阅读说明：本技术 一种由鹿骨制备谷氨酸螯合钙的方法 (Method for preparing calcium glutamate chelate from deer bone ) 是由 李峰 李倩 张振秋 于 2019-10-17 设计创作，主要内容包括：本发明公布一种由鹿骨制备谷氨酸螯合钙的方法,包括以下步骤：1)制备鹿骨粉：将新鲜梅花鹿鹿骨剔去肉、筋膜、骨髓,洗净,于烘箱105℃干燥至恒重,粉碎,过60目筛,并符合质量要求,即得梅花鹿骨粉；2)制备鹿骨螯合钙：将鹿骨粉与谷氨酸质量比按1:1~5的比例混合,加入水,调pH 6.0~8.0,60~70℃螯合；取上清液减压浓缩,加无水乙醇沉淀,沉淀物干燥粉碎,即得鹿骨谷氨酸螯合钙粉。发明方法简单,螯合率高、含钙量高,所制备的鹿骨-谷氨酸螯合钙粉,保留了原料药中的营养物质,如维生素D等,无副作用。(The invention discloses a method for preparing calcium glutamate chelate from deer bones, which comprises the following steps of 1) preparing deer bone meal, namely removing meat, fascia and bone marrow from fresh sika deer bones, cleaning, drying in an oven at 105 ℃ to constant weight, crushing, sieving by a 60-mesh sieve, and meeting the quality requirement to obtain the sika deer bone meal, 2) preparing the calcium glutamate chelate, namely mixing the deer bone meal and the glutamic acid according to the mass ratio of 1:1 ~ 5, adding water, adjusting the pH value to 6.0 ~ 8.0.0, chelating at 60 ~ 70 ℃, taking supernatant, concentrating under reduced pressure, adding absolute ethyl alcohol for precipitation, drying and crushing precipitates to obtain the deer bone calcium glutamate chelate powder.)

1. A method for preparing calcium glutamate chelate from deer bone comprises the following steps:

1) preparing deer bone powder: removing meat, fascia and bone marrow from fresh sika deer bone, cleaning, drying in oven at 105 deg.C to constant weight, pulverizing, sieving with 60 mesh sieve to obtain sika deer bone powder;

2) the deer bone calcium chelate is prepared by mixing deer bone powder and glutamic acid according to the mass ratio of 1:1 ~ 5, adding water, adjusting pH to 6.0 ~ 8.0.0, chelating at 60 ~ 70 deg.C, collecting supernatant, concentrating under reduced pressure, precipitating with anhydrous ethanol, drying precipitate, and pulverizing to obtain deer bone calcium glutamate chelate powder.

2. The method of claim 1, wherein in step (2), the chelation time is 50 ~ 70 min.

3. The method according to claim 1, wherein in the step (2), the precipitation temperature is 0 ~ 4 ℃, and the precipitation time is 12 ~ 24 h.

4. The method according to claim 1, characterized in that it comprises in particular the steps of:

1) preparing deer bone powder: removing meat, fascia and bone marrow from fresh sika deer bone, cleaning, drying in oven at 105 deg.C to constant weight, pulverizing, sieving with 60 mesh sieve to obtain sika deer bone powder;

2) the deer bone calcium chelate is prepared by mixing deer bone powder and glutamic acid according to the mass ratio of 1:1 ~ 5, adding water, adjusting the pH of the solution to 6.0 ~ 8.0.0 with NaOH, chelating at 60 ~ 70 ℃ for 50 ~ 70min, continuously stirring, centrifuging, collecting the supernatant, concentrating under reduced pressure, adding absolute ethanol, precipitating at 0 ~ 4 ℃ for 12 ~ 24h, drying the precipitate, and pulverizing to obtain the deer bone calcium glutamate chelate powder.

5. The method according to claim 1, characterized in that it comprises in particular the steps of:

1) preparing deer bone powder: removing meat, fascia and bone marrow from fresh sika deer bone, cleaning, drying in oven at 105 deg.C to constant weight, pulverizing, sieving with 60 mesh sieve to obtain sika deer bone powder;

2) preparing deer bone chelated calcium: mixing deer bone powder 1 part, glutamic acid 1 part, and distilled water 200 parts, and mixing with 1 mol/L^-1Adjusting the pH value of NaOH to be 7.0, and carrying out heat preservation and chelation at 70 ℃ for 60 min; filtering while hot, concentrating the filtrate under reduced pressure, adding anhydrous ethanol until the alcohol concentration is 90%, precipitating with ethanol at 4 deg.C for 12h, vacuum filtering, and drying the precipitate under reduced pressure to obtain calcium glutamate chelated powder.

