CN104644694A - Preparation method of ultramicro spirulina powder as well as preparation and application thereof - Google Patents
Preparation method of ultramicro spirulina powder as well as preparation and application thereof Download PDFInfo
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Abstract
The invention discloses a preparation process of ultramicro spirulina powder. The preparation process of the ultramicro spirulina powder comprises the following two steps: (1) directly superfine grinding the spirulina; and (2) uniformly mixing the spirulina water extract and the extracted spirulina residue product to obtain the spirulina powder. The average grain size of the spirulina powder is 200-800 nm. The prescription and the preparation process of the tablet, the capsule and the soft capsule of the ultramicro spirulina powder and the common spirulina powder (less than 100 meshes) are created and researched based on the ultramicro spirulina powder. The additive amount of the auxiliary materials is greatly reduced; by adopting the new preparation molding process, the problems of unreasonable prescription of the current spirulina product, many auxiliary materials, multiple varieties, low purity, tedious production process and low product quality can be solved; and the industrial production speed can be quickened and the production efficiency can be increased. The prepared product is detected. The function test proves that the ultramicro spirulina powder and the common spirulina powder have the radiation-proof effect and liver-protective effect.
Description
Technical field
The present invention relates to the preparation method of ultra micro Spirulina powder, its preparation and application thereof, belong to technical field of Chinese medicine.
Background technology
Spirulina typically refers to the cyanophyceae that two kinds supply the joint spiral shell Trentepohlia of the mankind and animal edible---the greatly common name of joint spiral shell algae (formal name used at school Arthrospira maxima) and blunt epimerite spiral shell algae (formal name used at school Arthrospira platensis).These two kinds were originally divided into Spirullina (formal name used at school Spirulina), after be divided into joint spiral shell Trentepohlia, but to be still referred to as traditionally " spirulina ".For thousands of years, spiral algae is worked as food always and eats by African Chad lakeside and Mexico Texcoco lake aboriginal, and whole world various countries it can be used as nutriment to take in a large number has also had the history of 40 years, also finds no excessive rear poisoning phenomenon.Therefore, people assert that this spiral algae long-term taking is safe and reliable usually, and they regulate the balance of human physiological functions, promote human metabolism, enhancing immunity, improves body constitution, the effect of resisting fatigue, anoxia enduring also accept by increasing people.And modern's rhythm of life is fast, operating pressure large, diet is tending towards convenient, delicious, cause nutrition can not balanced absorption, body fat accumulation, body fluid acidify, mental fatigue, physically-draining, cause the crowd such as hypertension, hyperlipidemia sharply to increase, the quality of life of people obviously declines.The exploitation of spirulina series products has market very widely.
But containing rich in protein in spirulina, polysaccharide, β-carotene, linoleic acid, trace element etc., its main active molecular weight is larger, be difficult to enrichment and optimization, be the technical barrier of Chemistry for Chinese Traditional Medicine always, and the raw material that spirulina series products uses in the market is mainly normal spiral algae powder (about 100 orders), nutrient substance stripping in normal spiral algae powder is more difficult, and absorption of human body difficulty is large.The present invention proposes spirulina super-refinement, can rationally solve this problem.
Micropowder technology refer to material particles is crushed to 100% a kind of Crushing of Ultrafine technology of particle diameter below 30 μm [Li Fengsheng etc. ultra-fine powder technology. Beijing: National Defense Industry Press, 2000], being the new branch of science that 20 century 70s grow up mid-term, is an interdiscipline, the inter-trade comprehensive branch of learning.Superfine powder is divided into again micron order, submicron order and nanometer grade powder usually.Current there is no strict defining to this noun of ultrafine powder both at home and abroad, usually by 1250 orders (namely 10 μm) powder body below, be referred to as ultrafine powder, the powder body that wherein particle diameter is greater than 1 μm is called micro materials; The powder body that particle diameter is greater than 0.1 μm is called submicron material; The powder body that particle diameter is in 0.001 ~ 0.1 μm (i.e. 1 ~ 100nm) is called nano material [Luo Fusheng, Han Aijun, Yang Yi, Li Fengsheng, the application of Zhuan Hongbo, Zheng Liang unit's .2001. ultra-fine powder technology in Chinese herbal medicine industry. Chinese herbal medicine .32 (10): 941-942].Because Particle pollution causes the increase of surface area and porosity, superfine powder is made to have unique physical and chemical performance, as good dispersibility, adsorptivity, dissolubility, chemism, biological activity etc.Superfine technique is a new technique promoting the modernization of Chinese medicine.Because the stripping of the effective medicinal ingredient in Chinese herbal medicine cell needs just can enter in solvent through several even tens cell wall, be then absorbed by the body.In general pulverized particles and decoction pieces, most cell is complete, and its particle is made up of several, tens even more cells.And quite a few cell component can not enter solvent through cell wall, can only throw away in vain.After cell wall breaking, the composition in broken cells directly can contact solvent, and its effective ingredient can directly enter solvent and be absorbed by the body.Meanwhile, greatly can increase the specific surface area of powder body after micronization of treditional Chinese medicine, increase medicine and medicine-feeding part contact area, prolong drug is at absorption site adsorption time.Therefore ultrafine Chinese herb effective ingredient emission and disengage speed, the Chinese medicine coarse powder that in the unit interval, the amount of human drug absorption's effective ingredient all can obtain than Ordinary pulverization method is high, and the kind of its effective ingredient disengaged also will force Ordinary pulverization method complete.The drug effect time can significantly shorten, and to the effect of human body more comprehensively, action intensity is higher for the property of medicine.Micro-powder of Chinese herbs is directly taken and can obviously be made the composition of absorption of human body more comprehensively, and absorption intensity can improve, and absorbtivity can increase, thus significantly improves bioavailability.Powder body mean diameter after micronizing can below 10 μm, and its uniformity improves, and color and luster is consistent, and powder is fine and smooth.Change that Chinese medicinal powder quality is coarse, phenomenon that fiber and powder separation lack of homogeneity, piebaldism are more, improve drug quality.Experimental result shows, Chinese crude drug, food and health product are after superfine efflorescence, granular size evenly, and improve the mouthfeel [Yang Lianwei of Chinese medicine, food and health product, influence research to its performance after the .2008. Study on Supermicro-pulverization of Traditional Chinese Drugs such as Zhao Xiaoyan, Li Ting. World Science technology-TCM Modernization .10 (6): 77-81].Therefore, current ultra-fine powder technology is for medicine and Health-care Foods Industry widely use.
