CN115104688A - A kind of liquid preparation of non-denatured type II collagen and preparation method thereof - Google Patents
A kind of liquid preparation of non-denatured type II collagen and preparation method thereof Download PDFInfo
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Abstract
Description
技术领域technical field
本发明属于食品加工技术领域,尤其涉及一种非变性II型胶原蛋白的液体制剂及其制备方法。The invention belongs to the technical field of food processing, and in particular relates to a liquid preparation of non-denatured type II collagen and a preparation method thereof.
背景技术Background technique
II型胶原蛋白广泛存在于动物软骨组织中,非变性II型胶原蛋白是指经提取后,仍能保留完整大分子胶原蛋白三螺旋结构的II型胶原蛋白,非变性II型胶原蛋白的二级结构是由三条肽链组成的三股螺旋,各个链中的氨基酸通过肽键结合在一起,而三条肽链则通过氢键、偶极-偶极键、离子键和范德华力相互作用保持在三螺旋结构中。但非变性II型胶原蛋白的三螺旋结构极易受内因或外因的影响,如环境温度高于35℃,能导致非变性II型胶原蛋白的三条肽链之间的氢键不断减弱,肽链的螺旋度减少,逐渐伸直解螺旋,整个蛋白质结构的无序性增加,变性后的II型胶原蛋白生物活性明显降低。Type II collagen widely exists in animal cartilage tissue. Non-denatured type II collagen refers to type II collagen that can still retain the triple helix structure of macromolecular collagen after extraction. The structure is a triple helix consisting of three peptide chains, the amino acids in each chain are held together by peptide bonds, and the three peptide chains are held in the triple helix by hydrogen bonds, dipole-dipole bonds, ionic bonds, and van der Waals interactions. in the structure. However, the triple helix structure of non-denatured type II collagen is easily affected by internal or external factors. For example, if the ambient temperature is higher than 35°C, the hydrogen bonds between the three peptide chains of non-denatured type II collagen can be continuously weakened and the peptide chains The helicity of the denatured collagen decreases, gradually straightens and unwinds, the disorder of the entire protein structure increases, and the biological activity of denatured type II collagen is significantly reduced.
非变性II型胶原蛋白是关节软骨中不可或缺的胶原蛋白成分,并且在软骨细胞的发育和成熟过程中发挥着至关重要的作用。同时在类风湿性关节炎、骨关节炎的病理研究中以及口服治疗类风湿关节炎方面已有临床试验报道,在类风湿性关节炎和骨关节炎的预防和治疗中极具开发应用潜力。Nondenatured type II collagen is an integral collagen component of articular cartilage and plays a crucial role in the development and maturation of chondrocytes. At the same time, clinical trials have been reported in the pathological research of rheumatoid arthritis and osteoarthritis and oral treatment of rheumatoid arthritis, and it has great potential for development and application in the prevention and treatment of rheumatoid arthritis and osteoarthritis.
非变性II型胶原蛋白虽然具有很高的生理活性,但由于非变性II型胶原白特定的致密纤维结构导致不溶于水且变性温度低,限制了非变性II型胶原蛋白在食品和保健食品领域的应用。Although non-denatured type II collagen has high physiological activity, due to the specific dense fibrous structure of non-denatured type II collagen, it is insoluble in water and the denaturation temperature is low, which limits the use of non-denatured type II collagen in the field of food and health food. Applications.
近年来,对于非变性II型胶原蛋白的研究逐渐增多,但多集中在提取工艺的研究,对难溶于水的非变性II型胶原蛋白的应用研究较少。在现有技术中,关于含有Ⅱ型胶原蛋白的咀嚼型或片剂型产品,不利于老年人服用,并且无法进行后续应用于活菌型酸奶、果汁、果冻等冷链食品中,进而起到增加食品改善膝关节健康的功能性。In recent years, the research on non-denatured type II collagen has gradually increased, but most of them focus on the research of extraction process, and the application of non-denatured type II collagen which is insoluble in water is less. In the prior art, chewable or tablet-type products containing type II collagen are unfavorable for the elderly to take, and cannot be subsequently applied to cold-chain foods such as live bacteria-type yogurt, fruit juice, jelly, etc. Increase the functionality of foods to improve knee health.
因此,亟待提供一种非变性II型胶原蛋白的胶体悬浮液,以及可低温水冲服并保持II型胶原蛋白活性的固体颗粒型饮品,填补保健食品领域针对非变性II型胶原蛋白产品只可生产片剂或胶囊而无其他类型产品的空白。Therefore, it is urgent to provide a colloidal suspension of non-denatured type II collagen, and a solid granular beverage that can be brewed with low temperature water and maintain the activity of type II collagen, filling the field of health food for non-denatured type II collagen products that can only be produced Tablets or capsules without blanks for other types of products.
