CN103230419A - Nitrogen-gas-protected cordyceps sinensis low-temperature ultrafine crushing processing method - Google Patents
Nitrogen-gas-protected cordyceps sinensis low-temperature ultrafine crushing processing method Download PDFInfo
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Abstract
The invention relates to a cordyceps sinensis crushing method, and specifically relates to a nitrogen-gas-protected cordyceps sinensis low-temperature ultrafine crushing processing method. According to the invention, nitrogen gas is adopted as the protection gas, and cordyceps sinensis is subjected to ultrafine crushing under a temperature of -20 DEG C. With the method, on the one hand, crushing time can be effectively reduced; and on the other hand, certain heat and oxygen sensitive effective components of cordyceps sinensis can be prevented from loss. Therefore, cordyceps sinensis preparation quality can be improved.
Description
Technical field
The invention belongs to the Cordyceps machining technology, especially a kind of processing method of nitrogen protection Cordyceps superfine comminution at low temperature.
Background technology
Cordyceps is fried in shallow oil soup or is stewed clothes mostly being traditionally, owing to do not break the cell wall of Cordyceps, effective ingredient is difficult to stripping, and human body is to its absorption rate less than 10%.Be to improve the utilization ratio of Cordyceps, increase human body to the absorption of active ingredients of cordyceps sinensis, effective method is after Cordyceps is pulverized, and takes after making dosage form products such as tablet, capsule, pill, medicated wine.Therefore, being crushed into of Cordyceps influenced one of the key link of Cordyceps product quality.
Pulverize existing a plurality of patented technologies at the former grass of Cordyceps.As patent CN1325728, adopt polishing twice, to crossing the 50-60 order, superfine grinding to 300 order is with carefully again with raw material corase grind.On this basis, patent CN101019898 adopts the method that polypide and Stroma are pulverized respectively, can obtain particle diameter at 2000 orders with thin microgranule.Above method is directly pulverized Cordyceps, or carries out pulverizing after the simple separate tissue (as polypide and Stroma are separated) again.The advantage of this disintegrating process is can be broken abundant with the former grass meal of Cordyceps, realizes superfine powder particle diameter product, improves the utilization ratio of Cordyceps.But there are two point defects in this disintegrating process: one, crushing process carries out at normal temperatures, the temperature that violent crushing process causes raises, can cause a lot of nutritional labelings in the Cordyceps, as degeneration or the volatilization of cordycepic acid, cordycepin, Cordyceps polysaccharide, Chinese caterpillar fungus polypeptide, protein, aminoacid, various active enzyme and other more than 40 kinds of volatile material etc.; Its two, crushing process is directly pulverized in air, the micropowder that obtains is exposed in the air, some effective ingredient such as Chinese caterpillar fungus polypeptide, protein, aminoacid and multivitamin are easily by airborne dioxygen oxidation inactivation.
At present, pulverize in the machining technology at Cordyceps, ultramicronising is pulverized the focus that remains this field process modification and lifting, but the problem of the active ingredients of cordyceps sinensis loss that pulverizing brings for ultramicronising does not cause enough attention as yet.Existing breaking method is difficult to avoid temperature to raise and the problem of the loss of effective components that oxidation brings, and can not satisfy the public to demand healthy, high-quality Cordyceps product.
Summary of the invention
The present invention be directed to the deficiency of above-mentioned prior art, a kind of processing method of nitrogen protection Cordyceps superfine comminution at low temperature is provided, it is characterized in that: under nitrogen protection, Cordyceps is carried out superfine comminution at low temperature.
Operation sequence of the present invention is as follows:
1, the drying of nitrogen
Be that 99.9% nitrogen carries out drying by drying system with purity, dry back nitrogen moisture content should be lower than 1%, to avoid bringing moisture into crushing system.
2, the feeding of the interpolation of Cordyceps raw material and nitrogen
Cordyceps Cordyceps raw material is put into the crushing cylinder of pulverizer, speed feeding drying nitrogen with 2L/min is full of whole crushing cylinder, continue the logical about 1min of nitrogen, discharge residual air in the cylinder, detect oxygen content with the oxygen detection instrument and be lower than 1% when following, close air bleeding valve earlier, close intake valve again, stop logical nitrogen.
3, the pre-cooling of crushing system
With fridge with crushing cylinder pre-cooling 1h to-20 ℃.
4, the control of the pulverizing of Cordyceps and powder particle diameter
Open the pulverizer switch, begin to pulverize.By the pulverizing time being set and pulverizing the powder particle diameter that frequency is controlled Cordyceps.
The present invention adopts drying nitrogen to protect gas as raw material pulverizing, under-20 ℃ Cordyceps is pulverized.Under nitrogen protection, aweto micropowder can be avoided contacting with oxygen, so the material of some easy oxidations has obtained protection in the Cordyceps.At low temperatures, raw material impact flexibility, percentage elongation reduce, be fragility, its interior tissue adhesion reduces, when having certain impact power, and more fragile beading, thereby reduced the pulverizing time, handle at low temperatures simultaneously, can avoid in the crushing process because the degeneration inactivation of effective ingredient, especially thermal sensitivity composition that the temperature rising brings.