The spirulina series products purity of selling in the market is not high, and contained adjuvant is more, complex production process, and cost is higher.A kind of spirulina such sheets agent producing process, a kind of spiral algae capsule manufacturing techniques and a kind of spiral algae soft capsule production technology are proposed in the present invention, thus solve the unreasonable of existing spirulina series products formula, purity is low, complex production process, the problem that product quality is not high, and quickening commercial speeds, increase productivity efficiency.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art part, the preparation method of ultra micro Spirulina powder, its preparation and application thereof are provided.
The present invention comprises following technical scheme:
Technical scheme 1: a kind of preparation method of ultra micro Spirulina powder, comprises the following steps:
1) Spirulina powder of dried moisture below 5% being carried out below coarse powder to 100 order, is normal spiral algae powder;
2) adopt the impact grinding of high energy nanometer to carry out superfine grinding the Spirulina powder crushed, to be situated between ceaselessly impacting 6 ~ 10 hours by the mill in high energy nanometer impact grinding tank body, to make the mean diameter of Spirulina powder reach 200 ~ 800nm.
Technical scheme 2: a kind of preparation method of ultra micro Spirulina powder, comprises the following steps:
1) freeze thawing is extracted: get spirulina and soak in distilled water, the W/W ratio of algae and water is 1: 1, overnight at room temperature, within second day, put into refrigerator and be chilled to-15 DEG C, then be put in 40 DEG C of climatic chambers and melt rapidly, multigelation 3 times, respectively centrifuging and taking supernatant, algae-residue after separation stays for subsequent use, merge, (primary drying phase control temperature is-5 DEG C, and vacuum chamber pressure is 15Pa in lyophilization, drying time is 380min), obtain water extract;
2) algae-residue product is obtained after algae-residue drying.
3) water extract and algae-residue product Homogeneous phase mixing are obtained product A.
4) product A adopted the impact grinding of high energy nanometer to carry out superfine grinding, to be situated between ceaselessly impacting 6 ~ 10 hours by the mill in high energy nanometer impact grinding tank body, to make the mean diameter of Spirulina powder reach 200 ~ 800nm.
Technical scheme 3: the preparation method of the spirulina tablet of the ultra micro Spirulina powder obtained containing said method or normal spiral algae powder, in described tablet, according to percetage by weight, normal spiral algae powder below 100 orders comprising 98% ~ 99.5% or ultra micro Spirulina powder, the hypromellose of 0.1% ~ 0.4%, the magnesium stearate of 0.4% ~ 1.6%, described preparation method comprises the following steps:
1) normal spiral algae powder or the ultra micro Spirulina powder of below 100 orders is accurately taken;
2) take hypromellose and purified water mixes in proportion, be mixed with the hypromellose cellulose solution of 5.0% as binding agent;
3) hypromellose cellulose solution is added in Spirulina powder, cross 20 mesh sieves and obtain wet granular.
4) wet granular is dried to pellet moisture for being less than 3.0% at 50 ~ 60 DEG C, obtained dry granule.
5) add magnesium stearate, mixing 20min, obtain always mixed granule.
6) be placed in tablet machine by always mixing granule, be heavily 0.4g tabletting with sheet, tablet weight variation controls within ± 5%.
Technical scheme 4: the preparation method of the spirulina capsule of the ultra micro Spirulina powder obtained containing said method or normal spiral algae powder, in described capsule, according to percetage by weight, normal spiral algae powder below 100 orders comprising 98% ~ 99.5% or ultra micro Spirulina powder, the hypromellose of 0.1% ~ 0.4%, the magnesium stearate of 0.4% ~ 1.6%, described preparation method comprises the following steps:
1) normal spiral algae powder or the ultra micro Spirulina powder of below 100 orders is accurately taken;
2) take hypromellose and purified water mixes in proportion, be mixed with the hypromellose cellulose solution of 5.0% as binding agent;
3) hypromellose cellulose solution is added in Spirulina powder, cross 20 mesh sieves and obtain wet granular.
4) wet granular is dried to pellet moisture for being less than 3.0% at 50 ~ 60 DEG C, obtained dry granule.
5) add magnesium stearate, mixing 20min, obtain always mixed granule.
6) total mixed granule is placed in Autocapsulefillingmachine to fill, capsule shells is divided into Plant fiber's capsule and gelatine capsule.
Technical scheme 5: the preparation method of the Spirulina soft capsule of the ultra micro Spirulina powder obtained containing said method or normal spiral algae powder, in described soft capsule, according to percetage by weight, the normal spiral algae powder below 100 orders comprising 30% ~ 40% or ultra micro Spirulina powder; The Non-transgenic soybean oil of 15% ~ 20%; The gelatin of 45% ~ 50%, glycerol and purified water, the weight ratio of gelatin, glycerol and purified water is 2.5:2.5:1, and described preparation method comprises the following steps:
1) accurately take the normal spiral algae powder of below 100 orders or ultra micro Spirulina powder in agitator, then add Non-transgenic soybean oil, uniform stirring mixes;
2) mixture after stirring is ground in colloid mill, then slough the gas in material at vacuum tank, capsule Dissolve things inside can be obtained;
3) by gelatin, glycerol, purified water, in adding glue tank, glue is changed;
4) glue and capsule Dissolve things inside batching are extruded qualified soft capsule through pellet press, 0.8g/ grain;
5) with edible ethanol cleaning soft capsule surface oil;
6) soft capsule is put into drying rotating cage inner drying.
