CN1152439A - Preparation process for full composition pearl crude liquid and pearl powder - Google Patents
Preparation process for full composition pearl crude liquid and pearl powder Download PDFInfo
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- CN1152439A CN1152439A CN96119665A CN96119665A CN1152439A CN 1152439 A CN1152439 A CN 1152439A CN 96119665 A CN96119665 A CN 96119665A CN 96119665 A CN96119665 A CN 96119665A CN 1152439 A CN1152439 A CN 1152439A
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Abstract
The preparative process firstly uses the lactic acid to expand and replace the medicinal pearl to separate out calcium lactate liquid and keratin. The calcium lactate liquid is used to obtain powder calcium lactate through the process of adding shell powder, heating, cooling, filtering and crystallising. The keratin is passed through the zymolysis by using compound zyme of elastase etc. The zymolytic liquid and powder calcium lactate are mixed to obtain the full composition pearl powder and pearl crude liquid. Said process is simple, the reaction condition is moderate and beneficial to prevent the active component to be damaged. By using said process, the full component of pearl can be inverted into comprehensive mixture-pearl crude powder or crude liquid, the crude liquid can be prepared into different concentration ones by adding distilled water for using in the production of pearl nutritive product.
Description
The present invention relates to a kind of technology of utilizing effective ingredient in the enzyme enzymolysis Margarita to prepare pearl crude liquid or Margarita powder.
Margarita is each your Chinese medicine since ancient times, and modern ESR technology has proved that Margarita has the ability of removing ultra-oxygen anion free radical and hydroxyl radical free radical, has function in delaying senility really.
The main body chemical analysis of Margarita is a calcium carbonate, and it accounts for 92% of gross weight, and calcium carbonate is slightly soluble in water and is difficult for being absorbed by human body.Also contain 18 kinds of protein aminoacid in the Margarita, 3 kinds of nonprotein amino acid and various trace elements, and newfound clethra loosestrife root or herb quinoline compounds, still undeveloped active polypeptide compounds etc., these materials are almost surrounded by calcium carbonate, even wear into fine powder, also have only sub-fraction to come out, can be absorbed seldom by the people, the hydrolyzed pearl effective component extracting is paid attention to by people for this reason.
The hydrolyzed pearl method of being taked now is just like disclosed High Temperature High Pressure pure water Hydrolyze method such as CN1046283A, disclosed acid-hydrolysis method such as CN1078891A, and all there is deficiency in these two kinds of Hydrolyze method, so substituted by enzyme hydrolysis method.CN1080323A adopts the single enzyme solution, it is through rare HCl pickling with Margarita powder, after softening, get enzymolysis solution with pepsin, papain or trypsin digestion, then with Carnis Anodonta seu crislaria add water, Ovum Gallus domesticus album adsorb behind the enzyme-added enzymolysis with above-mentioned enzymolysis solution merge pearl crude liquid." the process modification research of tradition " Margarita hydrolyzed solution " " (seeing the journal vol of Zhanjiang Aquatic Production College, 14 ND, 2 Dee1994, P57-60) adopts complex enzyme zymohydrolysis, it is to mix making beating behind Margarita powder decalcification, the Pinctada margaritifera whole viscera eliminating sargassum smell, then use earlier papain, the back trypsin digestion, enzyme denaturing, filtration, decolouring, embedding then, sterilize pearl crude liquid, the employing compound enzyme of saying so, actual is two kinds of single enzymes enzymolysis successively, the total amino acid content that extracts has only 465mg/100ml.
Purpose of the present invention aims to provide a kind of with complex enzyme zymohydrolysis extraction Margarita whole part, the technology of preparation Margarita powder and pearl crude liquid.Adopt this technology, Margarita need not worn into powder, and the whole effective ingredient in the Margarita can not only keep, and is present in former powder of Margarita or the pearl crude liquid, in order to absorption of human body with active ortho states.