发明内容SUMMARY OF THE INVENTION
为了解决上述问题,本发明提出了一种非变性II型胶原蛋白的液体制剂,所述液体制剂为胶体悬浮液或能采用35℃以下的水冲调成胶体悬浮液的悬浮型固体饮料。In order to solve the above problems, the present invention proposes a liquid preparation of non-denatured type II collagen, which is a colloidal suspension or a suspension-type solid beverage that can be prepared into a colloidal suspension with water below 35°C.
所述胶体悬浮液,均匀透明,悬浮稳定性能至少保持30天,在pH3-7条件下均能保持稳定。The colloidal suspension is uniform and transparent, and the suspension stability can be maintained for at least 30 days, and can be kept stable under the condition of pH 3-7.
所述胶体悬浮液由以下原料组成:2-10份非变性II型胶原蛋白粉、1-5份亲水胶体、1-3份低聚糖、1-5份水解II型胶原蛋白,余量用水补充至100份。The colloidal suspension is composed of the following raw materials: 2-10 parts of non-denatured type II collagen powder, 1-5 parts of hydrophilic colloid, 1-3 parts of oligosaccharides, 1-5 parts of hydrolyzed type II collagen, the balance Make up to 100 servings with water.
所述悬浮型固体饮料由以下原料组成:权利要求2所述胶体悬浮液除去水分的产品25-70份;鱼胶原蛋白肽10-20份、沙棘粉5-10份、柠檬酸0-10份、维生素C 0-5份、柠檬酸钠0-3份、姜黄0.1-1份、香精0-1份。The suspension-type solid beverage is composed of the following raw materials: 25-70 parts of the colloidal suspension of
所述悬浮型固体饮料由以下原料组成:亲水胶体5-30份、非变性II型胶原蛋白粉10-15份、低聚糖0-15份、鱼胶原蛋白肽10-20份、水解II型胶原蛋白10-20份、沙棘粉5-10份、柠檬酸0-10份、维生素C 0-5份、柠檬酸钠0-3份、姜黄0.1-1份、香精0-1份。The suspended solid beverage is composed of the following raw materials: 5-30 parts of hydrophilic colloids, 10-15 parts of non-denatured type II collagen powder, 0-15 parts of oligosaccharides, 10-20 parts of fish collagen peptides, and hydrolyzed II 10-20 parts of collagen type, 5-10 parts of sea buckthorn powder, 0-10 parts of citric acid, 0-5 parts of vitamin C, 0-3 parts of sodium citrate, 0.1-1 part of turmeric, 0-1 part of essence.
所述的亲水胶体为黄原胶、卡拉胶、结冷胶、魔芋胶、果胶、海藻酸钠或羧甲基纤维素钠中的一种或多种;Described hydrophilic colloid is one or more in xanthan gum, carrageenan, gellan gum, konjac gum, pectin, sodium alginate or sodium carboxymethyl cellulose;
所述的低聚糖为菊粉、低聚果糖、低聚麦芽糖、低聚木糖中的一种或多种。The oligosaccharide is one or more of inulin, fructo-oligosaccharide, malt-oligosaccharide and xylo-oligosaccharide.
一种胶体悬浮液的制备方法,包括以下步骤:A preparation method of colloidal suspension, comprising the following steps:
a.配料:按配比在无菌水中加入非变性II型胶原蛋白粉、低聚糖、水解II型胶原蛋白,在3000-5000rpm条件下剪切分散10-60min,得到粗分散液;a. Ingredients: add non-denatured type II collagen powder, oligosaccharides, and hydrolyzed type II collagen in sterile water according to the proportions, shear and disperse at 3000-5000rpm for 10-60min to obtain a coarse dispersion;
b.高压均质:粗分散液进入高压均质机,在20MPa-60 MPa均质压力下循环2-5次,得到分散液,温度控制在18-28℃;b. High pressure homogenization: the coarse dispersion liquid enters the high pressure homogenizer, and circulates 2-5 times under the homogenization pressure of 20MPa-60MPa to obtain the dispersion liquid, and the temperature is controlled at 18-28℃;
c.溶胶:将亲水胶体按1:50-1:100料液比添加至80℃以上热水中,在3000-8000rpm条件下剪切5-30min,使其充分溶胀,冷却至30-40℃,得到胶体溶液;c. Sol: Add the hydrophilic colloid to hot water above 80°C at a material-to-liquid ratio of 1:50-1:100, shear at 3000-8000rpm for 5-30min to fully swell, and cool to 30-40 ℃ to obtain a colloidal solution;
d.混合:将步骤b分散液与步骤c胶体溶液混合均匀,得到混合液;d. Mixing: mixing the dispersion liquid in step b and the colloidal solution in step c uniformly to obtain a mixed liquid;
e.高压微射流均质:混合液进入高压微射流均质机,在80-150MPa条件下均质1-3次,控制温度在28-38℃,得到悬浮液;e. High-pressure micro-jet homogenization: the mixed liquid enters the high-pressure micro-jet homogenizer, and is homogenized 1-3 times under the condition of 80-150MPa, and the temperature is controlled at 28-38°C to obtain a suspension;
f.冷却静置:将悬浮液静置,冷却,得到凝胶;f. Cooling and standing: the suspension is allowed to stand and cool to obtain a gel;
g.剪切凝胶:将凝胶在1000-5000rpm下剪切分散,得到胶体悬浮液。g. Shear gel: The gel is sheared and dispersed at 1000-5000 rpm to obtain a colloidal suspension.