Technical scheme 6: containing the ultra micro Spirulina powder that said method is obtained, in described ultra micro Spirulina powder, protein content is not less than 60.4g/100g, and β-carotene carotene content is not less than 320mg/100g.And normal spiral algae powder is characterized as: protein content is not less than 50.8g/100g, β-carotene carotene content is not less than 228mg/100g.
Technical scheme 7: the ultra micro Spirulina powder obtained containing said method is being prepared radioprotective, protected the liver and strengthen the application in immune drug or health product.
The present invention has following technique effect:
The object of technical scheme 1 is the preparation method providing a kind of spirulina superfine powder (200 ~ 800nm), existing market Spirulina Products is all mainly for raw material [is 60 ~ 120 orders as application number 201110308518.8. mono-kind adds Spirulina powder used in the spirulina tablet of glycerol and the patent of processing method thereof with normal spiral algae powder; Spirulina powder used in patent as the preparation method of an application number 00130805.X. spirulina tablet is 50 ~ 80 orders], the product that not find with spirulina superfine powder be raw material.But the patent that application number is 01100320.0 1 kinds of nano spirulina preparation medicines and preparation method thereof proposes the scheme of preparation 0.2 ~ 200nm spirulina superfine powder and applies for a patent; but this particle diameter is not protected; in actual production process; the particle diameter of spirulina superfine powder all can not reach below 200nm and the average overwhelming majority is less than 100nm; the ultra micro Spirulina powder of this particle diameter can only be present in theory, cannot be converted into actual production.The present invention verifies through actual production, and has detailed data (referring to table 1) to confirm, the particle diameter of the ultra micro Spirulina powder prepared by preparation method provided by the invention is on average between 200 ~ 800nm.Propose this preparation method to be intended to allow ultra micro Spirulina powder be more prone to allow absorption of human body, improve the mouthfeel [Yang Lianwei of spirulina, influence research to its performance after the .2008. Study on Supermicro-pulverization of Traditional Chinese Drugs such as Zhao Xiaoyan, Li Ting. World Science technology-TCM Modernization .10 (6): 77-81].
The object of technical scheme 2 is the preparation method providing another spirulina superfine powder (200 ~ 800nm), containing rich in protein in spirulina, polysaccharide, β-carotene, linoleic acid, trace element etc., its main active molecular weight is larger, be difficult to enrichment and optimization, it is the technical barrier of Chemistry for Chinese Traditional Medicine always, existing technology of preparing is mainly spirulina after water extraction, algae-residue is directly discarded, the wasting of resources can be caused like this, environmental pollution and the loss of medicine source [as application number, to be 201310046031.6 1 kinds of algae-residues extracted from spirulina in the patent of the method for phycocyanin be exactly directly discards], after extracting active substance according to the method in this patent, we carry out detection to algae-residue and find still there is polysaccharide (content is more) in algae-residue, protein, β-carotene, trace element etc. nutrient substance, visible, a large amount of wastings of resources and drug effect Value Loss are caused.Preparation method in embodiment 2 is proposed in view of the above circumstances, after spirulina is extracted, (algae-residue drying divides 3 kinds of methods: A lyophilization: primary drying phase control temperature is-5 DEG C, and vacuum chamber pressure is 15Pa, and drying time is 380min to carry out drying respectively to extraction concentrated solution and algae-residue; B. freeze-day with constant temperature: at the dry 8h of 40 DEG C of thermostatic drying chambers; C. vacuum drying: at the dry 12h. of 60 DEG C of vacuum drying ovens), then prepare ultra micro Spirulina powder according to the preparation method in technical scheme 1.This preparation method proposes first, make use of the dissolution with solvents characteristic rule of chemical composition of Chinese materia medica on the one hand, make use of ultramicrotechnique on the other hand, two kinds of technology are through ingenious combination, form new patent of invention, be intended to human body can better be absorbed the nutritional labeling of spirulina and can not cause a large amount of wastes.
The object of technical scheme 3 is the formula and the preparation method that provide a kind of spirulina tablet, and the formula of current spiral algae sheet has following 2 shortcomings: 1) kind of adjuvant many [as application number be in the formula proposed in the patent of 201010541210.3 1 kinds of spiral algae sheets and preparation method thereof adjuvant up to 6 kinds]; 2) the accounting amount of adjuvant large [as application number be in the formula proposed in the patent of 201310664176.2 1 kinds of spiral algae sheets and preparation method thereof adjuvant content up to 10%].Adjuvant is to the side effect of human body, the healthy topic paid close attention to very much of academia in recent years always, if a large amount of adjuvant of adult's long-term taking can to human body cause very large burden [Wang Qi .2013. food additive is to the influence research of human health. CNPC and chemical standard and quality .22].In the formula that the present invention proposes, adjuvant content is only about 0.75%, but surprisingly, but the reasonable preparation of tablet can be met, thus solve the unreasonable of existing algae tablet formulation, purity is low, complex production process, the problem that product quality is not high, and quickening commercial speeds, increase productivity efficiency.
The object of technical scheme 4 is the formula and the preparation method that provide a kind of spirulina capsule, and the formula of current spirulina capsule has following shortcoming: the accounting amount of adjuvant large (as adjuvant content in the formula that proposes in the patent of application number 200910223872.3 1 kinds of spirulina capsules and production process thereof reaches 2%).Adjuvant is to the side effect of human body, the healthy topic paid close attention to very much of academia in recent years always, if a large amount of adjuvant of adult's long-term taking can to human body cause very large burden [Wang Qi .2013. food additive is to the influence research of human health. CNPC and chemical standard and quality .22].In the formula that the present invention proposes, adjuvant content is only 0.75%, thus solves the unreasonable of existing algae capsule formula, and purity is low, complex production process, the problem that product quality is not high, and accelerates commercial speeds, and increase productivity efficiency.