Technical Field

The invention relates to a preparation method of a novel sika deer bone calcium glutamate chelated calcium as a bone calcium source, belonging to the technical field of medicine preparation.

Background

Calcium is a macro element with the largest demand of human body, and calcium deficiency can cause a plurality of diseases. Statistical analysis by the World Health Organization (WHO) indicated that 106 of the basic diseases in human 165 were associated with calcium deficiency. Such as osteoporosis, arteriosclerosis, senile dementia, etc. According to the fourth national nutrition survey result in China, the daily intake of calcium of adults in China is 390.6mg, and only 50% of the intake recommended by the Nutrition society is achieved.

The calcium supplement preparations sold in the market at present are mainly divided into three types, the first type is inorganic calcium, so-called first generation calcium supplement products, such as calcium carbonate, calcium oxide, calcium hydrophosphate and the like; the second type is organic acid calcium, so-called second generation calcium supplement products, such as calcium gluconate, calcium citrate, calcium lactate, etc.; the third type is organic calcium, so-called third generation calcium supplement products, such as amino acid chelated calcium. The first generation and the second generation calcium supplement products mostly have the problems of difficult dissolution, poor calcium absorption, excessive heavy metals and the like. In the third generation of calcium supplement products, calcium appears in the form of amino acid chelate, so that the solubility, the absorptivity and the bioavailability of the calcium are greatly improved, and the calcium supplement products are favored by the market.

The existing calcium sources for preparing amino acid chelated calcium mainly comprise two types, namely, inorganic calcium sources such as calcium hydroxide or calcium oxide are chelated with amino acid; the other is that organic calcium source, such as animal bone, is hydrolyzed by acid to obtain soluble calcium salt, which is chelated with amino acid. The former has the disadvantages that the raw material is inorganic calcium, which is not environment-friendly enough, and the reaction time is longer, the chelating rate is low, and the energy consumption is higher; the latter has the disadvantage that the acid hydrolysis of animal bones destroys organic components in the animal bones which are beneficial for calcium absorption, such as VD₂、VD₃And the like, the effective components in the raw materials cannot be fully utilized.

The bone calcium raw material used for amino acid chelated calcium is mainly used for edible animal bones such as cattle, sheep, fish and the like, while some medicinal animal bones such as deer bones are not fully utilized. The Chinese traditional medical ancient book famous medical records that the deer bone has the efficacy of 'mainly treating internal deficiency and continuing to stop injury', and is used for treating rheumatism, limb pain and cold arthralgia of bones and muscles; modern researches show that the deer bone contains rich amino acids and vitamin D components capable of promoting calcium absorption besides high calcium content (the calcium content is measured to be 17% in the research of the invention and is higher than that of other animal bone powder reported in literatures). However, in the existing deer raising industry in China, deer bones are discarded as byproducts, so that great waste is caused. If deer bones are used as an organic calcium source to prepare the deer bone amino acid chelated calcium, not only can calcium supplement products in the market be enriched and the absorption rate of the calcium supplement products be improved, but also a good foundation is laid for improving the value of the deer industry.

A method for preparing amino acid chelated calcium at home and abroad mainly comprises ① hydrolysis of protein in a water phase to prepare the amino acid chelated calcium, ② high-pressure fluid nano-milling technology, ③ microwave solid-phase synthesis, ④ ion exchange method, electrolysis method and the like, wherein the method ① is widely adopted because of easy realization of experimental conditions and simple process without expensive equipment, but has higher cost for hydrolyzing protein with enzyme, inorganic acid is used for destroying organic components in bone calcium source, the method ② is novel, quick chelation of amino acid and calcium is realized, product quality is stable, but required equipment is expensive, the method ③ chelation reaction time is shorter, energy consumption is less, pollution is less, efficiency is high, but requirements on equipment are higher, investment is larger, radiation can be generated in the operation process of a microwave acid hydrolysis reactor, the method ④ has the advantages of simple conditions, no pollution to the environment, low production cost, high conversion rate, high product purity, tedious operation process, long time consumption, large energy consumption and difficulty in selective ion permeation through membrane regeneration.