一种悬浮型固体饮料的制备方法,包括以下步骤:A preparation method of a suspended solid beverage, comprising the following steps:
1)将权利要求1所述的胶体悬浮液进行冷冻干燥处理,预冻温度-80℃至-20℃、干燥时间24-72h,粉碎时间5-15min、撞击速度为10-20次·s-1、粉碎温度控制在5-18℃,得到平均粒径小于40μm的胶体悬浮液除去水分的产品,即非变性II型胶原蛋白的胶体悬浮液冻干粉;1) The colloidal suspension described in
2)按照配比称取步骤1)胶体悬浮液冻干粉及原料,按照原料重量由轻到重逐级梯度混合,使混合程度更加均匀;充分混合均匀后,在无菌环境下以复合膜进行分装,得到悬浮型固体饮料。2) Weigh step 1) colloidal suspension freeze-dried powder and raw materials according to the proportion, and mix them in a step-by-step gradient from light to heavy according to the weight of the raw materials to make the mixing degree more uniform; Carry out sub-packaging to obtain a suspended solid beverage.
一种悬浮型固体饮料的制备方法,包括以下步骤:A preparation method of a suspended solid beverage, comprising the following steps:
1)按配比称取原料鱼胶原蛋白肽、沙棘粉、柠檬酸、维生素C、柠檬酸钠、姜黄和香精,充分混合均匀后加入权利要求1所述的胶体悬浮液中,搅拌均匀,得到混合液;1) Weigh raw fish collagen peptide, sea buckthorn powder, citric acid, vitamin C, sodium citrate, turmeric and essence by proportioning, add in the colloidal suspension according to claim 1 after fully mixing, stir to obtain mixed liquid;
2)将步骤1)混合液进行冷冻干燥,预冻温度-60℃,干燥时间24-72h,粉碎时间5-15min、撞击速度为10-20次·s-1、粉碎温度控制在5-18℃,粉碎后在无菌环境下以复合膜进行分装,得到悬浮型固体饮料。2) Freeze-dry the mixed solution in step 1), the pre-freezing temperature is -60°C, the drying time is 24-72h, the pulverization time is 5-15min, the impact speed is 10-20 times·s -1 , and the pulverization temperature is controlled at 5-18 ℃, pulverized and subpackaged with a composite film in a sterile environment to obtain a suspension-type solid beverage.
一种悬浮型固体饮料的制备方法,包括以下步骤:A preparation method of a suspended solid beverage, comprising the following steps:
1)将非变性II型胶原蛋白粉与亲水胶体按照质量比1:9-9:1混合进行粉碎,粉碎时间15-120min,转速100-500r/min,粉碎温度5-18℃,制得平均粒径小于40μm的非变性II型胶原蛋白/亲水胶体胶体复合粉;1) The non-denatured type II collagen powder and the hydrophilic colloid are mixed according to the mass ratio of 1:9-9:1 and pulverized. Non-denatured type II collagen/hydrocolloid colloid composite powder with an average particle size of less than 40 μm;
2)按照配比称取含非变性II型胶原蛋白/亲水胶体胶体复合粉及剩余原料,按照原料重量由轻到重逐级梯度混合,充分混合均匀后,在无菌环境下以复合膜进行分装,得到悬浮型固体饮料。2) Weigh the non-denatured type II collagen/hydrocolloid colloid composite powder and the remaining raw materials according to the ratio, mix them in a step-by-step gradient according to the weight of the raw materials, and mix them thoroughly. Carry out sub-packaging to obtain a suspended solid beverage.
本发明的有益效果在于:The beneficial effects of the present invention are:
1.本发明制备的含非变性II型胶原蛋白的胶体悬浮液,均匀透明,悬浮稳定性好;含非变性II型胶原蛋白的悬浮型固体饮料能用35℃以下的冷水冲调,避免温度高于35℃以上引起的II型胶原蛋白的热变性,拥有较好的速溶性、悬浮性、口感清爽、营养丰富、具有优异的保健成分,有利于骨关节健康。1. The colloidal suspension containing non-denatured type II collagen prepared by the present invention is uniform and transparent, and has good suspension stability; the suspension-type solid beverage containing non-denatured type II collagen can be prepared with cold water below 35° C. The thermal denaturation of type II collagen caused by higher than 35°C has good instant solubility, suspension, refreshing taste, rich nutrition, excellent health care ingredients, and is beneficial to bone and joint health.