The object of technical scheme 5 is the formula and the preparation method that provide a kind of Spirulina soft capsule, and soft capsule is a kind of novel health food dosage form.Oil or oily and the quantitative pressure injection of powdery functional materials suspension can be encapsulated in glued membrane by soft capsule, form size, different seal capsule, there is excellent isolation features, can keep apart to the functional material of light, oxygen sensitivity and air, light, avoid the oxidation of active substance, make product keep stable content before the deadline, ensure the performance of effect.Soft gel products novel appearance, tempting, the very attractive and novel sense to consumer and safe to carry, instant.The formula of current Spirulina soft capsule has following shortcoming: Spirulina powder content is few, adjuvant many (in the patent of application number 200310107810.9 Spirulina soft capsule and preparation method thereof, Spirulina soft capsule capsule liquid is by spirulina fine powder 3%-15% and adjuvant 85%-97%), adjuvant is to the side effect of human body, the healthy topic paid close attention to very much of academia in recent years always, if a large amount of adjuvant of adult's long-term taking can to human body cause very large burden [Wang Qi .2013. food additive is to the influence research of human health. CNPC and chemical standard and quality .22].In the formula that the present invention proposes, in soft capsule liquid, adjuvant is 32%, reduces adjuvant content greatly.The present invention combines soft capsule and ultra micro Spirulina powder cleverly, namely has the advantage of soft capsule, has again the advantage that ultra micro Spirulina powder easily absorbs.
The object of technical scheme 6 is the principal character of the ultra micro Spirulina powder providing the preparation used in the present invention: this feature is except 200 ~ 800nm except meeting mean diameter, ultra micro Spirulina powder is characterized as: protein content is not less than 60.4g/100g, and β-carotene carotene content is not less than 320mg/100g.And normal spiral algae powder is characterized as: protein content is not less than 50.8g/100g, β-carotene carotene content is not less than 228mg/100g;
The object of technical scheme 7 is that the ultra micro Spirulina powder providing said method to obtain is being prepared radioprotective, protected the liver and strengthen the application in immune drug or health product.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further elaborated:
The preparation method of embodiment 1 ultra micro Spirulina powder (mean diameter is 200 ~ 800nm)
Get normal spiral algae (Sanya Hai Wang marine organisms Science and Technology Ltd. produces the spirulina provided, and dry, pulverize, and crosses 100 mesh sieves), be processed into ultra micro Spirulina powder (200 ~ 800nm), its method comprises the following steps:
1. the Spirulina powder of dried (moisture is below 5%) is carried out below coarse powder to 100 order.
2. adopt the impact grinding of high energy nanometer to carry out superfine grinding the Spirulina powder crushed, to be situated between ceaselessly impacting 6 ~ 10 hours by the mill in high energy nanometer impact grinding tank body, to make the mean diameter of Spirulina powder reach 200 ~ 800nm.
Production detailed data is in table 1
Table 1 ultra micro Spirulina powder Production development tables of data
| Batch | Product batch number | Material quantity (g) | Output (g) | Waste (g) | Yield (%) | Assay |
| 1 | 20130903 | 50083 | 48552 | 1531 | 96.94 | Qualified |
| 2 | 20130904 | 49979 | 48501 | 1478 | 97.04 | Qualified |
| 3 | 20130905 | 50035 | 48496 | 1539 | 96.92 | Qualified |
(remarks: these 3 lot number techniques are identical, raw material dosage is different.)
The preparation method of embodiment 2 ultra micro Spirulina powder (mean diameter is 200 ~ 800nm)
1. freeze thawing is extracted: (Sanya Hai Wang marine organisms Science and Technology Ltd. produces the spirulina provided to get normal spiral algae, dry, pulverize, cross 100 mesh sieves) in distilled water, soak (algae: water is 1: 1, W/W) overnight at room temperature, within second day, put into refrigerator and be chilled to-15 DEG C, then be put in 40 DEG C of climatic chambers and melt rapidly, multigelation 3 times, centrifuging and taking supernatant respectively, algae-residue after separation stays for subsequent use, merge, (primary drying phase control temperature is-5 DEG C in lyophilization, vacuum chamber pressure is 15Pa, drying time is 380min) obtain water extract,
2. algae-residue obtains algae-residue product after the drying.
3. water extract and algae-residue product Homogeneous phase mixing are obtained product A.
4. by the preparation technology in embodiment 1, ultra micro Spirulina powder prepared by product A.
Production detailed data is in table 2
Table 2 ultra micro Spirulina powder Production development tables of data
3 kinds of drying meanss of (remarks: these 3 lot numbers corresponding step 2 respectively) algae-residue.)
3 kinds of drying meanss are respectively: 1, lyophilization: identical with supernatant method (lot number 20130911)
2, naturally dry (lot number 20130912)
3,40 degree of drying in oven (lot number 20130913)
Embodiment 3
A: the preparation technology 1 (adopting raw material to be normal spiral algae powder) of spiral algae sheet
1) formula 1: normal spiral algae powder: 3930g; Hypromellose: 16g; Magnesium stearate: 64g.
1. 3930g normal spiral algae powder (Sanya Hai Wang marine organisms Science and Technology Ltd. produces the spirulina provided, and dry, pulverize, and crosses 100 mesh sieves) is accurately taken.
2. take 16g hypromellose and purified water mixes in proportion, be mixed with the hypromellose cellulose solution of 5.0% as binding agent;
3. hypromellose cellulose solution is added in Spirulina powder, cross 20 mesh sieves and obtain wet granular.
4. wet granular is dried to pellet moisture for being less than 3.0% at 50 ~ 60 DEG C, obtained dry granule.
5. add 64g magnesium stearate, mixing 20min, obtain always mixed granule.
6. be placed in tablet machine by always mixing granule, be heavily 0.4g tabletting with sheet, tablet weight variation controls within ± 5%.
2) formula 2: normal spiral algae powder: 3990g; Hypromellose: 4g; Magnesium stearate: 16g.
Technique is with formula 1.
