CN106281048B - A kind of preparation method of low fishlike smell dog salmon fishskin gelatin - Google Patents
A kind of preparation method of low fishlike smell dog salmon fishskin gelatin Download PDFInfo
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Abstract
Description
技术领域technical field
本发明涉及一种鱼皮食品的制作领域,特别涉及一种低鱼腥味马哈鱼鱼皮明胶的制作方法。The invention relates to the field of making fish skin food, in particular to a method for making salmon skin gelatin with low fishy smell.
背景技术Background technique
明胶是胶原蛋白的水解产物,即胶原蛋白分子在热作用下断裂降解形成的天然高分子混合物,具有较高的安全性。猪牛等哺乳动物的皮和骨等一直是明胶的主要来源,但由于疯牛病、口蹄疫、禽流感等动物疾病的爆发使人们对哺乳动物明胶产生了质疑,欧盟甚至已经禁止食品中使用牛源明胶产品,而宗教信仰也在一定程度上阻碍了猪源明胶的应用。世界范围内明胶市场需求逐年增长,供不应求。因此,寻找新型资源开发明胶产品,取代猪、牛源明胶是明胶产业的必然发展趋势。鱼皮中胶原蛋白含量达到30%左右,是优质的潜在明胶资源。鱼皮明胶具有良好的生物可降解性和生物相容性,同时具有低致敏性等特点。利用鱼皮开发明胶产品不仅能够缓解明胶产业压力,还可以减少环境污染和资源浪费,提高水产加工副产物的经济价值。Gelatin is a hydrolyzed product of collagen, that is, a natural polymer mixture formed by breaking and degrading collagen molecules under the action of heat, which has high safety. The skin and bones of mammals such as pigs and cattle have always been the main source of gelatin. However, due to the outbreak of animal diseases such as mad cow disease, foot-and-mouth disease, and bird flu, people have questioned mammalian gelatin. The European Union has even banned the use of bovine gelatin in food. Products, and religious beliefs also hinder the application of pig-derived gelatin to a certain extent. The worldwide market demand for gelatin is increasing year by year, and the supply is in short supply. Therefore, it is an inevitable development trend of the gelatin industry to find new resources to develop gelatin products and replace pig and cattle source gelatin. The collagen content in fish skin reaches about 30%, which is a high-quality potential gelatin resource. Fish skin gelatin has good biodegradability and biocompatibility, as well as low allergenicity. Using fish skin to develop gelatin products can not only relieve the pressure on the gelatin industry, but also reduce environmental pollution and resource waste, and increase the economic value of by-products of aquatic product processing.
马哈鱼属鲑科鱼类,是著名的冷水性溯河产卵洄游鱼。我国是马哈鱼加工大国,由此产生大量废弃鱼皮。马哈鱼是名贵冷水鱼种,其鱼皮明胶与其它鱼类相比有自身特点,更易被吸收利用,被认为是开发胶原蛋白肽等功能产品的良好资源,具有广阔的市场开发价值。目前国内未见马哈鱼鱼皮明胶的提取报道,国外对马哈鱼鱼皮明胶的提取研究也鲜有报道。Salmon belongs to the family Salmonidae and is a well-known cold-water anadromous fish that spawns and migrates. my country is a big salmon processing country, resulting in a large amount of discarded fish skin. Salmon is a rare cold-water fish. Compared with other fish, its skin gelatin has its own characteristics and is easier to be absorbed and utilized. It is considered to be a good resource for developing functional products such as collagen peptides, and has broad market development value. At present, there is no report on the extraction of salmon skin gelatin in China, and there are few reports on the extraction of salmon skin gelatin abroad.
明胶生产工艺通常包括原料预处理、提取和干燥三部分,其中预处理和提取步骤是将胶原蛋白转化为明胶的关键步骤,预处理工艺直接关系到明胶的产量与品质。目前,明胶提取大多采用热水提取法,即指原料经过除脂肪、除杂蛋白等前处理后,在一定温度条件下直接用热水提取。The gelatin production process usually includes three parts: raw material pretreatment, extraction and drying. The pretreatment and extraction steps are the key steps to convert collagen into gelatin. The pretreatment process is directly related to the yield and quality of gelatin. At present, hot water extraction is mostly used for gelatin extraction, that is, raw materials are directly extracted with hot water at a certain temperature after pretreatment such as fat removal and protein removal.
传统鱼皮明胶提取工艺存在如下弊端:The traditional fish skin gelatin extraction process has the following disadvantages:
一、采用正己烷、石油醚、乙醚和正丁醇等有机溶剂进行除脂,影响明胶产品安全性,同时试剂成本高,且污染环境;1. Using organic solvents such as n-hexane, petroleum ether, diethyl ether and n-butanol for degreasing affects the safety of gelatin products, while the cost of reagents is high and pollutes the environment;
二、高浓度的碱液和盐酸浸泡原料,不易去除鱼皮中黑色素等物质,影响明胶产品外观性状,同时存在操作安全隐患;2. Soak raw materials with high concentration of lye and hydrochloric acid, it is not easy to remove melanin and other substances in fish skin, affect the appearance of gelatin products, and there are hidden dangers in operation safety;
三、鱼皮采用强酸脱钙,破坏明胶完整性,影响其功能性质;3. Fish skin is decalcified with strong acid, which destroys the integrity of gelatin and affects its functional properties;
四、鱼皮明胶的哈喇味腥味较重。4. Fish skin gelatin has a strong fishy smell.
发明内容Contents of the invention
本发明的目的在于开发一种安全、环保的马哈鱼鱼皮高值化加工的工艺,充分开发利用鱼皮中的胶原蛋白肽,提高马哈鱼加工过程中副产物的利用率,避免资源浪费与环境污染;同时丰富马哈鱼食品种类。The purpose of the present invention is to develop a safe and environmentally friendly process for high-value processing of salmon skin, fully develop and utilize collagen peptides in fish skin, improve the utilization rate of by-products in the processing of salmon, and avoid resources Waste and environmental pollution; at the same time enrich the food types of salmon.