2.本发明制备的含非变性II型胶原蛋白的胶体悬浮液,可使水不溶的非变性II型胶原蛋白稳定悬浮,均匀透明,改善了非变性II型胶原蛋白的悬浮性。2. The colloidal suspension containing the non-denatured type II collagen prepared by the present invention can stably suspend the water-insoluble non-denatured type II collagen, uniform and transparent, and improves the suspension of the non-denatured type II collagen.
3.本发明制备的含非变性II型胶原蛋白悬浮型固体饮料,风味佳,速溶性、悬浮稳定性好,具有一定的保健成分,有利于骨关节健康。3. The non-denatured type II collagen-containing suspension-type solid beverage prepared by the present invention has good flavor, instant solubility, good suspension stability, and has certain health-care ingredients, which is beneficial to bone and joint health.
4.本发明制备的含非变性II型胶原蛋白悬浮型固体饮料可采用冷水冲调,避免了高温导致的非变性II型胶原蛋白变性,最大程度保持其功能活性,增加了非变性II型胶原蛋白在食品领域的应用范围,填补了保健食品领域针对非变性II型胶原蛋白产品只可生产片剂或胶囊而无其他类型产品的空白,拓宽了非变性II型胶原蛋白的应用范围。4. The non-denatured type II collagen-containing suspended solid beverage prepared by the present invention can be prepared with cold water, which avoids the denaturation of non-denatured type II collagen caused by high temperature, maintains its functional activity to the greatest extent, and increases non-denatured type II collagen. The application range of protein in the food field fills the gap in the health food field that only tablets or capsules can be produced for non-denatured type II collagen products and no other types of products, and broadens the application range of non-denatured type II collagen.
附图说明Description of drawings
图1为实施例2制备的含非变性II型胶原蛋白悬浮型固体饮料冲调情况;Fig. 1 is the preparation situation of the suspension-type solid beverage containing non-denatured type II collagen prepared in Example 2;
图2为实施例3制备的含非变性II型胶原蛋白悬浮型固体饮料冲调情况;Fig. 2 is the preparation situation of the suspension type solid beverage containing non-denatured type II collagen prepared in Example 3;
图3为实施例4制备的含非变性II型胶原蛋白悬浮型固体饮料冲调情况;Fig. 3 is the preparation situation of the suspension-type solid beverage containing non-denatured type II collagen prepared in Example 4;
图4-a、4-b、4-c和4-d分别为实施例5中Turbiscan Lab测定的含非变性II型胶原蛋白胶体悬浮液及对照组背散射光强度随时间的变化规律;Figures 4-a, 4-b, 4-c and 4-d respectively show the variation law of the backscattered light intensity with time of the non-denatured type II collagen-containing colloidal suspension and the control group measured by Turbiscan Lab in Example 5;
图5为实施例5中含非变性II型胶原蛋白胶体悬浮液及对照组TSI值随时间的变化曲线;Fig. 5 is the change curve of TSI value with time of non-denatured type II collagen colloid suspension and control group in Example 5;
图6为实施例5中含非变性II型胶原蛋白胶体悬浮液及对照组粒径分布情况;Fig. 6 is the particle size distribution of non-denatured type II collagen colloid suspension and control group in Example 5;
图7为实施例5中含非变性II型胶原蛋白胶体悬浮液贮藏30d前的状态Figure 7 shows the state of the colloidal suspension containing non-denatured type II collagen in Example 5 before storage for 30 days
图8为实施例5中含非变性II型胶原蛋白胶体悬浮液贮藏30d后的状态。8 shows the state of the non-denatured type II collagen-containing colloid suspension in Example 5 after storage for 30 days.
具体实施方式Detailed ways
以下结合附图和具体实施例对本发明作进一步的详细说明:The present invention will be described in further detail below in conjunction with the accompanying drawings and specific embodiments:
实施例1Example 1
一种非变性II型胶原蛋白的胶体悬浮液及其制备方法A kind of colloidal suspension of non-denatured type II collagen and preparation method thereof
原料及配比:2-10份非变性II型胶原蛋白粉、1-5份亲水胶体、1-3份低聚糖、1-5份水解II型胶原蛋白,余量用水补充至100份。Raw materials and proportions: 2-10 parts of non-denatured type II collagen powder, 1-5 parts of hydrophilic colloid, 1-3 parts of oligosaccharides, 1-5 parts of hydrolyzed type II collagen, and the rest to 100 parts with water .