The implementation of the object of the invention is: complete-component pearl powder and pearl crude liquid preparation technology,
1, medicinal Margarita is cleaned, and be placed on its weight ratio be 1: soak expanded, displacement in 3-5 days in 30% lactic acid of 5-6, inorganic calcium becomes calcium lactate liquid, heat 60 ℃-75 ℃ 1 hour, further react, then separate calcium lactate liquid and angle glutelin;
2, the conch meal of adding 2-5% in calcium lactate liquid transfers pH value to 6.4-6.8, stirs neutralizing acid, then is heated to 60 ℃-75 ℃ half an hour, filters cooling, gets the calcium lactate coarse crystallization;
3, coarse crystallization adding distil water was heated to 60 ℃-75 ℃ half an hour, and cooling recrystallization isolated by filtration, drying, pulverizing get pure lactic acid calcium powder;
4, get the angle glutelin, be that 15% amount adds water and gets solution by weight, add the pancreas peptide E enzyme of its weight 1.2-1.6%, the chymase of 0.4-0.6%, the serinase of 0.4-0.6% in solution, the accent pH value is 6.5-7.5, is incubated 40 ℃-55 ℃, enzymolysis 3-4 hour;
5, get enzymolysis solution and boil enzyme denaturing half an hour, filtrate is got in pressure filtration,
6, enzymolysis filtrate and pure lactic acid calcium powder are mixed after, full composition pearl crude liquid, again fill sterilize product, or enzymolysis filtrate is sprayed onto on the pure lactic acid calcium powder, behind the mixing 40 ℃-50 ℃ vacuum drying 30-40 minute, the complete-component pearl powder.
The present invention is described in detail in detail with reference to the accompanying drawings.
Fig. 1 process chart of the present invention
Fig. 2 alanine maximum absorption wavelength sketch map
Fig. 3 process conditions factor and total amino acids relation with contents figure
With reference to accompanying drawing, the present invention adopts the medicinal pearl that meets 1990 editions one one 199 pages of Chinese Pharmacopoeias, and pearl is, displacement expanded by lactic acid earlier, isolates calcium lactate liquid and angle glutelin, angle glutelin pancreas peptide E enzyme, chymotrypsin, serinase complex enzyme hydrolysis. Adopt the relative acid hydrolysis of this technology, single enzyme hydrolysis to be excellent, specifically relatively see Table 1:
Table 1
| Project | Acid hydrolysis | The single enzyme hydrolysis | Complex enzyme for hydrolyzing |
| Material is processed | Pearl powder | Pearl powder | Pearl need not pulverized |
| Decalcification | Hydrochloric acid | Hydrochloric acid | Organic acid |
| Catalyst | Strong acid | Single vegetable protein hydrolase | The complex enzyme system that is formed by the animal and plant proteolytic enzyme |
| Hydrolysis temperature | 120℃ | 65℃ | 40-55℃ |
| Time | 24 hours | 7-8 hour | 3-4 hour |
| Efficient | 1-2 time | Need repeatedly be hydrolyzed more than 2 times, filter and process the normal difficulty that takes place | Only need once, filter smoothly |
| The amino acid kind | 3 indifferences | ||
| Total amino acid content | Both indifferences | Improve more than 3 times | |
| The inorganic acid Liquid Residue | Have | Do not have | Do not have |
| Active ingredient | Calcium is lost some active ingredient may be destroyed | Calcium is lost and is not damaged | The advantage calcium that keeps single enzymolysis is not lost, and comprises the full composition of pearl |
As seen, adopt this technology enzyme hydrolysis temperature low from table 1, the time is short, not only can all extract the whole active ingredients in the pearl, and also make it be activated state.
With the enzymolysis liquid of single enzyme, complex enzyme enzyme hydrolysis gained, with the content of colorimetric method for determining total amino acid, specifically test as follows:
One, instrument and reagent
Complex enzyme hydrolysis pearl crude liquid: this technology preparing product
Reference substance: alanine A.R.
It is pure that ninhydrin, ethylene glycol, normal propyl alcohol, titanium trichloride are analysis
Acetate buffer solution (PH5): 0.2mol/l NaAC liquid 7.0ml+0.2mol/lHAC liquid 3.0ml
756MC type spectrophotometer: Shanghai is analyzed and is tried to clamor three factories
Two, experimental section
1, the preparation of reagent and contrast liquid:
Ninhydrin solution: ethylene glycol 17.5ml, ninhydrin 5.0%, acetate buffer solution (PH5) 75ml, titanous chloride. 1.0ml, mix homogeneously, it is standby to put refrigerator cold-storage;
Alanine contrast liquid: the alanine reference substance 2.64mg that precision takes by weighing dry constant weight puts in the 25ml measuring bottle, adds water to scale, shakes up promptly to get (105.6ng/ml) contrast liquid.