为达到上述目的,本发明提供了一种低鱼腥味马哈鱼鱼皮明胶的制备方法,包括如下步骤:In order to achieve the above object, the invention provides a method for preparing salmon skin gelatin with low fishy smell, comprising the steps of:
S1、原料预处理:取马哈鱼鱼皮,清洗,备用;S1. Raw material pretreatment: take the salmon skin, wash it, and set it aside;
马哈鱼鱼皮,无须剃鳞,只需除去碎肉、泥沙等杂质。There is no need to shave the skin of salmon, only need to remove impurities such as minced meat and silt.
S2、向步骤S1得到的备用鱼皮中加入洗洁精水溶液,18~25℃浸泡3~5h,冲洗,收集鱼皮,即为脱脂鱼皮;S2. Add an aqueous solution of detergent to the spare fish skin obtained in step S1, soak at 18-25°C for 3-5 hours, rinse, and collect the fish skin, which is defatted fish skin;
所述备用鱼皮与所述洗洁精水溶液的质量体积比为1g:5~15ml;The mass-to-volume ratio of the standby fish skin to the aqueous detergent solution is 1g:5-15ml;
所述洗洁精水溶液为家庭常用的洗洁精加水稀释制得,高效、去油快、易冲洗不残留的洗洁精即可。The detergent aqueous solution is obtained by diluting common household detergent with water, and the detergent is high-efficiency, fast in degreasing, easy to rinse and leaves no residue.
S3、向步骤S2中得到的脱脂鱼皮加入氢氧化钠溶液,18~25℃浸泡3~8h,水洗至pH值为7~9,收集鱼皮,得到碱处理鱼皮;S3, adding sodium hydroxide solution to the defatted fish skin obtained in step S2, soaking at 18-25°C for 3-8 hours, washing with water until the pH value is 7-9, collecting the fish skin to obtain the alkali-treated fish skin;
所述氢氧化钠溶液浓度为0.01~0.1mol/L,所述脱脂鱼皮与所述氢氧化钠溶液的质量体积比为1g:3~15ml;The concentration of the sodium hydroxide solution is 0.01~0.1mol/L, and the mass volume ratio of the defatted fish skin to the sodium hydroxide solution is 1g:3~15ml;
S4、向步骤S3制得的碱处理鱼皮中加入过氧化氢水溶液,18~25℃浸泡1~4h,收集鱼皮,得到脱色鱼皮;S4. Add aqueous hydrogen peroxide solution to the alkali-treated fish skin prepared in step S3, soak at 18-25°C for 1-4 hours, collect the fish skin, and obtain decolorized fish skin;
所述过氧化氢水溶液体积浓度为0.5~2%,所述碱处理鱼皮与所述过氧化氢水溶液的质量体积比为1g:3~15ml;The volume concentration of the aqueous hydrogen peroxide solution is 0.5 to 2%, and the mass volume ratio of the alkali-treated fish skin to the aqueous hydrogen peroxide solution is 1g:3 to 15ml;
S5、向步骤S4制得的脱色鱼皮中加入柠檬酸溶液,18~25℃浸泡1~3h,用水洗3次,收集鱼皮,得到脱钙鱼皮;S5, adding citric acid solution to the decolorized fish skin prepared in step S4, soaking at 18-25° C. for 1-3 hours, washing with water 3 times, collecting the fish skin to obtain decalcified fish skin;
所述柠檬酸溶液的浓度为0.1~0.8mol/L,所述脱色鱼皮与所述柠檬酸溶液的质量体积比为1g:8~25ml;The concentration of the citric acid solution is 0.1~0.8mol/L, and the mass volume ratio of the decolorized fish skin and the citric acid solution is 1g:8~25ml;
S6、向步骤S5制得的脱钙鱼皮中加入磷酸溶液,18~25℃浸泡2~5h,水洗至pH值为6~7,收集鱼皮,得到酸处理鱼皮;S6, adding phosphoric acid solution to the decalcified fish skin prepared in step S5, soaking at 18-25°C for 2-5 hours, washing with water until the pH value is 6-7, collecting the fish skin to obtain acid-treated fish skin;
所述磷酸溶液的浓度为0.05~0.1mol/L,所述脱钙鱼皮与所述磷酸溶液的质量体积比为1g:4ml~10ml;The concentration of the phosphoric acid solution is 0.05~0.1mol/L, and the mass volume ratio of the decalcified fish skin to the phosphoric acid solution is 1g:4ml~10ml;
S7、向步骤S6制得的酸处理鱼皮中添加迷迭香提取物,在40~80℃环境下,加水浸提8~18h,冷却至18~25℃后,离心收集上清液,即为明胶溶液;S7. Add rosemary extract to the acid-treated fish skin prepared in step S6, add water for extraction at 40-80°C for 8-18 hours, cool to 18-25°C, and centrifuge to collect the supernatant, that is For gelatin solution;
所述酸处理鱼皮与加入水的质量体积比为1g:2~12ml;所述鱼皮与所述迷迭香提取物的质量比为1g:0.0005~0.005g;The mass volume ratio of the acid-treated fish skin to the water added is 1g:2-12ml; the mass ratio of the fish skin to the rosemary extract is 1g:0.0005-0.005g;
本发明所述迷迭香提取物为购自河南豫中生物科技有限公司的迷迭香粗提物。The rosemary extract of the present invention is the crude extract of rosemary purchased from Henan Yuzhong Biotechnology Co., Ltd.
S8、将步骤S7制得的明胶溶液冷冻干燥24~36h,得到低鱼腥味马哈鱼鱼皮明胶。S8. Freeze-dry the gelatin solution prepared in step S7 for 24-36 hours to obtain salmon skin gelatin with low fishy smell.