非变性II型胶原蛋白的胶体悬浮液的制备方法如下:A colloidal suspension of native type II collagen was prepared as follows:
a.配料:在1000mL无菌水中加入30g含非变性II型胶原蛋白粉、15g菊粉、16g份水解II型胶原蛋白,在3000rpm条件下剪切分散15min,得到粗分散液。a. Ingredients: add 30g of non-denatured type II collagen powder, 15g of inulin and 16g of hydrolyzed type II collagen into 1000mL sterile water, shear and disperse at 3000rpm for 15min to obtain a coarse dispersion.
b.高压均质:粗分散液进入高压均质机,在35MPa均质压力下循环2次,得到分散液,温度控制在28℃;b. High-pressure homogenization: the coarse dispersion liquid enters the high-pressure homogenizer, and is circulated twice under the homogenization pressure of 35MPa to obtain the dispersion liquid, and the temperature is controlled at 28°C;
c.溶胶:在1000mL无菌水中加入10g黄原胶:结冷胶:魔芋胶=4:3:3混合胶体,在无菌环境下,加入80℃热水,在5000rpm条件下剪切分散10min,使其充分溶胀,冷却至35℃,得到胶体溶液;c. Sol: add 10g xanthan gum to 1000mL sterile water: gellan gum: konjac gum=4:3:3 mixed colloid, add hot water at 80°C in a sterile environment, shear and disperse at 5000rpm for 10min , make it fully swollen, and cooled to 35 °C to obtain a colloidal solution;
d.混合:在35℃将步骤b所得分散液与步骤c所得胶体溶液混合均匀,得到混合液;d. Mixing: uniformly mix the dispersion obtained in step b and the colloidal solution obtained in step c at 35°C to obtain a mixed solution;
e.高压微射流均质:将混合液在高压微射流均质机质,在100MPa条件下均质2次,控制温度在30℃,得到悬浮液;e. High-pressure micro-jet homogenization: homogenize the mixed solution in a high-pressure micro-jet homogenization machine for 2 times under the condition of 100MPa, and control the temperature at 30°C to obtain a suspension;
f.冷却静置:将混合分散液静置,冷却,得到具有一定胶凝强度的水凝胶;f. Cooling and standing: standing the mixed dispersion and cooling to obtain a hydrogel with a certain gel strength;
g.剪切凝胶:将凝胶在2000rpm下剪切分散,得到胶体悬浮液。g. Shear gel: The gel is sheared and dispersed at 2000 rpm to obtain a colloidal suspension.
实施例2Example 2
一种含非变性II型胶原蛋白的悬浮型固体饮料及其制备方法A kind of suspension type solid beverage containing non-denatured type II collagen and preparation method thereof
称取含非变性II型胶原蛋白的胶体悬浮液冻干粉25份、菊粉15份、鱼胶原蛋白肽15份、水解II型胶原蛋白20份、沙棘粉10份、柠檬酸5份、维生素C2份、柠檬酸钠2份、姜黄1份、香精5份。Weigh 25 parts of lyophilized powder of colloidal suspension containing non-denatured type II collagen, 15 parts of inulin, 15 parts of fish collagen peptide, 20 parts of hydrolyzed type II collagen, 10 parts of sea buckthorn powder, 5 parts of citric acid,
制备方法包括含非变性II型胶原蛋白的胶体悬浮液冻干粉制备和固体饮料调配。制备方法如下:The preparation method includes the preparation of lyophilized powder of colloidal suspension containing non-denatured type II collagen and the preparation of solid beverage. The preparation method is as follows:
1)含非变性II型胶原蛋白的胶体悬浮液冻干粉的制备1) Preparation of lyophilized powder of colloidal suspension containing non-denatured type II collagen
同实施例1制备非变性II型胶原蛋白的胶体悬浮液,将该胶体悬浮液置于-80℃冰箱预冻3h,通过冷冻干燥设备进行干燥、干燥时间48h。The colloidal suspension of non-denatured type II collagen was prepared in the same manner as in Example 1, and the colloidal suspension was pre-frozen in a -80° C. refrigerator for 3 hours, and dried by freeze drying equipment for 48 hours.
