimp oil from the waste of Crayfish clarkii provided by the embodiment of the present invention.
具体实施方式 Detailed ways
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。In order to make the object, technical solution and advantages of the present invention clearer, the present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described here are only used to explain the present invention, not to limit the present invention.
图1示出了本发明实施例提供的从克氏原鳌虾废弃物中提取天然虾油的方法的实现流程。Fig. 1 shows the implementation process of the method for extracting natural shrimp oil from the waste of Crayfish clarkii provided by the embodiment of the present invention.
龙虾下脚料预处理：水煮后，剔除肉，收集所有下脚料，在鼓风干燥箱中干燥。条件40～60℃，10h左右(温度过高会导致龙虾头中油脂的快速氧化，干燥时间过长，同样会导致油脂的长时间氧化，同时会影响生产效率)，使龙虾的含水量保持在20％左右(因为水分含量低时，提取速率反而不高；水分含量太高时，提取过程中龙虾头粉末容易与提取溶剂形成粘稠状混合物，影响溶剂与龙虾头粉末的分离，而且部分极性油脂提取不完全)，利用多功能粉碎机粉碎40目，备用。Pretreatment of lobster scraps: After boiling, remove the meat, collect all scraps, and dry them in a blast drying oven. Condition 40～60℃, about 10h (too high temperature will lead to rapid oxidation of oil in the lobster head, too long drying time will also cause long-term oxidation of oil and affect production efficiency), so that the water content of the lobster can be kept at About 20% (because when the water content is low, the extraction rate is not high; when the water content is too high, the lobster head powder is easy to form a viscous mixture with the extraction solvent during the extraction process, which affects the separation of the solvent and the lobster head powder, and some of them are extremely Incomplete oil extraction), use a multifunctional pulverizer to pulverize to 40 mesh, and set aside.
有机溶剂震荡提取：将1∶7(g∶ml)虾粉和80％的乙醇装入样品瓶，密封，放入台式恒温震荡箱中，30～60℃，100rpm/min，浸提1～2h，浸提2次，此时提取率可达到11.04％。Organic solvent vibration extraction: put 1:7 (g:ml) shrimp powder and 80% ethanol into a sample bottle, seal it, put it in a desktop constant temperature vibration box, 30-60 ° C, 100 rpm/min, leaching for 1-2 hours , leaching twice, and the extraction rate can reach 11.04%.
离心分离：将浸提液转移到离心管中，在5000rpm下离心10min，取上清液为粗虾油。Centrifugal separation: transfer the extract to a centrifuge tube, centrifuge at 5000rpm for 10min, and take the supernatant as crude shrimp oil.
回收有机溶剂：将粗虾油在旋转蒸发仪上进行回收有机溶剂，温度为50℃，真空度为-0.1Mpa。Recovering the organic solvent: the crude shrimp oil was recovered on a rotary evaporator with a temperature of 50°C and a vacuum of -0.1Mpa.
脱胶：称取一定质量的粗虾油，用水浴锅加热至50～70℃，按质量比(磷酸∶油)加入0.1～0.3％浓度为85％的磷酸，加热搅拌30min，静置冷却。将虾油转移到离心管中，5000rpm/min离心10min，转移上层油层。Degumming: Weigh a certain quality of crude shrimp oil, heat it to 50-70°C with a water bath, add 0.1-0.3% phosphoric acid with a concentration of 85% according to the mass ratio (phosphoric acid: oil), heat and stir for 30 minutes, and let it stand for cooling. Transfer the shrimp oil to a centrifuge tube, centrifuge at 5000rpm/min for 10min, and transfer the upper oil layer.
脱酸：称取一定质量的脱胶得到的虾油，用水浴锅加热至40～60℃，按质量比(NaOH∶油)加入0.2～0.4％浓度为15％～20％，加热搅拌30min，静置冷却。将虾油转移到离心管中，5000rpm/min离心10min，转移上层油层。Deacidification: Weigh a certain amount of shrimp oil obtained by degumming, heat it to 40-60°C in a water bath, add 0.2-0.4% according to the mass ratio (NaOH: oil) to a concentration of 15%-20%, heat and stir for 30min, and let it stand. Set aside to cool. Transfer the shrimp oil to a centrifuge tube, centrifuge at 5000rpm/min for 10min, and transfer the upper oil layer.
脱色：称取一定质量的脱酸得到的虾油，用水浴锅加热至60～80℃，按质量比(凹土∶油)加入1～3％的凹土，加热搅拌15min，静置冷却。将虾油转移到离心管中，5000rpm/min离心10min，转移上层油层。Decolorization: Weigh a certain amount of deacidified shrimp oil, heat it to 60-80°C with a water bath, add 1-3% attapulgite according to the mass ratio (attapulgite: oil), heat and stir for 15 minutes, and let stand to cool. Transfer the shrimp oil to a centrifuge tube, centrifuge at 5000rpm/min for 10min, and transfer the upper oil layer.
水洗，干燥：将经过脱胶，脱酸，脱色的虾油，放入15％的水，3500rpm离心10min，分离。重复2次。最后置于冷冻干燥箱中-40℃，-0.05～-0.1MPa干燥12h得精制虾油。Washing and drying: Put the degummed, deacidified and decolored shrimp oil into 15% water, centrifuge at 3500rpm for 10min, and separate. Repeat 2 times. Finally, place it in a freeze-drying oven at -40°C and dry at -0.05 to -0.1 MPa for 12 hours to obtain refined shrimp oil.
本发明实施例利用乙醇作为提取剂，进行振荡提取，对克氏原螯虾废弃物中的天然虾油进行有效提取，通过本方法，可获得11.04％的虾油，该虾油透明澄清、呈现出虾青素体现的浅酒红色、具有龙虾所特有香味，营养价值丰富，不饱和脂肪酸含量达到总脂肪酸的47.98％、顺式脂肪酸含量占不饱和脂肪酸含量的95.65％以及EPA和DHA含量占多不饱和脂肪酸含量的7.15％，同时乙醇作为有机溶剂提取安全可靠。如能工厂化，不但可以减少资源浪费，还可以减少环境污染，提高企业的经济效益。In the embodiment of the present invention, ethanol is used as the extractant to perform vibration extraction to effectively extract the natural shrimp oil in the waste of Procambarus clarkii. Through this method, 11.04% of the shrimp oil can be obtained. The shrimp oil is transparent and clear, showing Astaxanthin is light wine red, has the unique fragrance of lobster, and is rich in nutritional value. The content of unsaturated fatty acids reaches 47.98% of the total fatty acids, the content of cis fatty acids accounts for 95.65% of the unsaturated fatty acids, and the content of EPA and DHA accounts for more The saturated fatty acid content is 7.15%, and ethanol is safe and reliable as an organic solvent for extraction. If it can be factoryized, it can not only reduce the waste of resources, but also reduce environmental pollution and improve the economic benefits of enterprises.
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements and improvements made within the spirit and principles of the present invention should be included in the protection of the present invention. within range.
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