优选方式下,步骤S2所述备用鱼皮与所述洗洁精水溶液的质量体积比为1g:5~8ml;In a preferred manner, the mass volume ratio of the spare fish skin described in step S2 to the aqueous detergent solution is 1g:5-8ml;
步骤S3所述脱脂鱼皮与所述氢氧化钠溶液的质量体积比为1g:5~8ml;The mass-to-volume ratio of the degreased fish skin to the sodium hydroxide solution in step S3 is 1g:5-8ml;
步骤S4所述碱处理鱼皮与所述过氧化氢水溶液的质量体积比为1g:5~8ml;The mass volume ratio of the alkali-treated fish skin to the hydrogen peroxide aqueous solution in step S4 is 1g:5-8ml;
步骤S5所述脱色鱼皮与所述柠檬酸溶液的质量体积比为1g:8ml;The mass volume ratio of the decolorized fish skin described in step S5 to the citric acid solution is 1g:8ml;
步骤S6所述脱钙鱼皮与所述磷酸溶液的质量体积比为1g:4~8ml;The mass volume ratio of the decalcified fish skin to the phosphoric acid solution in step S6 is 1g:4-8ml;
步骤S7所述酸处理鱼皮与加入水的质量体积比为1g:5ml;所述鱼皮与所述迷迭香提取物的质量比为1g:0.002~0.003g。The mass volume ratio of the acid-treated fish skin to the water added in step S7 is 1g:5ml; the mass ratio of the fish skin to the rosemary extract is 1g:0.002-0.003g.
优选方式下,步骤S2、步骤S3、步骤S4、步骤S5、步骤S6所述浸泡过程每60~80分钟换一次浸泡溶液。In a preferred manner, the soaking process described in steps S2, S3, S4, S5, and S6 is changed every 60 to 80 minutes.
优选方式下,步骤S7所述离心的条件为:离心力4000~10000g,环境温度18~25℃,离心时间10~30min。In a preferred manner, the centrifugation conditions in step S7 are: centrifugal force 4000-10000g, ambient temperature 18-25°C, and centrifugation time 10-30min.
优选方式下,步骤S7所述冷冻干燥的方式为:真空冷冻干燥,干燥前将步骤S7制得的明胶溶液置于-80℃预冻2~4h。In a preferred manner, the freeze-drying method in step S7 is: vacuum freeze-drying, and the gelatin solution prepared in step S7 is pre-frozen at -80° C. for 2 to 4 hours before drying.
本发明相比于以往的工艺和同类产品有以下创新及优势:Compared with previous techniques and similar products, the present invention has the following innovations and advantages:
1、本发明以马哈鱼鱼皮为原料,提供了一种马哈鱼鱼皮明胶的制备方法,提高了废弃马哈鱼加工过程中副产物鱼皮的利用率,减少了环境污染。1. The present invention provides a preparation method of salmon skin gelatin using salmon skin as a raw material, which improves the utilization rate of by-product fish skin in the discarded salmon processing process and reduces environmental pollution.
2、本发明中的马哈鱼鱼皮无需进行剃鳞工艺,操作简便,降低了工人的操作难度,加工成本低、生产效率高。2. The salmon skin in the present invention does not need to be scaled, which is easy to operate, reduces the difficulty of operation for workers, has low processing cost and high production efficiency.
3、本发明中采用洗洁精水溶液代替传统方法中的有机溶剂除去鱼皮中的脂肪,用量少、成本低、无污染;洗洁精溶液浓度低、用量少,经过反复冲洗,可达无残留,使制备的明胶产品更安全,且一定程度上减少了鱼皮明胶产品的腥味。3, adopt liquid detergent solution to replace the organic solvent in the traditional method to remove the fat in the fish skin among the present invention, consumption is few, cost is low, pollution-free; Reaching no residue, making the prepared gelatin product safer, and reducing the fishy smell of the fish skin gelatin product to a certain extent.
4、本发明采用的氢氧化钠碱液浓度低于现有技术,且能达到较好去除杂蛋白的效果。4. The concentration of sodium hydroxide lye used in the present invention is lower than that of the prior art, and can achieve a better effect of removing foreign proteins.
5、本发明采用过氧化氢溶液短时浸泡处理鱼皮,使得鱼皮明胶的提取率明显增加,同时达到了鱼皮脱色的效果,使获得的明胶颜色性质更好;过氧化氢本身易分解,且溶液的浓度较低,反复冲洗后,可达到无残留。5. The present invention uses hydrogen peroxide solution to soak fish skin for a short time, so that the extraction rate of fish skin gelatin is significantly increased, and at the same time, the decolorization effect of fish skin is achieved, and the color properties of the obtained gelatin are better; hydrogen peroxide itself is easy to decompose , and the concentration of the solution is low, after repeated washing, no residue can be achieved.
6、本发明采用柠檬酸对鱼皮进行脱钙处理,获得的鱼皮明胶溶液更加澄清透明,明胶的颜色性质得到显著改善。6. The present invention uses citric acid to decalcify fish skin, and the obtained fish skin gelatin solution is more clear and transparent, and the color property of gelatin is significantly improved.
7、本发明在提取过程中添加少量迷迭香提取物,能够抑制提取过程中的脂肪氧化,有效减少鱼皮明胶产品的腥味。7. The present invention adds a small amount of rosemary extract in the extraction process, which can inhibit fat oxidation in the extraction process and effectively reduce the fishy smell of fish skin gelatin products.
8、本发明采用不同温度提取明胶,获得性质不同的鱼皮明胶,生产中可根据需要选择特定的处理条件、提取温度获得所需性质的明胶产品。8. The present invention uses different temperatures to extract gelatin to obtain fish skin gelatin with different properties. During production, specific processing conditions and extraction temperatures can be selected according to needs to obtain gelatin products with required properties.