2)固体饮料调配2) Preparation of solid beverages
按照配比称取含非变性II型胶原蛋白的胶体悬浮液冻干粉及其他所需原料,按照重量比接近的原料先混合,从重量较轻的原料开始进行逐级梯度混合,混合顺序依次为:姜黄、维生素C、柠檬酸钠、柠檬酸、香精、沙棘粉、菊粉、鱼胶原蛋白肽、水解II型胶原蛋白、含非变性II型胶原蛋白的胶体悬浮液冻干粉;充分混合均匀后,在无菌条件下以复合膜进行分装,得到含非变性II型胶原蛋白固体饮料,规格为5g/袋。Weigh the lyophilized powder of colloidal suspension containing non-denatured type II collagen and other required raw materials according to the ratio, mix the raw materials with close weight ratios first, and start from the lighter weight raw materials for step-by-step gradient mixing, and the mixing order is in turn For: turmeric, vitamin C, sodium citrate, citric acid, essence, sea buckthorn powder, inulin, fish collagen peptides, hydrolyzed type II collagen, colloidal suspension lyophilized powder containing non-denatured type II collagen; well mixed After homogenization, the composite film is used for sub-packaging under aseptic conditions to obtain a solid beverage containing non-denatured type II collagen with a specification of 5g/bag.
食用方法:用100mL 25℃水冲调,含非变性II型胶原蛋白悬浮型固体饮料在0s、10s、20s和30s的冲调情况变化照片如图1所示,充分搅拌30s内即可得到胶体悬浮液饮用。How to eat: Mix with 100mL of 25℃ water. The photos of the change of the mixing situation of the non-denatured type II collagen-containing suspension solid beverage at 0s, 10s, 20s and 30s are shown in Figure 1, and the colloid can be obtained within 30s after fully stirring. Suspension for drinking.
实施例3Example 3
一种含非变性II型胶原蛋白的悬浮型固体饮料及其制备方法A kind of suspension type solid beverage containing non-denatured type II collagen and preparation method thereof
原料及配比:非变性II型胶原蛋白8份、黄原胶12份、菊粉30份、鱼胶原蛋白肽20份、水解II型胶原蛋白20份、沙棘粉5份、姜黄素5份。Raw materials and proportions: 8 parts of non-denatured type II collagen, 12 parts of xanthan gum, 30 parts of inulin, 20 parts of fish collagen peptide, 20 parts of hydrolyzed type II collagen, 5 parts of sea buckthorn powder, and 5 parts of curcumin.
制备方法包括含非变性II型胶原蛋白的胶体悬浮液制备和固体饮料调配。制备方法如下:The preparation method includes the preparation of a colloidal suspension containing non-denatured type II collagen and the preparation of a solid beverage. The preparation method is as follows:
1)含非变性II型胶原蛋白的胶体悬浮液的制备1) Preparation of colloidal suspension containing native type II collagen
同实施例1。Same as Example 1.
2)固体饮料调配2) Preparation of solid beverages
按照配比称取除非变性II型胶原蛋白粉以外的其他所需原料,充分混合均匀后加入含非变性II型胶原蛋白的胶体悬浮液中,搅拌均匀,将该混合液进行冷冻干燥,预冻温度-60℃、干燥时间48h,干燥后进行粉碎,粉碎时间10min、撞击速度为20次·s-1,粉碎温度18℃,过200目筛,在无菌环境下以复合膜进行分装,得到含非变性II型胶原蛋白固体饮料。Weigh other required raw materials other than non-denatured type II collagen powder according to the proportion, mix well and add them to the colloidal suspension containing non-denatured type II collagen, stir evenly, freeze-dry the mixture and pre-freeze it The temperature is -60°C, the drying time is 48h, and then pulverized after drying. The pulverization time is 10min, the impact speed is 20 times·s -1 , the pulverization temperature is 18°C, and it is passed through a 200-mesh sieve. A solid beverage containing non-denatured type II collagen was obtained.
食用方法:用100mL 30℃水冲调,含非变性II型胶原蛋白悬浮型固体饮料在0s、10s、20s和30s的冲调情况变化照片如图2所示,充分搅拌30s内即可得到胶体悬浮液饮用。Edible method: Use 100mL of 30 ℃ water to mix, and the photos of the change of the mixing situation of the non-denatured type II collagen suspension solid beverage at 0s, 10s, 20s and 30s are shown in Figure 2, and the colloid can be obtained within 30s of thorough stirring. Suspension for drinking.
实施例4Example 4
一种含非变性II型胶原蛋白的悬浮型固体饮料及其制备方法A kind of suspension type solid beverage containing non-denatured type II collagen and preparation method thereof
原料及配比:非变性II型胶原蛋白8份、黄原胶12份、菊粉30份、鱼胶原蛋白肽20份、水解II型胶原蛋白20份、沙棘粉5份、姜黄素5份。Raw materials and proportions: 8 parts of non-denatured type II collagen, 12 parts of xanthan gum, 30 parts of inulin, 20 parts of fish collagen peptide, 20 parts of hydrolyzed type II collagen, 5 parts of sea buckthorn powder, and 5 parts of curcumin.