2, measure the selection of wavelength:
Precision is measured alanine contrast liquid 2.5ml and is put in the 25ml measuring bottle, add water 7.5ml, ninhydrin solution 2.5ml, boiling water bath insulation 15min takes out the flowing water cooling, treat to add normal propyl alcohol behind the colour stable: the solution of water=1: 1 is to scale, shake up, place 10min, between the 500-600nm wavelength, scan, with alanine is the retinue solution work blank of " 0 ", and the result has absorption maximum (as Fig. 2) at the 565nm place.
3, the preparation of standard curve:
Precision is measured alanine contrast liquid (105.6ng/ml) 1.5,2.0,2.5,3.0 3.5ml puts respectively in the 25ml measuring bottle, adds water to 10ml, ninhydrin solution 2.5ml, be incubated 15min in the boiling water bath, take out the flowing water cooling, add normal propyl alcohol: the solution of water=1: 1 is to scale, shake up, placing 10min, measure trap A value in accordance with the law at 565nm wavelength place, is the retinue solution work blank of " 0 " with alanine.Record the A value and be respectively 0.375,0.528,0.680,0.835,0.988.Getting equation through rectilinear regression is:
A＝-0.085+0.0726I????γ＝0.9999
4, average recovery is measured:
Precision is measured sample 1ml and is put in the 50ml measuring bottle, adds water to scale, shakes up, and precision is measured 1ml and put in the 25ml measuring bottle totally 7 parts again.Wherein 5 parts of each accurate alanine reference substance liquid a certain amount of (seeing Table 1) that add of difference are large down from being added to the operation of 10ml method according to standard curve, measure the A value, substitution regression equation calculation content.The results are shown in Table 2: table 2
Average recovery rate is: 96.66%
| Sample number | The sample amount of recording (ug) | Addition (ug) | Record total amount (ug) | The response rate (%) |
| ????1 ????2 ????3 ????4 ????5 | ????155.2 ????155.2 ????155.2 ????155.2 ????155.2 | ????52.8 ????52.8 ????105.6 ????105.6 ????105.6 | ????207.4 ????205.8 ????258.3 ????254.8 ????257.2 | ????98.86 ????95.83 ????97.63 ????94.32 ????96.59 |
5, sample determination:
Precision is measured each 1ml of sample 1,2, No. 3, puts respectively in the 10ml measuring bottle, adds water to scale, shakes up, and is standby; Precision is measured each 1ml of sample 4,5,6,7,8, No. 9, puts respectively in the 50ml measuring bottle, adds water to scale, shakes up, standby.
Wherein 1,2, No. 3 sample is a carase, and dosage is 2.5%, 4,5, No. 6 sample trypsin, and dosage is that 3%, 7,8, No. 9 sample is three kinds of compound enzymes such as pancreas peptide E enzyme.
Precision is measured above-mentioned each 1ml of 1-9 sample diluting liquid, puts respectively in the 25ml measuring bottle, plays the method operation according to self-watering under the standard curve item to 10ml, mensuration A value, and result of calculation sees Table 3:
Table 3
As seen from the table, adopt complex enzyme zymohydrolysis, by the total amino acids content height that is extracted in the glutelin of angle.
2,3 significance test
Experimental result adopts extreme difference to calculate and variance analysis (F
0.1 (2.2)=1, F
0.05 (2.2)=9, F
0.01 (2.2)=99), concrete outcome sees Table 4.
Table 4
| Soruces of variation | Sum of deviation square | Degree of freedom | Mean square | The F value | Significance | Extreme difference |
| A B C error | ????24.214 ????2.406 ????1.270 ????0.087 | ????2 ????2 ????2 ????2 | ??12.107 ???1.203 ???0.640 ???0.044 | ??275.159 ???27.341 ???14.545 | ??＜0.01 ??＜0.05 ??＜0.10 | ??3.718 ??1.264 ??0.893 ??0.238 |
As seen from the table: 1. factor A (combination of enzyme) all has the highly significant effect to every index; 2. factor B (concentration of angle glutelin) has remarkable effect; 3. factor C (reaction temperature) has certain effect.