综上,本发明方法采用洗洁精除脂、过氧化氢脱色、柠檬酸脱钙等工艺对鱼皮进行预处理,采用不同温度热水同时添加少量迷迭香提取物,提取获得一系列乳化性、起泡性、凝胶强度较好且鱼腥味较低的高品质鱼皮明胶,本发明改善了鱼皮明胶的性质,拓展了应用范围。In summary, the method of the present invention uses detergent degreasing, hydrogen peroxide decolorization, citric acid decalcification and other processes to pretreat the fish skin, and uses hot water at different temperatures to add a small amount of rosemary extract at the same time to obtain a series of emulsification. High-quality fish skin gelatin with good properties, foamability and gel strength and low fishy smell. The invention improves the properties of the fish skin gelatin and expands the application range.
具体实施方式Detailed ways
以下实施例对本发明的技术方案做进一步的说明,有助于了解本专利,但本发明的实施方案不受所述实施例的限制,本发明的保护范围有权利要求来决定。The following examples further illustrate the technical solutions of the present invention, which help to understand the patent, but the embodiments of the present invention are not limited by the examples, and the protection scope of the present invention is determined by the claims.
实施例1Example 1
制备马哈鱼鱼皮明胶的方法,包括以下步骤:The method for preparing salmon skin gelatin comprises the following steps:
(1)取马哈鱼鱼皮,无须剃鳞,除去碎肉、泥沙等杂质,切碎,洗净,备用;(1) Take salmon skin, remove scales without shaving, remove impurities such as minced meat and silt, chop, wash, and set aside;
(2)将洗净的鱼皮用体积分数1%洗洁精水溶液浸泡,浸泡时间为3h,每1h换一次溶液,马哈鱼鱼皮与洗洁精水溶液的质量体积比为1g:5ml,浸泡结束后用自来水冲洗3次,收集鱼皮;(2) Soak the cleaned fish skin with a volume fraction of 1% detergent solution, the soaking time is 3h, change the solution every 1h, the mass volume ratio of salmon skin and detergent solution is 1g:5ml, Rinse 3 times with tap water after soaking to collect fish skin;
(3)向(2)步骤中得到的鱼皮加0.05mol/L氢氧化钠溶液浸泡4h,每80min换一次溶液,鱼皮与氢氧化钠溶液的质量体积比为1g:5ml,碱处理后,水洗至中性,收集鱼皮;(3) Add 0.05mol/L sodium hydroxide solution to the fish skin obtained in (2) step and soak for 4h, change the solution once every 80min, the mass volume ratio of fish skin and sodium hydroxide solution is 1g:5ml, after alkali treatment , washed with water until neutral, and the fish skin was collected;
(4)向(3)步骤中得到的鱼皮加入体积浓度为1%过氧化氢溶液浸泡,浸泡时间为2h,每1h换溶液,鱼皮与过氧化氢溶液的质量体积比为1g:5ml,浸泡后,自来水冲洗3次,收集鱼皮;(4) adding volume concentration to the fish skin obtained in (3) step is 1% hydrogen peroxide solution soaking, soaking time is 2h, every 1h changes solution, the mass volume ratio of fish skin and hydrogen peroxide solution is 1g:5ml , after soaking, rinse with tap water 3 times to collect the fish skin;
(5)向(4)步骤中得到的鱼皮中加入0.1mol/L柠檬酸溶液浸泡2h,每1h换一次溶液,鱼皮与柠檬酸溶液的质量体积比为1g:8ml;浸泡后,自来水冲洗3次,收集鱼皮;(5) Add 0.1mol/L citric acid solution to the fish skin obtained in step (4) and soak for 2 hours, change the solution every 1 hour, the mass volume ratio of fish skin and citric acid solution is 1g: 8ml; after soaking, tap water Rinse 3 times to collect fish skin;
(6)向(5)步骤中的到的鱼皮中加入0.05mol/L磷酸浸泡3h,每1.5h换一次溶液,鱼皮与磷酸溶液的质量体积比为1g:4ml,酸处理后,水洗至中性,收集鱼皮;(6) Add 0.05mol/L phosphoric acid to the fish skin obtained in step (5) and soak for 3 hours, change the solution every 1.5 hours, the mass volume ratio of fish skin and phosphoric acid solution is 1g:4ml, after acid treatment, wash with water to neutral, to collect the fish skin;
(7)将(6)步骤中的鱼皮用去离子水在45℃下进行提取10h,迷迭香提取物添加量为鱼皮质量的2‰,鱼皮与去离子水的质量体积比为1g:5ml;冷却至室温后,离心(1000g,10min,18℃),收集上清液;(7) Extract the fish skin in step (6) with deionized water for 10 h at 45° C., the amount of rosemary extract added is 2‰ of the fish skin quality, and the mass volume ratio of fish skin to deionized water is 1g: 5ml; after cooling to room temperature, centrifuge (1000g, 10min, 18°C), and collect the supernatant;
(8)将(7)中获得的明胶溶液置于-80℃下2h,而后进行真空冷冻干燥24h即的明胶产品。(8) Put the gelatin solution obtained in (7) at -80° C. for 2 hours, and then conduct vacuum freeze-drying for 24 hours to obtain the gelatin product.
本实施例制得的鱼皮明胶的具体性状见表1~6。The specific properties of the fish skin gelatin prepared in this embodiment are shown in Tables 1-6.
另外,制作不加H2O2的明胶产品作为对比例,即除未经过步骤(4)处理外,其他过程与实施例1均相同。In addition, a gelatin product without adding H 2 O 2 was made as a comparative example, that is, the other processes were the same as in Example 1 except that it was not processed in step (4).
