CN116326782A - Protein calcium and preparation method thereof - Google Patents

Abstract

The invention discloses protein calcium and a preparation method thereof. Alpha-lactalbumin is dissolved to prepare protein solution; soluble calcium salt is weighed to prepare calcium solution; protein solution and calcium solution are mixed and stirred to form protein calcium containing bound calcium solution; weighing calcium citrate, adding the above reaction solution, stirring and ultrasonication, so that the calcium citrate is more fully dispersed to form a suspension; spray-dried to prepare a powder. The invention selects a protein that can not only wrap insoluble calcium, but also combine with calcium ions, and the production steps are relatively simple, so that the production plan and products can be implemented; the calcium content of the product is increased, and the absorption and utilization of calcium is smooth two-sided effects.

Description

A kind of calcium protein and preparation method thereof

technical field

The invention relates to protein calcium and its preparation method, in particular to protein-bound calcium and embedded free calcium

Background technique

Calcium intake is critical for maintaining normal bone density in children/adolescents, achieving high peak bone mass, reducing fractures, and reducing the risk of osteoporosis in old age. Due to the lack of calcium in the human body at this stage, the research and development of calcium preparations has attracted more and more people's attention and attention.

At present, increasing protein intake while supplementing calcium will have a positive correlation effect on the growth of bone tissue, but sufficient protein intake while supplementing calcium will have a good effect on bone improvement. For raw materials with low calcium content, a larger dose is required to consume the same amount of calcium element.

Chinese invention application patent (CN201510094700.6) discloses "a new type of calcium enhancer based on insoluble calcium and food-derived protein complex and its preparation and characterization method". Calcium is dispersed in water to form a suspension, and then mixed according to the mass ratio of protein and insoluble calcium of 2:1 to 1:200, the mixed solution after the reaction is separated by centrifugation or standing, and the obtained precipitate is rinsed and redispersed. Spray-drying or freeze-drying treatment to obtain insoluble calcium-protein composite powder. This method avoids the problems of poor product taste and high preparation cost caused by adding additional stabilizers to stabilize insoluble calcium salts, but it cannot meet the high utilization and high absorption of protein-bound calcium; moreover, it cannot achieve the effect of gradual release of calcium sources. The purpose of the present invention is to overcome the deficiencies of the prior art and develop a calcium protein product with safe raw materials, stable performance, high calcium content, good absorption performance and simple preparation process.

Contents of the invention

The object of the present invention is to provide a method for preparing calcium proteinate in view of the deficiencies of the prior art, (1) dissolving α-lactalbumin to prepare protein solution;

(2) Take by weighing soluble calcium salt, prepare calcium solution;

(3) The protein solution is mixed with the calcium solution and stirred to form a protein-calcium solution containing bound calcium;

(4) take calcium citrate, add above-mentioned reaction solution, stir, ultrasonic, make calcium citrate disperse more fully, form suspension;

(5) Spray drying and preparing into powder.

Further, the mass concentration of the α-lactalbumin solution is 2-30% (w/w), further 8-12% (w/w), further 10% (w/w).

Further, the soluble calcium salt is calcium chloride or calcium lactate, such as L-calcium lactate.

Further, the mass concentration of the calcium solution is 0.1-5%, further 0.5-1.5%, and further 1%.

Further, the mixing mass ratio of protein solution and calcium solution is (1-5):(5:1), further 1:1.

Further, the stirring condition of protein liquid and calcium solution is 0-35°C, preferably 10-30°C, more preferably 20-25°C.

Further, the protein solution and the calcium solution are mixed and stirred for 0.5min-2h, for example, 30min.

Further, the ultrasonication time of the calcium citrate and the reaction solution is more than 2 minutes, for example, 5 minutes, 10 minutes, 20 minutes.

Further, spray drying conditions: air inlet temperature 185-195°C, air outlet temperature 80-90°C, creep speed 10-50rpm.

The present invention also provides protein calcium, which is prepared by the above-mentioned method.

The present invention also provides protein calcium, which contains a combination of α-lactalbumin and calcium, and insoluble calcium wrapped by α-lactalbumin.

Further, the insoluble calcium encapsulated by α-lactalbumin is calcium citrate and/or calcium carbonate.