2,4 enzymatic hydrolysis conditions is preferred:
With total amino acids content K is ordinate, is abscissa with A, B, C three factors, its graph of a relation as shown in the figure, as seen from the figure: A factor: K
3＞K
2＞K
1, B factor: K
1＞K
2＞K
3, C factor: K
3＞K
2＞K
1, therefore most preferred enzymatic hydrolysis condition is A
3B
1C
3, promptly the three kinds of enzymes that are combined as of enzyme make up, and the concentration of angle glutelin is 15%, and reaction temperature is 60 ℃.
The pearl crude liquid of employing explained hereafter of the present invention is the total amino acids content height of literature value quite, specifically relatively sees Table 5.
Table 5
| Aminoacid title enzymolysis product literature value mg/100ml mg/100ml | Aminoacid title enzymolysis product literature value mg/100ml mg/100ml |
| Aspartic acid ASP 261.63 201.50 threonine THR 108.50 41.20 serine SER 124.76 151.90 glutamic acid Q U 411.43 105.70 glycine Q Y 160.25 356.30 alanine ALA 140.35 384.20 cystine EYS 32.90 80.50 little propylhomoserin VAL 115.95 108.00 methionine MET 56.17 92.30 | Isoleucine ILE 106.42 66.40 leucine LEU 197.96 124.60 tyrosine TYR 92.48 74.20 phenylalanine PHE 90.36 171.30 lysine LYS 193.51 86.20 histidine HIS 40.36 19.50 arginine ARG 235.88 89.00 proline PRO 88.92 46.40 summations 2459.20 2199.20 |
Annotate: literature value is selected from Huang autumn Oriolus chinensis diffusus, Zhang Min, Tu Chengshui: Margarita is differentiated and quality is inquired into." pharmaceutical analysis " magazine 13 (4): 266,1993.
During the enzyme-added enzymolysis of angle glutelin solution, also can add two kinds in above-mentioned three kinds, i.e. pancreas peptide E enzyme and chymase, or pancreas peptide E enzyme and serinase, dosage dosage during with three kinds of enzymes.Add two kinds of enzyme enzymolysis, effect is better than single enzyme, but is slightly poorer than three kinds of compound enzymes.
Direct drug injection thing Margarita of the present invention is a raw material, need not pulverize, and technical process is simple, reaction condition gentleness, the destruction that helps preventing active component.Adopt this technology, various inorganic salt compositions in the Margarita can be become solubility micromolecule organic salt, isolating angle glutelin is aminoacid and little peptide with the complex enzyme zymohydrolysis, make the whole part of Margarita transfer comprehensive mixture to---former powder of Margarita or stock solution, stock solution can be mixed with the solution of variable concentrations by required adding distil water, is used for the production of pearl nutritional goods.
Claims (3)
1, full composition pearl crude liquid or Margarita powder preparation technology is characterized in that specific embodiment is:
1) medicinal Margarita is cleaned, and be placed on its weight ratio be 1: soak expanded, displacement in 3-5 days in 30% lactic acid of 5-6, inorganic calcium becomes calcium lactate liquid, heat 60 ℃-75 ℃ 1 hour, further react, then separate calcium lactate liquid and angle glutelin,
2) conch meal of adding 2-5% in calcium lactate liquid transfers pH value to 6.4-6.8, stirs neutralizing acid, then is heated to 60 ℃-75 ℃ half an hour, filters cooling, gets the calcium lactate coarse crystallization;
3) coarse crystallization adding distil water was heated to 60 ℃-75 ℃ half an hour, and cooling recrystallization isolated by filtration, drying, pulverizing get pure lactic acid calcium powder;
4) get the angle glutelin, be that 15% amount adds water and gets solution by weight, add the pancreas peptide E enzyme of its weight 1.2-1.6%, the chymase of 0.4-0.6%, the serinase of 0.4-0.6% in solution, the accent pH value is 6.5-7.5, is incubated 40 ℃-55 ℃, enzymolysis 3-4 hour;
5), get enzymolysis solution and boil enzyme denaturing half an hour, filtrate is got in pressure filtration,
6), enzymolysis filtrate and pure lactic acid calcium powder mixed after, full composition pearl crude liquid, again fill sterilize product, or enzymolysis filtrate is sprayed onto on the pure lactic acid calcium powder, behind the mixing 40 ℃-50 ℃ vacuum drying 30-40 minute, the complete-component pearl powder.