制备方法包括非变性II型胶原蛋白/亲水胶体胶体复合粉的制备和固体饮料调配,具体如下:The preparation method includes the preparation of non-denatured type II collagen/hydrocolloid colloid composite powder and the preparation of solid beverages, and the details are as follows:
1)非变性II型胶原蛋白/亲水胶体胶体复合粉的制备方法1) Preparation method of non-denatured type II collagen/hydrocolloid colloid composite powder
按照2:3比例称取非变性II型胶原蛋白和黄原胶,混合均匀后倒入高能纳米冲击磨进行研磨,研磨时间6h,冷却温度2℃,机器功率4kw,转速400r/min,研磨介质氧化锆陶瓷球,研磨后得到非变性II型胶原蛋白/亲水胶体胶体复合粉。Weigh non-denatured type II collagen and xanthan gum in a ratio of 2:3, mix them evenly, and pour into a high-energy nano-impact mill for grinding. The grinding time is 6h, the cooling temperature is 2°C, the machine power is 4kw, the speed is 400r/min, and the grinding medium Zirconia ceramic balls are ground to obtain non-denatured type II collagen/hydrocolloid colloid composite powder.
2)固体饮料调配2) Preparation of solid beverages
按照配比称取称取所需原料,按照沙棘粉、姜黄素、鱼胶原蛋白肽、水解II型胶原蛋白、菊粉、非变性II型胶原蛋白/亲水胶体胶体复合粉的顺序进行逐级梯度混合,充分混合均匀后,在无菌条件下以复合膜进行分装,得到含非变性II型胶原蛋白固体饮料,规格为5g/袋。Weigh the required raw materials according to the proportion, and proceed step by step in the order of sea buckthorn powder, curcumin, fish collagen peptide, hydrolyzed type II collagen, inulin, non-denatured type II collagen/hydrocolloid colloid composite powder Gradient mixing, after fully mixing and evenly mixing, under aseptic conditions, the composite membrane is used for sub-packaging to obtain a non-denatured type II collagen-containing solid beverage with a specification of 5g/bag.
食用方法:用100mL 10℃水冲调,含非变性II型胶原蛋白悬浮型固体饮料在0s、10s、20s和30s的冲调情况变化照片如图3所示,充分搅拌30s内即可得到胶体悬浮液饮用。Edible method: use 100mL of 10 ℃ water to mix, and the photos of the change of the mixing situation of the non-denatured type II collagen-containing suspension solid beverage at 0s, 10s, 20s and 30s are shown in Figure 3, and the colloid can be obtained within 30s of full stirring. Suspension for drinking.
实施例5Example 5
非变性II型胶原蛋白的胶体悬浮液稳定性及贮藏性研究Study on the Stability and Storage of Colloidal Suspension of Non-denatured Type II Collagen
以实施例1所得产品为受试样品,同时设置三个对照组,如表1所示,通过Turbiscan Lab稳定性分析仪测试其稳定性,将四种样品分别在25℃条件下测量其透射光和背散射光强度随时间的变化曲线。首先,设定所需的测试温度,并将待测样品置于样品池中,样品高度为0-42mm,在该温度下平衡30min,之后采用连续扫描方式,每隔25s采集一组数据,连续扫描30min,可以得到透射光和背散射光强度随时间的变化曲线。测试结果透射光信号几乎为0,因此,分析背散射光强度随时间的变化规律如图4-a至图4-d,计算并绘制在指定测量时间内的TSI值随时间的变化曲线如图5所示。Taking the product obtained in Example 1 as the test sample, and setting three control groups at the same time, as shown in Table 1, the stability was tested by the Turbiscan Lab stability analyzer, and the transmission of the four samples was measured at 25 ° C respectively. Light and backscattered light intensity versus time. First, set the required test temperature, put the sample to be tested in the sample cell, the sample height is 0-42mm, equilibrate at this temperature for 30min, and then use the continuous scanning method to collect a set of data every 25s, continuously After scanning for 30 min, the curve of the intensity of transmitted light and backscattered light with time can be obtained. The transmitted light signal is almost 0 in the test result. Therefore, the variation law of backscattered light intensity with time is analyzed as shown in Figure 4-a to Figure 4-d, and the variation curve of TSI value with time within the specified measurement time is calculated and drawn as shown in Figure 4-d. 5 shown.