3) formula 3 (optimization formula): normal spiral algae powder: 3980g; Hypromellose: 10g; Magnesium stearate: 20g.
Technique is with formula 1.
Optimization formula production detailed data is in table 3:
Table 3 normal spiral algae sheet (optimization formula) Production development tables of data
(remarks: these 3 lot number techniques are identical, composition of raw materials is different.)
The preparation technology 2 (adopting the ultra micro Spirulina powder of preparation in embodiment 1 and 2) of B, spiral algae sheet:
1) formula 1:: ultra micro Spirulina powder: 3930g; Hypromellose: 16g; Magnesium stearate: 64g.
1. 3930g ultra micro Spirulina powder (preparing in embodiment 1 and 2) is taken respectively.
2. take 16g hypromellose and purified water mixes in proportion, be mixed with the hypromellose cellulose solution of 5.0% as binding agent;
3. hypromellose cellulose solution is added in ultra micro Spirulina powder, cross 20 mesh sieves and obtain wet granular.
4. wet granular is dried to pellet moisture for being less than 3.0% at 50 ~ 60 DEG C, obtained dry granule.
5. add 64g magnesium stearate, mixing 20min, obtain always mixed granule.
6. be placed in tablet machine by always mixing granule, be heavily 0.4g tabletting with sheet, tablet weight variation controls within ± 5%.
2) formula 2: ultra micro Spirulina powder: 3990g; Hypromellose: 4g; Magnesium stearate: 16g.
Technique is with formula 1.
3) formula 3 (optimum): ultra micro Spirulina powder: 3980g; Hypromellose: 10g; Magnesium stearate: 20g.
Technique is with formula 1.
Optimization formula production detailed data is in table 4:
Table 4 ultra micro spiral algae sheet (optimum) Production development tables of data
(remarks: these 6 lot number techniques are identical, composition of raw materials and/or ultra micro Spirulina powder raw material sources difference.)
Embodiment 4
Preparation technology's (raw material is normal spiral algae powder) of A spirulina capsule:
1) formula 1: normal spiral algae powder: 3930g; Hypromellose: 16g; Magnesium stearate: 64g.
1. 3930g spirulina common flour (Sanya Hai Wang marine organisms Science and Technology Ltd. produces the spirulina provided, and dry, pulverize, and crosses 100 mesh sieves) is accurately taken.
2. take 16g hypromellose and purified water mixes in proportion, be mixed with the hypromellose cellulose solution of 5.0% as binding agent
3. hypromellose cellulose solution is added in ultra micro Spirulina powder, cross 20 mesh sieves and obtain wet granular.
4. wet granular is dried to pellet moisture for being less than 3.0% at 50 ~ 60 DEG C, obtained dry granule.
5. add 64g magnesium stearate, mixing 20min, obtain always mixed granule.
6. total mixed granule is placed in Autocapsulefillingmachine to fill, capsule shells is divided into Plant fiber's capsule and gelatine capsule.
2) formula 2: normal spiral algae powder: 3990g; Hypromellose: 4g; Magnesium stearate: 16g.
Technique is with formula 1.
3) formula 3 (optimum): normal spiral algae powder: 3980g; Hypromellose: 10g; Magnesium stearate: 20g.
Technique is with formula 1.
Optimization formula production detailed data is in table 5:
Table 5 normal spiral algin capsule (optimum) Production development tables of data
(remarks: these 3 lot number techniques are identical, composition of raw materials is different.)
The preparation technology 2 (adopting the ultra micro Spirulina powder of preparation in embodiment 1 and 2) of B spirulina capsule:
1) formula 1:: ultra micro Spirulina powder: 3930g; Hypromellose: 16g; Magnesium stearate: 64g.
1. 3930g ultra micro Spirulina powder (embodiment 1 and embodiment preparation) is taken respectively
2. take 16g hypromellose and purified water mixes in proportion, be mixed with the hypromellose cellulose solution of 5.0% as binding agent
3. hypromellose cellulose solution is added in ultra micro Spirulina powder, cross 20 mesh sieves and obtain wet granular.
4. wet granular is dried to pellet moisture for being less than 3.0% at 50 ~ 60 DEG C, obtained dry granule.
5. add 64g magnesium stearate, mixing 20min, obtain always mixed granule.
6. total mixed granule is placed in Autocapsulefillingmachine to fill, capsule shells is divided into Plant fiber's capsule and gelatine capsule.
2) formula 2: ultra micro Spirulina powder: 3990g; Hypromellose: 4g; Magnesium stearate: 16g.
Technique is with formula 1.
3) formula 3 (optimum): ultra micro Spirulina powder: 3980g; Hypromellose: 10g; Magnesium stearate: 20g.
Technique is with formula 1.
Optimization formula production detailed data is in table 6:
Table 6 ultra micro spirulina capsule (optimum) Production development tables of data
(remarks: these 6 lot number techniques are identical, composition of raw materials and/or ultra micro Spirulina powder raw material sources difference.)
Embodiment 5
The preparation technology 1 (raw material is normal spiral algae powder) of A Spirulina soft capsule:
1) formula 1: normal spiral algae powder: 2400g; Non-transgenic soybean oil: 1600g; Gelatin: 1667g; Glycerol: 1667g; Purified water: 666g.
Technological process is as follows:
1. accurately take 2400g normal spiral algae powder (Sanya Hai Wang marine organisms Science and Technology Ltd. produces the spirulina provided, and dry, pulverize, and crosses 100 mesh sieves) in agitator, then add 1600g Non-transgenic soybean oil, uniform stirring mixes;
2. the mixture after stirring is ground in colloid mill, then slough the gas in material at vacuum tank, capsule Dissolve things inside can be obtained;
3. glue is changed by 1667g gelatin, 1667g glycerol, adding of 666g purified water glue tank;
4. glue and capsule Dissolve things inside batching are extruded qualified soft capsule (0.8g/ grain) through pellet press;
5. with edible ethanol cleaning soft capsule surface oil;
6. soft capsule is put into drying rotating cage inner drying;
2) formula 2: normal spiral algae powder: 3200g; Non-transgenic soybean oil: 1200g; Gelatin: 1500g; Glycerol: 1500g; Purified water: 600g.