实施例2Example 2
制备马哈鱼鱼皮明胶的方法,包括以下步骤:The method for preparing salmon skin gelatin comprises the following steps:
(1)取马哈鱼鱼皮,无须剃鳞,除去碎肉、泥沙等杂质,切碎,洗净,备用;(1) Take salmon skin, remove scales without shaving, remove impurities such as minced meat and silt, chop, wash, and set aside;
(2)将洗净的鱼皮用体积分数0.5%洗洁精水溶液浸泡,浸泡时间为4h,每1h换一次溶液,马哈鱼鱼皮与洗洁精水溶液的质量体积比为1g:8ml,浸泡结束后用自来水冲洗3次,收集鱼皮;(2) Soak the cleaned fish skin with a volume fraction of 0.5% detergent solution, the soaking time is 4h, change the solution every 1h, the mass volume ratio of salmon skin and detergent solution is 1g:8ml, Rinse 3 times with tap water after soaking to collect fish skin;
(3)向(2)步骤中得到的鱼皮加0.08mol/L氢氧化钠溶液浸泡4h,每80min换一次溶液,鱼皮与氢氧化钠溶液的质量体积比为1g:8ml,碱处理后,水洗至中性,收集鱼皮;(3) Add 0.08mol/L sodium hydroxide solution to the fish skin obtained in (2) step and soak for 4h, change the solution once every 80min, the mass volume ratio of fish skin and sodium hydroxide solution is 1g:8ml, after alkali treatment , washed with water until neutral, and the fish skin was collected;
(4)向(3)步骤中得到的鱼皮加入体积浓度为1%过氧化氢溶液浸泡,浸泡时间为2h,每1h换溶液,鱼皮与过氧化氢溶液的质量体积比为1g:8ml,浸泡后,自来水冲洗3次,收集鱼皮;(4) adding volume concentration to the fish skin obtained in (3) step is 1% hydrogen peroxide solution soaking, soaking time is 2h, every 1h changes solution, the mass volume ratio of fish skin and hydrogen peroxide solution is 1g:8ml , after soaking, rinse with tap water 3 times to collect the fish skin;
(5)向(4)步骤中得到的鱼皮中加入0.2mol/L柠檬酸溶液浸泡2h,每1h换一次溶液,鱼皮与柠檬酸溶液的质量体积比为1g:8ml;浸泡后,自来水冲洗3次,收集鱼皮;(5) Add 0.2mol/L citric acid solution to the fish skin obtained in step (4) and soak for 2 hours, change the solution every 1 hour, the mass volume ratio of fish skin and citric acid solution is 1g: 8ml; after soaking, tap water Rinse 3 times to collect fish skin;
(6)向(5)步骤中的到的鱼皮中加入0.08mol/L磷酸浸泡3h,每1.5h换一次溶液,鱼皮与磷酸溶液的质量体积比为1g:8ml,酸处理后,水洗至中性,收集鱼皮;(6) Add 0.08mol/L phosphoric acid to the fish skin obtained in step (5) and soak for 3 hours, change the solution every 1.5 hours, the mass volume ratio of fish skin and phosphoric acid solution is 1g:8ml, after acid treatment, wash with water to neutral, to collect the fish skin;
(7)将(6)步骤中的鱼皮用去离子水在55℃下进行提取10h,迷迭香添提取物加量为3‰,鱼皮与去离子水的质量体积比为1g:5ml;冷却至室温后,离心(1000g,20min,18℃),收集上清液;(7) Extract the fish skin in step (6) with deionized water at 55°C for 10 hours, the amount of rosemary extract is 3‰, and the mass volume ratio of fish skin to deionized water is 1g:5ml ; After cooling to room temperature, centrifuge (1000g, 20min, 18°C) to collect the supernatant;
(8)将(7)中获得的明胶溶液置于-80℃下2h,而后进行真空冷冻干燥24h即的明胶产品。(8) Put the gelatin solution obtained in (7) at -80° C. for 2 hours, and then conduct vacuum freeze-drying for 24 hours to obtain the gelatin product.
本实施例制得的鱼皮明胶的具体性状见表1~6。The specific properties of the fish skin gelatin prepared in this embodiment are shown in Tables 1-6.
另外,制作不加H2O2的明胶产品作为对比例,即除未经过步骤(4)处理外,其他过程与实施例2均相同。In addition, a gelatin product without adding H 2 O 2 was made as a comparative example, that is, the other processes were the same as in Example 2 except that it was not processed in step (4).
实施例3Example 3
制备马哈鱼鱼皮明胶的方法,包括以下步骤:The method for preparing salmon skin gelatin comprises the following steps:
(1)取马哈鱼鱼皮,无须剃鳞,除去碎肉、泥沙等杂质,切碎,洗净,备用;(1) Take salmon skin, remove scales without shaving, remove impurities such as minced meat and silt, chop, wash, and set aside;
(2)将洗净的鱼皮用体积分数2%洗洁精水溶液浸泡,浸泡时间为4h,每1h换一次溶液,马哈鱼鱼皮与洗洁精水溶液的质量体积比为1g:10ml,浸泡结束后用自来水冲洗3次,收集鱼皮;(2) Soak the cleaned fish skin with a volume fraction of 2% detergent aqueous solution, the soaking time is 4h, and change the solution every 1h, the mass volume ratio of salmon skin and detergent aqueous solution is 1g:10ml, Rinse 3 times with tap water after soaking to collect fish skin;
(3)向(2)步骤中得到的鱼皮加0.1mol/L氢氧化钠溶液浸泡3h,每1h换一次溶液,鱼皮与氢氧化钠溶液的质量体积比为1g:10ml,碱处理后,水洗至中性,收集鱼皮;(3) Add 0.1mol/L sodium hydroxide solution to the fish skin obtained in (2) step and soak for 3h, change the solution every 1h, the mass volume ratio of fish skin and sodium hydroxide solution is 1g:10ml, after alkali treatment , washed with water until neutral, and the fish skin was collected;
(4)向(3)步骤中得到的鱼皮加入体积浓度为1%过氧化氢溶液浸泡,浸泡时间为2h,每1h换溶液,鱼皮与过氧化氢溶液的质量体积比为1g:10ml,浸泡后,自来水冲洗3次,收集鱼皮;(4) adding volume concentration to the fish skin obtained in (3) step is 1% hydrogen peroxide solution soaking, soaking time is 2h, every 1h changes solution, the mass volume ratio of fish skin and hydrogen peroxide solution is 1g:10ml , after soaking, rinse with tap water 3 times to collect the fish skin;