Beneficial effect:

(1) On the one hand, because the product has protein-bound calcium and encapsulated calcium citrate at the same time, the calcium content of the product is increased; The large amount of calcium releases and absorbs slowly, making the absorption and utilization of calcium more gentle.

(2) The present invention selects a protein that can not only wrap insoluble calcium, but also combine with calcium ions, and the production steps are relatively simple, so that the production plan and products can be implemented; The absorption and utilization of calcium have two effects.

(3) Compared with the calcium citrate suspension, the externally bound calcium shell has better stability and dispersibility, which improves the effect of absorption and utilization.

Terminology Explanation

α-lactalbumin, or α-LA, contains a tightly bound Ca ²⁺ that strongly affects stability and structure; some α-lactalbumins are glycoproteins, carrying a single, typically linked glycan Some α-lactalbumin Proteins, which have a relatively high proportion of glycosylated molecules, should be understood as α-lactalbumin and derivatives of α-lactalbumin, which are all within the protection scope of this patent.

Description of drawings

Fig. 1 is the particle size situation of protein calcium;

Figure 2 is the scanning electron microscope microstructure;

Figure 3 shows the stability of the product after reconstitution.

Detailed ways

In order to facilitate the understanding of those skilled in the art, the present invention will be further described below in conjunction with the examples, and the contents mentioned in the embodiments are not intended to limit the present invention.

Example 1

Weigh 10g of α-LA, dissolve it in 90g of water, prepare a protein solution with a mass concentration of 10% (w/w), and at the same time, prepare a 0.6% (w/w) calcium chloride (dihydrate) solution, the two, etc. The mass was mixed and stirred at room temperature for 1h. Then weigh 8g of calcium citrate powder and add it to the above mixed solution, stir and ultrasonic for 5 minutes to form a suspension, which is spray-dried into powder, and the obtained calcium protein powder is white, D ₅₀ =7.78±0.25μm, the microstructure of scanning electron microscope Clear, the calcium citrate is basically wrapped completely, and it is a sandwich calcium structure. The suspension (2.5%, w/w) formed by rehydrating 0.25g of calcium protein powder was left to stand at room temperature for 1 hour, and the results showed that the stability of calcium proteinate was significantly better than that of calcium citrate.

Example 2

Weigh the α-LA of 10g, be dissolved in 90g water, prepare the protein solution of mass concentration 10% (w/w), meanwhile, prepare the L-calcium lactate (pentahydrate) solution (0.6% Calcium chloride (dihydrate) and 1.25% calcium lactate (pentahydrate, same calcium content), the two are mixed in equal mass, and stirred at room temperature for 1 hour. Then weigh 8g of calcium citrate powder and add it to the above mixture, stir and sonicate for 5 minutes to form a suspension, which is then spray-dried into powder. The calcium protein powder obtained is white and has good fluidity, D ₅₀ =6.79±0.05μm, scan Electron microscopy at an excitation voltage of 5kV and a magnification of 10,000 times observed a clear powder particle structure (see the third picture in Figure 2), and the calcium citrate was completely wrapped, which was a sandwich calcium structure. The suspension (2.5%, w/w) formed by rehydrating 0.25 g of the powder showed basically no delamination after standing at room temperature for 1 h, and its stability was better than that of calcium citrate.

Example 3

Weigh 10g of α-LA, dissolve it in 90g of water, prepare a protein solution with a mass concentration of 10% (w/w), and at the same time, prepare a 6% (w/w) L-calcium lactate solution, mix the two in equal mass, Stir at room temperature for 1 h. Then weigh 8g of calcium citrate powder and add it to the above mixed solution, stir and ultrasonic for _5min to form a suspension, and then spray-dry it into a powder. The powder particle structure observed at 5kV and 10,000 times magnification is clear (see the fourth picture in Figure 2), and the calcium citrate is basically completely wrapped, which is a sandwich calcium structure. But the particles are not complete, and the wrapping effect is not as good as that of Examples 1 and 2. The suspension (2.5%, w/w) formed by rehydrating 0.25 g of the powder had no obvious separation after standing at room temperature for 1 h.