Technique is with formula 1.
3) formula 3 (optimum): normal spiral algae powder: 2780g; Non-transgenic soybean oil: 1320g; Gelatin: 1625g; Glycerol: 1625g; Purified water: 650g.
Technique is with formula 1.
Optimization formula production detailed data is in table 7:
Table 7 normal spiral algae soft capsule (optimum) Production development tables of data
(remarks: these 3 lot number techniques are identical, composition of raw materials is different.)
The preparation technology 2 (raw material adopts the ultra micro Spirulina powder of preparation in embodiment 1 and 2) of B Spirulina soft capsule:
1) formula 1: ultra micro Spirulina powder: 2400g; Non-transgenic soybean oil: 1600g; Gelatin: 1667g; Glycerol: 1667g; Purified water: 666g.
Technological process is as follows:
The technological process preparing Spirulina soft capsule is as follows:
1. accurately take 2400g ultra micro Spirulina powder (prepared by embodiment 1 and embodiment 2) in agitator, then add 1600g Non-transgenic soybean oil, uniform stirring mixes;
2. the mixture after stirring is ground in colloid mill, then slough the gas in material at vacuum tank, capsule Dissolve things inside can be obtained;
3. glue is changed by 1667g gelatin, 1667g glycerol, adding of 666g purified water glue tank;
4. glue and capsule Dissolve things inside batching are extruded qualified soft capsule (0.8g/ grain) through pellet press;
5. with edible ethanol cleaning soft capsule surface oil;
6. soft capsule is put into drying rotating cage inner drying;
2) formula 2: ultra micro Spirulina powder: 3200g; Non-transgenic soybean oil: 1200g; Gelatin: 1500g; Glycerol: 1500g; Purified water: 600g.Technique is with formula 1.
3) formula 3 (optimum): ultra micro Spirulina powder: 2780g; Non-transgenic soybean oil: 1320g; Gelatin: 1625g; Glycerol: 1625g; Purified water: 650g.Technique is with formula 1.
Optimization formula production detailed data is in table 8:
Table 8 ultra micro Spirulina soft capsule (optimum) Production development tables of data
(remarks: these 6 lot number techniques are identical, composition of raw materials and/or ultra micro Spirulina powder raw material sources difference.)
Embodiment 6
Get normal spiral algae powder, ultra micro Spirulina powder (embodiment 1 and 2 respectively gets portion) sample respectively, detect physical and chemical composition wherein and microbe composition, detailed data is in table 9, visible 1) normal spiral algae powder is characterized as: protein content is not less than 50.8g/100g, and β-carotene carotene content is not less than 228mg/100g (in negative 10% of measured value); Ultra micro Spirulina powder (embodiment 1) is characterized as: protein content is not less than 60.4g/100g, and β-carotene carotene content is not less than 320mg/100g (in negative 10% of measured value); Ultra micro Spirulina powder (embodiment 2) protein content is not less than 65.6g/100g, and β-carotene carotene content is not less than 361mg/100g (in negative 10% of measured value).2) protein of ultra micro Spirulina powder (embodiment 1 and embodiment 2) and β-carotene carotene content are than the height of normal spiral algae powder, demonstrate ultra micro Spirulina powder and are more prone to absorb.
Table 9
Detection method is as follows:
Protein detection:
The method specified by GB 5009.5 measures.
β-carotene detects
The method specified by GB/T 5009.83 measures.
Plumbous detection
The method specified by GB/T 5009.12 measures.
Total arsenic detects
The method specified by GB/T 5009.11 measures.
Total mercury detects
The method specified by GB/T 5009.17 measures.
Cadmium detects
The method specified by GB/T 5009.15 measures.
Microbiological indicator detects
The method inspection specified by GB/T 4789.24.
Embodiment 7
Ultra micro Spirulina powder is to the research of white mice radiation resistance
Spirulina is a class rudimentary plant, belongs to Cyanophyta, Oscillariaceae, is the biology that nutritional labeling that on the current earth, the mankind are known is abundant, the most balanced.According to surveying and determination, spirulina contains rich in protein (65%), aminoacid, mineral, vitamin, β-carotene, linolenic acid, chlorophyll etc.Once spirulina was carried out to the Toxicological evaluation of system both at home and abroad, Ministry of Public Health determines that it is safe new resource food.In recent years, more and more deep to the understanding of spirulina efficacy effect both at home and abroad, but the rare report of the radiation-resistant research of relevant spirulina.The impact of ultra micro spirulina on radiation aspect of this experimental observation, is intended to for developmental research provides scientific basis based on the health food of ultra micro Spirulina powder.
1. materials and methods
1.1 tested material
Normal spiral algae powder (the normal spiral algae powder of preparation in embodiment 3), ultra micro Spirulina powder (embodiment 1 and embodiment 2).Inspection product are powdery, and every part is 0.4g, and adult recommends take in 4.8g every day.By adult 60kg weighing machine, human body recommended intake can be converted as 0.08g/kg.bw every day.Kunming mouse, 20d age, body weight (16-20) g, male and female half and half.
1.2 test method
1.2.1 animal experiment and assay method
After 110 white mice adapt to feed 7d, blood sampling counting leukocyte after numbering, press leucocyte level again, and reference weight is divided into 11 groups at random, normal spiral algae powder three dosage groups respectively, ultra micro Spirulina powder (embodiment 1) three dosage groups, ultra micro Spirulina powder (embodiment 2) three dosage groups and a radiation matched group, often organize 10.Namely 0.8 three dosage component do not give tested material by 10 times, 20 times, 30 times (, 1.6,2.4g/kg.bw) of human body recommended intake (0.08g/kg.bw), and radiation matched group gives pure water.Each group of mouse stomach capacity is 0.10ml/kg.bw, and after continuous gavage 15d, with 60Co radiation exposure these 10 groups, irradiation distance 75cm, irradiates visual field 20cm*20cm, irradiation time 8min.In irradiate the 3rd, 7,15, within 30 days, get blood, measure Blood Physiological Indexes with automatic clinical chemistry analyzer.