(5)向(4)步骤中得到的鱼皮中加入0.3mol/L柠檬酸溶液浸泡2h,每1h换一次溶液,鱼皮与柠檬酸溶液的质量体积比为1g:10ml;浸泡后,自来水冲洗3次,收集鱼皮;(5) Add 0.3mol/L citric acid solution to the fish skin obtained in step (4) and soak for 2 hours, change the solution every 1 hour, the mass volume ratio of fish skin and citric acid solution is 1g: 10ml; after soaking, tap water Rinse 3 times to collect fish skin;
(6)向(5)步骤中的到的鱼皮中加入0.1mol/L磷酸浸泡3h,每1.5h换一次溶液,鱼皮与磷酸溶液的质量体积比为1g:10ml,酸处理后,水洗至中性,收集鱼皮;(6) Add 0.1mol/L phosphoric acid to the fish skin obtained in step (5) and soak for 3 hours, change the solution every 1.5 hours, the mass volume ratio of fish skin and phosphoric acid solution is 1g:10ml, after acid treatment, wash with water to neutral, to collect the fish skin;
(7)将(6)步骤中的鱼皮用去离子水在65℃下进行提取10h,迷迭香提取物添加量为4‰,鱼皮与去离子水的质量体积比为1g:5ml;冷却至室温后,离心(1000g,10min,18℃),收集上清液;(7) Extract the fish skin in step (6) with deionized water at 65° C. for 10 h, the amount of rosemary extract added is 4‰, and the mass volume ratio of fish skin to deionized water is 1 g: 5 ml; After cooling to room temperature, centrifuge (1000g, 10min, 18°C), and collect the supernatant;
(8)将(7)中获得的明胶溶液置于-80℃下2h,而后进行真空冷冻干燥24h即的明胶产品。(8) Put the gelatin solution obtained in (7) at -80° C. for 2 hours, and then conduct vacuum freeze-drying for 24 hours to obtain the gelatin product.
本实施例制得的鱼皮明胶的具体性状见表1~6。The specific properties of the fish skin gelatin prepared in this embodiment are shown in Tables 1-6.
另外,制作不加H2O2的明胶产品作为对比例,即除未经过步骤(4)处理外,其他过程与实施例3均相同。In addition, a gelatin product without adding H 2 O 2 was made as a comparative example, that is, the other processes were the same as in Example 3 except that it was not processed in step (4).
实施例4Example 4
制备马哈鱼鱼皮明胶的方法,包括以下步骤:The method for preparing salmon skin gelatin comprises the following steps:
(1)取马哈鱼鱼皮,无须剃鳞,除去碎肉、泥沙等杂质,切碎,洗净,备用;(1) Take salmon skin, remove scales without shaving, remove impurities such as minced meat and silt, chop, wash, and set aside;
(2)将洗净的鱼皮用体积分数1%洗洁精水溶液浸泡,浸泡时间为4h,每1h换一次溶液,马哈鱼鱼皮与洗洁精水溶液的质量体积比为1g:7ml,浸泡结束后用自来水冲洗3次,收集鱼皮;(2) Soak the cleaned fish skin with a volume fraction of 1% detergent aqueous solution, the soaking time is 4h, and change the solution every 1h, the mass volume ratio of salmon skin and detergent aqueous solution is 1g:7ml, Rinse 3 times with tap water after soaking to collect fish skin;
(3)向(2)步骤中得到的鱼皮加0.05mol/L氢氧化钠溶液浸泡3h,每1h换一次溶液,鱼皮与氢氧化钠溶液的质量体积比为1g:7ml,碱处理后,水洗至中性,收集鱼皮;(3) add 0.05mol/L sodium hydroxide solution to the fish skin obtained in (2) step and soak for 3h, change the solution every 1h, the mass volume ratio of fish skin and sodium hydroxide solution is 1g:7ml, after alkali treatment , wash with water until neutral, and collect the fish skin;
(4)向(3)步骤中得到的鱼皮加入体积浓度为2%过氧化氢溶液浸泡,浸泡时间为2h,每1h换溶液,鱼皮与过氧化氢溶液的质量体积比为1g:7ml,浸泡后,自来水冲洗3次,收集鱼皮;(4) adding volume concentration to the fish skin obtained in (3) step is 2% hydrogen peroxide solution soaking, soaking time is 2h, every 1h changes solution, the mass volume ratio of fish skin and hydrogen peroxide solution is 1g:7ml , after soaking, rinse with tap water 3 times to collect the fish skin;
(5)向(4)步骤中得到的鱼皮中加入0.5mol/L柠檬酸溶液浸泡2h,每1h换一次溶液,鱼皮与柠檬酸溶液的质量体积比为1g:15ml;浸泡后,自来水冲洗3次,收集鱼皮;(5) Add 0.5mol/L citric acid solution to the fish skin obtained in step (4) and soak for 2 hours, change the solution every 1 hour, the mass volume ratio of fish skin and citric acid solution is 1g: 15ml; after soaking, tap water Rinse 3 times to collect fish skin;
(6)向(5)步骤中的到的鱼皮中加入0.05mol/L磷酸浸泡3h,每1.5h换一次溶液,鱼皮与磷酸溶液的质量体积比为1g:7ml,酸处理后,水洗至中性,收集鱼皮;(6) Add 0.05mol/L phosphoric acid to soak in the fish skin obtained in (5) step for 3h, change the solution every 1.5h, the mass volume ratio of fish skin and phosphoric acid solution is 1g:7ml, after acid treatment, wash with water to neutral, to collect fish skin;
(7)将(6)步骤中的鱼皮用去离子水在75℃下进行提取10h,迷迭香提取物添加量为5‰,鱼皮与去离子水的质量体积比为1g:5ml;冷却至室温后,离心(1000g,10min,18℃),收集上清液;(7) Extract the fish skin in step (6) with deionized water at 75° C. for 10 h, the amount of rosemary extract added is 5 ‰, and the mass volume ratio of fish skin to deionized water is 1 g: 5 ml; After cooling to room temperature, centrifuge (1000g, 10min, 18°C), and collect the supernatant;
(8)将(7)中获得的明胶溶液置于-80℃下2h,而后进行真空冷冻干燥24h即的明胶产品。(8) Put the gelatin solution obtained in (7) at -80° C. for 2 hours, and then conduct vacuum freeze-drying for 24 hours to obtain the gelatin product.