2, technology according to claim 1 is characterized in that adding the pancreas peptide E enzyme of its weight 1.2-1.6%, the coagulation protease trypsin of 0.4-0.6% in the glutelin solution of angle, the accent pH value is 6.5-7.5, is incubated 40 ℃-55 ℃, enzymolysis 3-4 hour.
3, technology according to claim 1 is characterized in that adding the pancreas peptide E enzyme of its weight 1.2-1.6%, the serinase of 0.4-0.6% in the glutelin solution of angle, the accent pH value is 6.5-7.5, is incubated 40 ℃-55 ℃, enzymolysis 3-4 hour.
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| CN96119665A CN1063490C (en) | 1996-10-25 | 1996-10-25 | Preparation process for full composition pearl crude liquid and pearl powder |
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| CN96119665A CN1063490C (en) | 1996-10-25 | 1996-10-25 | Preparation process for full composition pearl crude liquid and pearl powder |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101100689B (en) * | 2007-08-07 | 2010-06-23 | 海南京润珍珠生物技术股份有限公司 | Method for preparing pearl active peptide |
| CN104905242A (en) * | 2014-03-14 | 2015-09-16 | 浙江欧诗漫生物股份有限公司 | A method for preparing pearl separated pearl soluble edible calcium and pearl compound whitening factor solution |
| TWI597017B (en) * | 2015-01-15 | 2017-09-01 | Osmun Biological Co Ltd | Method for preparing pearl protein and water-soluble pearl protein and acid-soluble pearl protein prepared by the method |
| CN107712587A (en) * | 2017-10-17 | 2018-02-23 | 广州润虹医药科技股份有限公司 | A kind of anti-oxidant anti-aging nutrient powder and preparation method thereof |
| CN110240627A (en) * | 2019-07-19 | 2019-09-17 | 浙江长生鸟健康科技股份有限公司 | A method of small active peptides being extracted from pearl powder using complex enzyme |
| CN112674174A (en) * | 2021-01-29 | 2021-04-20 | 刘刚 | Milk containing pearl extract and preparation method thereof |
| CN114403437A (en) * | 2022-01-27 | 2022-04-29 | 海南久常制药有限公司 | A method for preparing Margarita powder |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1025549C (en) * | 1990-12-06 | 1994-08-03 | 王四明 | Prepn. for series products of water soluble full component pearl powder |
| CN1032593C (en) * | 1991-02-04 | 1996-08-21 | 李新建 | Method for preparation of liq. pearl from solid pearl |
-
1996
- 1996-10-25 CN CN96119665A patent/CN1063490C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101100689B (en) * | 2007-08-07 | 2010-06-23 | 海南京润珍珠生物技术股份有限公司 | Method for preparing pearl active peptide |
| CN104905242A (en) * | 2014-03-14 | 2015-09-16 | 浙江欧诗漫生物股份有限公司 | A method for preparing pearl separated pearl soluble edible calcium and pearl compound whitening factor solution |
| WO2015135346A1 (en) * | 2014-03-14 | 2015-09-17 | 浙江欧诗漫生物股份有限公司 | Method for separating and preparing pearl extract from pearls |
| EP3108873A4 (en) * | 2014-03-14 | 2016-12-28 | Osmun Biological Co Ltd | Method for separating and preparing pearl extract from pearls |
| TWI597017B (en) * | 2015-01-15 | 2017-09-01 | Osmun Biological Co Ltd | Method for preparing pearl protein and water-soluble pearl protein and acid-soluble pearl protein prepared by the method |
| CN107712587A (en) * | 2017-10-17 | 2018-02-23 | 广州润虹医药科技股份有限公司 | A kind of anti-oxidant anti-aging nutrient powder and preparation method thereof |
| CN110240627A (en) * | 2019-07-19 | 2019-09-17 | 浙江长生鸟健康科技股份有限公司 | A method of small active peptides being extracted from pearl powder using complex enzyme |
| CN110240627B (en) * | 2019-07-19 | 2023-06-27 | 浙江长生鸟健康科技股份有限公司 | Method for extracting small molecule active peptide from pearl powder by utilizing complex enzyme |
| CN112674174A (en) * | 2021-01-29 | 2021-04-20 | 刘刚 | Milk containing pearl extract and preparation method thereof |
| CN114403437A (en) * | 2022-01-27 | 2022-04-29 | 海南久常制药有限公司 | A method for preparing Margarita powder |
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