2. results and analysis
The impact that 2.1 Spirulina powder count raying murine interleukin
Compare with radiation matched group, * P<0.05; Compare with radiation matched group, * * P<0.01.Predose respectively organizes murine interleukin counting does not have notable difference, and after radiation, murine interleukin significantly declines, but gos up gradually along with the prolongation of time.After radiation after 15d, superfine powder group is significantly higher than concurrent control.After irradiation after 30d, superfine powder group reaches normal level.Above result shows: the effect that after ultra micro Spirulina powder has obviously promotion radiation, murine interleukin gos up.
2.2 Spirulina powder are on the impact of raying Mouse Blood red blood cell count(RBC)
Compare with radiation matched group, * P<0.05.After radiation, the peripheral blood red cell in mice level declines to some extent, drops to minimum point at 15d, and then erythrocyte number starts slow rising, at 30d, substantially reaches the level before test.
3. discuss
Result of the test shows; ultra micro spiral vermicelli, to after 60Co radiation exposure, has and significantly raises murine interleukin number, the effect of erythrocyte number; according to " function of health food assessment process and method of inspection specification ", prompting ultra micro spiral vermicelli has assistant protection function to radiation hazradial bundle.
Embodiment 8
Ultra micro Spirulina powder is to the experimental study of hepatic injury
Spirulina is a class rudimentary plant, belongs to Cyanophyta, Oscillariaceae, is the biology that nutritional labeling that on the current earth, the mankind are known is abundant, the most balanced.According to surveying and determination, spirulina contains rich in protein (65%), aminoacid, mineral, vitamin, β-carotene, linolenic acid, chlorophyll etc.Once spirulina was carried out to the Toxicological evaluation of system both at home and abroad, Ministry of Public Health determines that it is safe new resource food.This experimental observation ultra micro spirulina, on the impact protecting the liver aspect, to be intended to for developmental research provides scientific basis based on the health food of ultra micro Spirulina powder.
1. materials and methods
1.1 material
Kunming mouse 60,20d age, body weight 16-20g, male and female half and half.Normal spiral algae powder (Sanya Hai Wang marine organisms Science and Technology Ltd. produces and provides), ultra micro Spirulina powder (embodiment 1 and embodiment 2).Inspection product are powdery, and every part is 0.4g, and adult recommends take in 4.8g every day.By adult 60kg weighing machine, human body recommended intake can be converted as 0.08g/kg.bw every day.
1.2 animal groupings
Get Kunming mouse, male and female half and half, be divided into 5 groups at random, be i.e. model group, normal saline group, normal spiral algae powder, ultra micro Spirulina powder (embodiment 1), ultra micro Spirulina powder (embodiment 2).
1.3 test procedure
Each group of mice gavage respectively, normal saline group, model group give normal saline 0.10ml/kg.bw, all the other each group gives normal spiral algae powder liquid respectively, ultra micro Spirulina powder liquid (embodiment 1), ultra micro Spirulina powder liquid (embodiment 2) 0.10ml/kg.bw, tested material is given respectively by 10 times, 20 times, 30 times (namely 0.8,1.6,2.4g/kg.bw) of human body recommended intake (0.08g/kg.bw), continuous gavage 7 days, once a day.
Model group and each administration group mice, after 2 hours, are often only pressed the CCl of 0.10ml/kg.bw lumbar injection 0.1% by last administration
4olive oil solution.Saline control group gives olive oil according to same dosage.After each group of modeling, fasting can't help water 18 hours.
Modeling after 18 hours femoral artery get blood, dissect simultaneously, get appropriate hepatic tissue at the same position of liver, make the liver homogenate of 10% under ice bath with normal saline, with the centrifugal 10min of 2000r/min, get supernatant for subsequent use.After blood coagulation, with the centrifugal 25min of 2500r/min, absorb serum for subsequent use.
2. result
2.1 respectively organize Spirulina powder to the impact of hepatic injury mice serum ALT, AST
Compare with normal saline group, * P<0.05; Compare with model group, * * P<0.01; Compare with normal spiral algae powder, * * * P<0.001
3 discuss
This experiment confirms, ultra micro Spirulina powder is active by reducing ALT, AST, alleviates hepatic injury, reaches hepatoprotective effect.
Embodiment 9
Ultra micro Spirulina powder acute toxicological experiment
Preliminary experiment: by acute toxicological experiment method, selects kunming mice 40, fasting, can't help water 12h.Ultra micro Spirulina powder (respectively in Example 1 lot number be 20130904 and embodiment 2 in lot number be 20130912) be mixed with the suspension of Cmax.Every each gavage of mice is about 0.8mL/20g (body weight), gavage 3 times in 24h, interval 4h.Then raise routinely, and observe the toxic reaction situation (outward appearance, activity, breathing, secretions, defecation, death etc.) of mice, and continuous weighting 7 days.Because of with maximum administration concentration, maximum administration capacity, all do not measure median lethal dose(LD 50) (LD50), therefore do maximum dosage-feeding experiment.
1) generally show
After administration in 14 days, experimental mice diet is normal, and fur is smooth, and freely, defecation is normal, and secretions without exception, its respiratory system, cardiovascular system, nervous system, digestive system and urinary system are showed no exception, and mice all survives in activity.Its, maximum dosage-feeding was respectively 177g/kg (in embodiment 1, lot number is 20130904), 180g/kg (in embodiment 2, lot number is 20130912) every day, was equivalent to 200 times of clinical adult's dosage.
2) body weight change situation
After administration in 14 days, body weight change without exception.