另外,制作不加H2O2的明胶产品作为对比例,即除未经过步骤(4)处理外,其他过程与实施例4均相同。In addition, a gelatin product without adding H 2 O 2 was made as a comparative example, that is, the other processes were the same as in Example 4 except that it was not processed in step (4).
本实施例制得的鱼皮明胶的具体性状见表1~6。The specific properties of the fish skin gelatin prepared in this embodiment are shown in Tables 1-6.
本发明各实施例制得的鱼皮明胶的具体性状如表1~6所示;其中,表1为各实施例的鱼皮明胶提取率,表2为各实施例制得的鱼皮明胶及商业明胶的颜色比较,表3为各实施例制得的鱼皮明胶及商业明胶的凝胶强度比较,表4为各实施例制得的鱼皮明胶及商业明胶的起泡性比较,表5为各实施例制得的鱼皮明胶及商业明胶的乳化性比较,表6为各实施例制得的鱼皮明胶及商业明胶的挥发性物质含量比较。The concrete character of the fish skin gelatin that each embodiment of the present invention makes is as shown in Table 1~6; Wherein, table 1 is the fish skin gelatin extraction rate of each embodiment, and table 2 is the fish skin gelatin that each embodiment makes and The color comparison of commercial gelatin, table 3 is the gel strength comparison of fish skin gelatin and commercial gelatin that each embodiment makes, and table 4 is the foamability comparison of fish skin gelatin and commercial gelatin that each embodiment makes, table 5 For the comparison of the emulsifying properties of the fish skin gelatin prepared in each embodiment and commercial gelatin, Table 6 is a comparison of the volatile matter content of the fish skin gelatin prepared in each embodiment and commercial gelatin.
表1Table 1
从表1数据可明显看出,本发明中过氧化氢的添加明显提高了明胶的提取率。As can be clearly seen from the data in Table 1, the addition of hydrogen peroxide in the present invention has obviously improved the extraction rate of gelatin.
本发明采用测色仪测定各实施例制得的鱼皮明胶冻干粉末及商业明胶的颜色,结果如表2所示。The present invention uses a colorimeter to measure the color of the fish skin gelatin freeze-dried powder and commercial gelatin prepared in each embodiment, and the results are shown in Table 2.
表2Table 2
在明胶产品中,钙含量多少对明胶的影响主要体现在透明度上,会影响明胶的亮度,从测色仪测定的L*值上就可以看出。如表2数据所示,本发明所提取的明胶L*(黑-白)值高于商业明胶,而a*(红-绿)、b*(黄-蓝)和△E值明显低于商业明胶,说明本发明提取的明胶颜色较好,间接说明脱钙效果较好。In gelatin products, the influence of calcium content on gelatin is mainly reflected in the transparency, which will affect the brightness of gelatin, which can be seen from the L* value measured by the colorimeter. As shown in table 2 data, the gelatin L* (black-white) value that the present invention extracts is higher than commercial gelatin, and a* (red-green), b* (yellow-blue) and △ E value are obviously lower than commercial gelatin Gelatin, shows that the color of the gelatin extracted by the present invention is better, indirectly shows that the decalcification effect is better.
本发明采用质构仪测定各实施例制得的鱼皮明胶及商业明胶的凝胶强度,测定方法如下:The present invention adopts texture analyzer to measure the gel strength of fish skin gelatin and commercial gelatin that each embodiment makes, and measuring method is as follows:
冻干的胶原蛋白溶解于60℃去离子水中,使最终浓度为6.67%(w/v)Lyophilized collagen was dissolved in deionized water at 60°C to a final concentration of 6.67% (w/v)
磁力搅拌直到胶原全部溶解,在10℃冰箱中16~18h,成胶。胶的尺寸:直径3cm,高2.5cm.用质构仪测定其凝胶特性,质构仪条件:载荷5kN,P/5探头,测试前速度为5.00mm/s,测试速度为1.00mm/s,测试后速度为5.00mm/s,探头深入距离为10mm。每个样品重复三次,取平均值。Stir magnetically until the collagen is completely dissolved, and place in a refrigerator at 10°C for 16-18 hours to form a gel. The size of the glue: 3cm in diameter, 2.5cm in height. Measure its gel properties with a texture analyzer. Conditions of the texture analyzer: load 5kN, P/5 probe, the speed before the test is 5.00mm/s, and the test speed is 1.00mm/s , the speed after the test is 5.00mm/s, and the probe penetration distance is 10mm. Each sample was repeated three times and the average value was taken.
结果如表3所示。The results are shown in Table 3.
表3table 3
从表3数据可看出:实施例1中的明胶凝胶强度和商业明胶较接近。本发明中的商业明胶为牛皮明胶,一般来说,鱼皮明胶的凝胶强度远低于哺乳动物明胶,很多鱼皮明胶研究中发现类似的结果,这是目前鱼皮明胶不能够完全代替哺乳动物明胶的一个重要原因。本发明所提取明胶的凝胶强度与商业明胶相比明胶凝胶强度和商业明胶非常接近,完全可替代哺乳动物明胶应用于冷冻冷藏产品中,实现合理的推广应用。As can be seen from the data in Table 3: the gel strength of gelatin in Example 1 is closer to that of commercial gelatin. The commercial gelatin in the present invention is cowhide gelatin. Generally speaking, the gel strength of fish skin gelatin is far lower than that of mammalian gelatin. Similar results have been found in many fish skin gelatin studies. This is because fish skin gelatin cannot completely replace breastfeeding at present. An important reason for animal gelatin. Compared with commercial gelatin, the gel strength of the gelatin extracted by the present invention is very close to that of commercial gelatin, and can completely replace mammalian gelatin and be used in frozen and refrigerated products to realize reasonable popularization and application.