从图中可知,实验组和对照组样品稳定性有显著差异。对照组三者的ΔBS值随时间的推移变化趋势相近,即底部出现沉淀,中间波动较大,顶部出现澄清,可知对照组的样品稳定性不好。相比较而言,未经处理的非变性II型胶原蛋白稳定性最差,ΔBS图像在底部出现较为明显的凸起,表明沉淀量较多,且顶部出现明显的凹峰,表明顶部澄清,再次证明了未经处理的非变性II型胶原蛋白在水中的溶解性极差,不利于作为液体制剂使用(如图4-a);若单纯加胶适量的胶溶解,与非变性II型胶原蛋白制成混悬液,也并不能较好的改变其分散性(如图4-b),仍会产生沉淀与分层现象;经过上述方法处理后的非变性II型胶原蛋白,凸峰发生了右移(如图4-c),说明样品分散性增强,沉淀有所减少,该方法对改善非变性II型胶原蛋白悬浮型有效果,但仍会有上层澄清现象出现。实验组的数据表明,经处理的非变性II型胶原蛋白胶体悬浮液ΔBS图像底部无明显凸起,中间断ΔBS变化情况不显著,顶部无明显分层现象,均一性稳定性好(如图4-d)。最后,为了表征样品整体稳定性大小,可由Turbiscan Easysoft软件定义的稳定性动力学指数(turbiscan stability index,TSI)比较各体系的相对稳定性,结果示于图5;TSI值越小,体系越稳定,TSI结果与上述分析一致,表明了该方法的独特性与有效性。It can be seen from the figure that there is a significant difference in the stability of the samples in the experimental group and the control group. The change trend of the three ΔBS values in the control group is similar with the passage of time, that is, precipitation at the bottom, large fluctuation in the middle, and clarification at the top, it can be seen that the stability of the samples in the control group is not good. In comparison, the untreated non-denatured type II collagen had the worst stability, and the ΔBS image showed a more obvious bulge at the bottom, indicating more sedimentation, and a clear concave peak at the top, indicating that the top was clear, and again It is proved that the untreated non-denatured type II collagen has extremely poor solubility in water, which is not conducive to use as a liquid preparation (as shown in Figure 4-a). Even if it is made into a suspension, its dispersibility cannot be changed well (as shown in Figure 4-b), and precipitation and stratification will still occur; for the non-denatured type II collagen treated by the above method, a convex peak occurs. Shifting to the right (as shown in Figure 4-c) indicates that the dispersibility of the sample is enhanced and the sedimentation is reduced. This method is effective in improving the suspension of non-denatured type II collagen, but the upper layer will still be clarified. The data of the experimental group showed that there was no obvious bulge at the bottom of the ΔBS image of the treated non-denatured type II collagen colloid suspension, no significant change in ΔBS in the middle, no obvious delamination at the top, and good uniformity and stability (as shown in Figure 4). -d). Finally, in order to characterize the overall stability of the sample, the relative stability of each system can be compared with the turbiscan stability index (TSI) defined by Turbiscan Easysoft software. The results are shown in Figure 5; the smaller the TSI value, the more stable the system is. , TSI results are consistent with the above analysis, indicating the uniqueness and effectiveness of this method.
表1实验组与对照组设定方法Table 1 Setting method of experimental group and control group
同样,以实施例1所得产品作为实验组,如表1所示,制备三个样品作为对照组,通过静态光散射粒度仪测定其粒径分布,结果示于图6,结果表明,该方法可以明显减小体系粒径,且实验组的粒径分布呈较“瘦”单峰形状,更有利于体系的分散稳定性,而对照组粒径较大,且峰面积较宽,不利于体系的稳定,与上述结果一致。Similarly, taking the product obtained in Example 1 as the experimental group, as shown in Table 1, three samples were prepared as the control group, and the particle size distribution was measured by a static light scattering particle size analyzer. The results are shown in Figure 6. The results show that this method can The particle size of the system is significantly reduced, and the particle size distribution of the experimental group is in a “skinny” single-peak shape, which is more conducive to the dispersion stability of the system, while the control group has a larger particle size and a wider peak area, which is not conducive to the stability of the system. stable, consistent with the above results.
将实验组样品分别置于pH3.8、pH5的柠檬酸溶液中、及可溶性固形物含量为10°Brix蔗糖水溶液中,于35℃、避光条件下进行30d的贮藏实验。分别于储存前后取样进行检验。检验项目为感官分析,试验结果如表2所示。The samples of the experimental group were placed in citric acid solution with pH 3.8 and
表2含非变性II型胶原蛋白的胶体悬浮液稳定性试验结果Table 2 Stability test results of colloidal suspensions containing non-denatured type II collagen
Turbiscan Lab稳定性及粒径分布的测试结果表明,该胶体悬浮液具有良好的稳定性及粒径分布。以储藏前和储藏后的非变性II型胶原蛋白胶体悬浮液的状态图片(示于图7和图8)作为对照,稳定性试验结果表明,该胶体悬浮液可在低酸、高酸及中性环境且低于35℃条件下避光保存30天,仍保持良好稳定性。Turbiscan Lab stability and particle size distribution test results show that the colloidal suspension has good stability and particle size distribution. Taking the state pictures of the non-denatured type II collagen colloidal suspension before and after storage (shown in Figure 7 and Figure 8) as a control, the stability test results show that the colloidal suspension can be in low acid, high acid and medium. It can be stored for 30 days in a sexual environment and below 35°C in the dark, and it still maintains good stability.
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