3) main organs is observed
2 groups of mices also pass through perusal through gross anatomy, and have no the abnormal phenomenas such as internal organs enlargement, atrophy, necrosis, main organs is all without any bad pathological changes, close with blank group.In sum, point out this medicine nontoxic, its clinical application amount is the dosage of a safety, clinical drug safety.
Claims (7)
1. a preparation method for ultra micro Spirulina powder, is characterized in that, comprises the following steps:
1) Spirulina powder of dried moisture below 5% being carried out below coarse powder to 100 order, is normal spiral algae powder;
2) adopt the impact grinding of high energy nanometer to carry out superfine grinding the Spirulina powder crushed, to be situated between ceaselessly impacting 6 ~ 10 hours by the mill in high energy nanometer impact grinding tank body, to make the mean diameter of Spirulina powder reach 200 ~ 800nm.
2. a preparation method for ultra micro Spirulina powder, is characterized in that, comprises the following steps:
1) freeze thawing is extracted: get spirulina and soak in distilled water, the W/W ratio of algae and water is 1: 1, overnight at room temperature, puts into refrigerator in second day and is chilled to-15 DEG C, is then put in 40 DEG C of climatic chambers and melts rapidly, multigelation 3 times, centrifuging and taking supernatant respectively, the algae-residue after separation stays for subsequent use, merges, lyophilization, obtains water extract;
2) algae-residue product is obtained after algae-residue drying;
3) water extract and algae-residue product Homogeneous phase mixing are obtained product A;
4) product A adopted the impact grinding of high energy nanometer to carry out superfine grinding, to be situated between ceaselessly impacting 6 ~ 10 hours by the mill in high energy nanometer impact grinding tank body, to make the mean diameter of Spirulina powder reach 200 ~ 800nm.
3. the preparation method of the ultra micro Spirulina powder obtained containing, for example method described in claim 1 or 2 or the spirulina tablet of normal spiral algae powder, it is characterized in that, in described tablet, according to percetage by weight, normal spiral algae powder below 100 orders comprising 98% ~ 99.5% or ultra micro Spirulina powder, the hypromellose of 0.1% ~ 0.4% and the magnesium stearate of 0.4% ~ 1.6%, described preparation method comprises the following steps:
1) normal spiral algae powder or the ultra micro Spirulina powder of below 100 orders is accurately taken;
2) take hypromellose and purified water mixes in proportion, be mixed with the hypromellose cellulose solution of 5.0% as binding agent;
3) hypromellose cellulose solution is added in Spirulina powder, cross 20 mesh sieves and obtain wet granular;
4) wet granular is dried to pellet moisture for being less than 3.0% at 50 ~ 60 DEG C, obtained dry granule;
5) add magnesium stearate, mixing 20min, obtain always mixed granule;
6) be placed in tablet machine by always mixing granule, be heavily 0.4g tabletting with sheet, tablet weight variation controls within ± 5%.
4. the preparation method of the ultra micro Spirulina powder obtained containing, for example method described in claim 1 or 2 or the spirulina capsule of normal spiral algae powder, it is characterized in that, in described capsule, according to percetage by weight, normal spiral algae powder below 100 orders comprising 98% ~ 99.5% or ultra micro Spirulina powder, the hypromellose of 0.1% ~ 0.4% and the magnesium stearate of 0.4% ~ 1.6%, described preparation method comprises the following steps:
1) normal spiral algae powder or the ultra micro Spirulina powder of below 100 orders is accurately taken;
2) take hypromellose and purified water mixes in proportion, be mixed with the hypromellose cellulose solution of 5.0% as binding agent;
3) hypromellose cellulose solution is added in Spirulina powder, cross 20 mesh sieves and obtain wet granular;
4) wet granular is dried to pellet moisture for being less than 3.0% at 50 ~ 60 DEG C, obtained dry granule;
5) add magnesium stearate, mixing 20min, obtain always mixed granule;
6) total mixed granule is placed in Autocapsulefillingmachine to fill, capsule shells is divided into Plant fiber's capsule and gelatine capsule.
5. the preparation method of the ultra micro Spirulina powder obtained containing, for example method described in claim 1 or 2 or the Spirulina soft capsule of normal spiral algae powder, it is characterized in that, in described soft capsule, according to percetage by weight, the normal spiral algae powder below 100 orders comprising 30% ~ 40% or ultra micro Spirulina powder; The Non-transgenic soybean oil of 15% ~ 20%; The gelatin of 45% ~ 50%, glycerol and purified water, the weight ratio of gelatin, glycerol and purified water is 2.5:2.5:1, and described preparation method comprises the following steps:
1) accurately take the normal spiral algae powder of below 100 orders or ultra micro Spirulina powder in agitator, then add Non-transgenic soybean oil, uniform stirring mixes;
2) mixture after stirring is ground in colloid mill, then slough the gas in material at vacuum tank, capsule Dissolve things inside can be obtained;
3) by gelatin, glycerol and purified water, in adding glue tank, glue is changed;
4) glue and capsule Dissolve things inside batching are extruded qualified soft capsule through pellet press, 0.8g/ grain;
5) with edible ethanol cleaning soft capsule surface oil;
6) soft capsule is put into drying rotating cage inner drying.
6. the ultra micro Spirulina powder that method is obtained as claimed in claim 1 or 2, it is characterized in that, in described ultra micro Spirulina powder, protein content is not less than 60.4 g/100g, and β-carotene carotene content is not less than 320 mg/100g.
7. the ultra micro Spirulina powder that method obtains as claimed in claim 1 or 2 is being prepared radioprotective, is being protected the liver and strengthen the application in immune drug or health product.
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| CN108420069A (en) * | 2018-03-23 | 2018-08-21 | 吉林农业大学 | A kind of beauty treatment whitening health-nutrition powder and its production method |
| CN108743892A (en) * | 2018-06-15 | 2018-11-06 | 海王（湖北）中医药研究总院有限公司 | The preparation method and applications of " Shengyang Yiwei Decoction " side's Chinese medical extract |
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