Example 4

Weigh 10g of α-LA, dissolve it in 90g of water, prepare a protein solution with a mass concentration of 10% (w/w), and at the same time, prepare a 1.25% (w/w) L-calcium lactate solution, mix the two in equal mass, Stir at room temperature for 1 h. Then weigh 12g of calcium citrate powder and add it to the above mixture, stir and ultrasonic for 5min to form _a suspension, and spray-dry to form a powder. The calcium protein powder obtained is white and has good fluidity. Electron microscope at an excitation voltage of 5kV and a magnification of 10,000 times observed a clear powder particle structure (see the fifth picture in Figure 2), and the calcium citrate was completely wrapped, which was a sandwich calcium structure. The suspension (2.5%, w/w) that 0.25g powder is rehydrated forms, after standing 1h at room temperature, there is no delamination, and the stability is better, the same as the "shell" of the example 2 sample, and the calcium content is higher high.

As can be seen from Fig. 1, embodiments 1-4 correspond to 1-4 respectively, and 0 is the control group spray-dried under the same conditions of calcium citrate solution cloudy liquid. It can be seen from D ₅₀ that the particle size of protein calcium is much larger than that of calcium citrate solution; and there are differences in particle size between protein calcium, but the difference is not large.

As can be seen from Figure 2, the first picture is the control group spray-dried under the same conditions as the calcium citrate solution turbid liquid, and embodiments 1-4 correspond to the second to fifth pictures in Figure 2 respectively. It can be seen from the figure that the calcium protein powder has a clear particle structure and forms a complete or basically complete shell, which can wrap calcium citrate.

It can be seen from Figure 3 that there is basically no or no obvious layering after reconstitution of calcium proteinate, while calcium citrate quickly forms a precipitate.

Those skilled in the art can understand that, unless otherwise defined, all terms (including technical terms and scientific terms) used herein have the same meaning as commonly understood by those of ordinary skill in the art to which this invention belongs. It should also be understood that terms, such as those defined in commonly used dictionaries, should be understood to have meanings consistent with their meaning in the context of the prior art, and unless specifically defined as herein, are not intended to be idealized or overly Formal meaning to explain.

It should be understood that the above detailed description of the technical solution of the present invention with the aid of preferred embodiments is illustrative rather than restrictive. Those skilled in the art can modify the technical solutions recorded in each embodiment on the basis of reading the description of the present invention, or perform equivalent replacements for some of the technical features; and these modifications or replacements do not make the corresponding technical solutions Essentially deviate from the spirit and scope of the technical solutions of the various embodiments of the present invention.

Claims (10)

1. A preparation method of protein calcium, characterized in that, (1) alpha-lactalbumin is dissolved to prepare protein solution; (2) Take by weighing soluble calcium salt, prepare calcium solution; (3) The protein solution is mixed with the calcium solution and stirred to form a protein-calcium solution containing bound calcium; (4) take calcium citrate, add above-mentioned reaction solution, stir, ultrasonic, make calcium citrate disperse more fully, form suspension; (5) Spray drying and preparing into powder. 2. The method according to claim 1, wherein the mass concentration of the α-lactalbumin solution is 2 to 30% (w/w), further 8 to 12% (w/w), and further 10% (w/w). 3. The method of claim 1, wherein the soluble calcium salt is calcium chloride or calcium lactate, such as calcium L-lactate. 4. The method according to claim 1, characterized in that the mass concentration of the calcium solution is 0.1-5%, further 0.5-1.5%, further 1%. 5. The method according to claim 1, characterized in that the mixing mass ratio of protein solution and calcium solution is (1-5):(5:1), further 1:1. 6. The method according to claim 1, characterized in that the stirring condition of protein solution and calcium solution is 0-35°C, preferably 10-30°C, more preferably 20-25°C. 7. The method according to claim 1, wherein the protein solution and the calcium solution are mixed and stirred for 0.5min-2h, for example 30min; and / or Further, the ultrasonic time of calcium citrate and the reaction solution is more than 2 minutes, for example, 5 minutes, 10 minutes, 20 minutes; and / or Spray drying conditions: air inlet temperature 185~195℃, outlet air temperature 80~90℃, creep speed 10~50rpm. 8. A calcium protein, characterized in that it is prepared by the method of any one of claims 1-7. 9. A calcium protein, characterized by comprising a conjugate of α-lactalbumin and calcium, and insoluble calcium encapsulated by α-lactalbumin. 10. The protein calcium according to claim 9, characterized in that the insoluble calcium encapsulated by α-lactalbumin is calcium citrate and/or calcium carbonate.

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