本发明将各实施例制得的鱼皮明胶冻干、复溶,即按不同的浓度(g/ml)算出所需要的冻干样品,然后溶于60℃水中,磁力搅拌至完全溶解,得到蛋白浓度分别为1、2、3g/ml的明胶溶液。The present invention freeze-dries and redissolves the fish skin gelatin prepared in each embodiment, that is, calculates the required freeze-dried samples according to different concentrations (g/ml), then dissolves them in water at 60°C, and magnetically stirs until completely dissolved to obtain Gelatin solutions with protein concentrations of 1, 2, and 3 g/ml, respectively.
表4为各实施例制得的鱼皮明胶及商业明胶的发泡性的测试结果;具体测试方法如下:用冻干样品配制不同浓度的胶原蛋白溶液,转移至10ml带刻度的试管中,室温,匀浆1min,13400rpm;样品静置0-30min;Table 4 is the test result of the foamability of the fish skin gelatin and commercial gelatin that each embodiment makes; , homogenate for 1min, 13400rpm; samples stand for 0-30min;
FE(%)=(VT/V0)×100FE(%)=(VT/V0)×100
FS(%)=(Vt/V0)×100FS(%)=(Vt/V0)×100
VT:匀浆后总体积;V0:匀浆前总体积;Vt:室温下静置30min的总体积。VT: total volume after homogenization; V0: total volume before homogenization; Vt: total volume at room temperature for 30 minutes.
表4Table 4
从表4数据可以看出:本发明中实施例4中的起泡性最好,与商业明胶非常接近。本发明提取的明胶在这方面的应用可以代替商业明胶,即哺乳动物明胶。As can be seen from the data in Table 4: the foamability in Example 4 of the present invention is the best, which is very close to commercial gelatin. The gelatin extracted by the present invention can replace commercial gelatin, ie mammalian gelatin, in this application.
本发明采用风光光度计法测定各实施例制得的鱼皮明胶及商业明胶的乳化性,具体测试方法如下:The present invention adopts the scenery photometer method to measure the emulsifying property of fish skin gelatin and commercial gelatin that each embodiment makes, and concrete test method is as follows:
(1)用冻干样品配制不同浓度的胶原蛋白溶液至少3ml;(1) Prepare at least 3ml of collagen solutions of different concentrations with freeze-dried samples;
(2)将1ml黄豆油与3ml不同浓度的胶原蛋白溶液匀浆:20000rpm,1min;(2) Homogenize 1ml soybean oil with 3ml collagen solutions of different concentrations: 20000rpm, 1min;
(3)分别在匀浆后0min和10min后吸出乳胶,并用0.1%SDS稀释100倍,涡旋混匀10s;(3) Aspirate the latex after 0 min and 10 min after homogenization, dilute 100 times with 0.1% SDS, and vortex mix for 10 s;
(4)用分光光度计测500nm下的吸光值,以0.1%SDS做空白对照;(4) Measure the absorbance value at 500nm with a spectrophotometer, and use 0.1% SDS as a blank control;
EAI(m2/g)=(2×2.303×A×DF)/L∮CEAI(m 2 /g)=(2×2.303×A×DF)/L∮C
A:500nm下的吸光值;DF:稀释倍数;L:比色皿路径长度(0.01m)∮:乳化液中油相的比例(0.25)油体积分数;C:水相中蛋白浓度(g/m3)A: absorbance value at 500nm; DF: dilution factor; L: path length of cuvette (0.01m)∮: ratio of oil phase in emulsion (0.25) oil volume fraction; C: protein concentration in water phase (g/m 3 )
ESI(min)=A0/(A0-A10)×△tESI(min)=A 0 /(A 0 -A 10 )×△t
△t=10min;A0和A10分别为0min和10min时500nm下的吸光值。Δt=10min; A 0 and A 10 are the absorbance values at 500nm at 0min and 10min respectively.
结果如表5所示。The results are shown in Table 5.
表5table 5
从表5数据可以看出:本发明中提取的明胶乳化性都很好,实施例1和实施例2中的明胶明显高于商业明胶,而实施例3和实施例4中的明胶与商业明胶接近。As can be seen from the data in Table 5: the gelatin emulsifying property extracted in the present invention is all very good, and the gelatin in embodiment 1 and embodiment 2 is obviously higher than commercial gelatin, and the gelatin in embodiment 3 and embodiment 4 and commercial gelatin near.
本发明通过GC-MS检测各实施例制得的鱼皮明胶及对照组鱼皮明胶的挥发性物质含量,结果如表6所示。其中,对照组鱼皮明胶为不加迷迭香提取物制得的鱼皮明胶,具体制备步骤与实施例1相同。The present invention detects the volatile substance content of the fish skin gelatin prepared in each embodiment and the fish skin gelatin of the control group by GC-MS, and the results are shown in Table 6. Wherein, the fish skin gelatin of the control group is fish skin gelatin prepared without adding rosemary extract, and the specific preparation steps are the same as in Example 1.
表6Table 6
注:ND代表未检出。Note: ND means not detected.
从表6数据可以明显看出:本发明提取的明胶,挥发性物质含量明显降低,腥味有所改善。As can be clearly seen from the data in Table 6: the gelatin extracted by the present invention has significantly reduced volatile matter content and improved fishy smell.
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明披露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。The above is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Anyone familiar with the technical field within the technical scope disclosed in the present invention, according to the technical solution of the present invention Any equivalent replacement or change of the inventive concepts thereof shall fall within the protection scope of the present invention.
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