CN101648884A discloses a method for preparing compound amino acid chelated calcium from low-value fresh water fishbone, which comprises the steps of cleaning fishbone, cooking, soaking with sodium hydroxide, washing to neutrality, drying, crushing, extracting calcium from fishbone powder by acidolysis, chelating calcium ions in fishbone powder with compound amino acid, centrifuging to obtain clear liquid, washing with absolute ethyl alcohol twice, centrifuging to obtain precipitate, drying and crushing to obtain a compound amino acid chelated calcium product.

CN106187798A discloses a preparation method of amino acid nano-chelated calcium, which comprises the following steps of 1) mixing bone meal and hydrochloric acid, heating and hydrolyzing the mixture to obtain soluble calcium, 2) mixing the soluble calcium and amino acid according to the molar ratio of 1:1 to obtain a mixed solution, 3) adding 1.5% by weight of citric acid into the mixed solution, homogenizing the mixed solution by a homogenizer to ensure that the solid granularity in the mixed solution is below 30 micrometers, spraying the mixed solution into a high-pressure fluid nano mill for chelation to obtain a clear solution, and 4) drying the solution to obtain the amino acid nano-chelated calcium.

Disclosure of Invention

The invention aims to provide an optimal preparation process of the amino acid chelated calcium prepared from deer bones, which is safe, efficient, cheap and environment-friendly.

The purpose of the invention can be realized by the following technical scheme:

a method for preparing calcium glutamate chelate from deer bone comprises the following steps:

1) preparing deer bone powder: removing meat, fascia and bone marrow from fresh sika deer bone, cleaning, drying in oven at 105 deg.C to constant weight, pulverizing, sieving with 60 mesh sieve, and making into sika deer bone powder.

2) Preparing deer bone chelated calcium: mixing the deer bone powder and glutamic acid according to the mass ratio of 1: 1-5, adding water, adjusting the pH value to 6.0-8.0, and chelating at 60-70 ℃; concentrating the supernatant under reduced pressure, precipitating with anhydrous ethanol, drying the precipitate, and pulverizing to obtain Os Cervi calcium glutamate chelated powder.

In the step (2), the chelating time is 50-70 min.

In the step (2), the precipitation temperature is 0-4 ℃, and the precipitation time is 12-24 hours.

A method for preparing calcium glutamate chelate from deer bones specifically comprises the following steps:

1) preparing deer bone powder: removing meat, fascia and bone marrow from fresh sika deer bone, cleaning, drying in oven at 105 deg.C to constant weight, pulverizing, sieving with 60 mesh sieve, and making into sika deer bone powder.

2) Preparing deer bone chelated calcium: mixing the deer bone powder and glutamic acid according to the mass ratio of 1: 1-5, adding water, adjusting the pH of the solution to 6.0-8.0 by NaOH, chelating at 60-70 ℃ for 50-70 min, continuously stirring, centrifuging to obtain a supernatant, concentrating under reduced pressure, adding absolute ethanol, precipitating at 0-4 ℃ for 12-24 h, drying the precipitate, and crushing to obtain the deer bone glutamic acid chelated calcium powder.

A method for preparing calcium glutamate chelate from deer bones specifically comprises the following steps:

1) preparing deer bone powder: removing meat, fascia and bone marrow from fresh sika deer bone, cleaning, drying in oven at 105 deg.C to constant weight, pulverizing, sieving with 60 mesh sieve, and making into sika deer bone powder.

2) Preparing deer bone chelated calcium: mixing deer bone powder and glutamic acid at a mass ratio of 1:1, wherein the pH value of the reaction solution is 7.0, the chelation reaction time is 60min, and the chelation reaction temperature is 70 ℃. Compared with the prior art, the invention has the beneficial effects that:

(1) the chelation rate is high, and simultaneously, the high VD is contained, so that the calcium resource in the deer bone can be fully utilized;

(2) the dissolubility is good, the bioavailability is high, and the stimulation of the medicine to the gastrointestinal tract can be reduced;

(3) no additive or preservative, and is safe and reliable;

(4) the production process is simple, is suitable for industrial and automatic production, does not produce three wastes, and reduces the pollution to the environment.

Drawings

FIG. 1 is a high performance liquid chromatogram of VD2 and VD3 reference substance determination

FIG. 2 is a high performance liquid chromatogram measured by VD2 and VD3 in deer bone.

Detailed Description