Adopt the breaking method of introducing among the present invention be applicable to the processing powder particle diameter from 500 orders to 2000 orders with thin Cordyceps powder; because in whole grinding and processing process; the effective ingredient of Cordyceps has obtained sufficient protection; the Cordyceps powder that obtains is at total leachable; compare the result that room temperature is pulverized in air on the dissolution of cordycepic acid, cordycepin, Cordyceps polysaccharide, adenosine and improve a lot, for the Cordyceps preparation of producing health, high-quality provides assurance.
The specific embodiment
Embodiment one:
The Cordyceps raw material is put into the crushing cylinder of pulverizer, the purity that feeds after the dried with the speed of 2L/min is that 99.9% nitrogen is full of whole crushing cylinder, continue the logical about 1min of nitrogen, discharge residual air in the cylinder, detect oxygen content with the oxygen detection instrument and be lower than 1% when following, close air bleeding valve earlier, close intake valve again, stop logical nitrogen; Open fridge, begin after crushing cylinder being pre-chilled to-20 ℃ to pulverize, should keep in the crushing process being malleation in the crushing cylinder, prevent air admission.The different pulverizing time is set and pulverizes frequency, the sub-sieve powder particle diameter is that 500 orders, 1000 orders, 2000 orders are with thin Cordyceps powder respectively.
The difference that below compares this method and the main effective ingredient dissolution of different-grain diameter Cordyceps powder that the room temperature processing obtains in air.Adopt following method that sample is carried out labelling: this method is pulverized the powder particle diameter obtain and is respectively 500 orders, 1000 orders, 2000 purpose Cordyceps powders and is labeled as " excellent 500 ", " excellent 1000 ", " excellent 2000 " respectively; Room temperature is pulverized the powder particle diameter obtain and is respectively 500 orders, 1000 orders, 2000 purpose Cordyceps powders and is labeled as " normal 500 ", " normal 1000 ", " normal 2000 " respectively in air.
1, total leachable determination of dissolution rate
Accurately take by weighing " normal 500 ", " normal 1000 ", " normal 2000 ", " excellent 500 ", " excellent 1000 ", " excellent 2000 " each 5g (is accurate to 0.00001g, establish parallel sample for every group, results averaged) in the alembic of 250ml, add 37 ℃ of distilled water 100ml, and place 37 ℃ ± 1 water-bath, water-bath 60min gets 50ml filtrate and measures total leachable quality.The total material of the Cordyceps powder dissolution in time of different breaking method processing sees Table 1.
The dissolution (g) of the total material of Cordyceps powder of the different breaking method processing of table 1
| The sample title | Normal 500 | Excellent 500 | Normal 1000 | Excellent 1000 | Normal 2000 | Excellent 2000 |
| Dissolution (g) | 0.18210 | 0.18920 | 0.21928 | 0.23523 | 0.33086 | 0.35742 |
The total material determination of dissolution rate of the Cordyceps powder result of different breaking method processing shows, adopt this method to pulverize the total material dissolution of Cordyceps powder that obtains and all be higher than the result that the room temperature pulverizing obtains in the air, and powder particle diameter is more little more obvious, when powder particle diameter reaches 2000 orders when thin, the result (0.33086g) that total material dissolution (0.39742g) of this method is pulverized than room temperature in air exceeds 8%.
2, the mensuration of cordycepic acid
2.1. chromatographic condition
Chromatographic column is the C18 of Chinese nation post (4.6mm * 250mm, 5 μ m), 30 ℃ of column temperatures.Mobile phase: V (acetonitrile): V (water)=80: 20, isocratic elution, flow velocity 0.8mL/min.Detector is waters2414 differential refraction detector (RID).
2.2. standard solution preparation
Accurately take by weighing the cordycepic acid standard sample, water standardize solution, each 5mL of cordycepic acid titer of preparation 0.1,0.3,0.5,0.7,0.9,1.1mg/mL.Respectively getting 10 μ L sample introduction analyses, is longitudinal and transverse coordinate drawing standard curve with peak area, mass concentration, obtains equation of linear regression: Y=1.28 * 10
5X-4396.88, r=0.9992, the range of linearity is 0.15～0.9mg/mL.
2.3. sample pretreatment
The filtrate of will be in the above-mentioned test 1 measuring total dissolution, with centrifuge with the quick centrifugal 5min of 15000rpm/min after, with 0.45 μ m filtering with microporous membrane, filtrate is analyzed for HPLC.
2.4. sample analysis
Draw each 10 μ L of standard sample and sample solution and inject high performance liquid chromatography, the record chromatogram, external standard method is with the content of cordycepic acid in the calculated by peak area sample.
Dissolution (the unit: mg/g) of the Cordyceps powder cordycepic acid of the different breaking method processing of table 2
| The sample title | Normal 500 | Excellent 500 | Normal 1000 | Excellent 1000 | Normal 2000 | Excellent 2000 |
| Dissolution | 14.28210 | 14.58920 | 16.51928 | 18.24923 | 21.43086 | 24.09742 |
The Cordyceps powder cordycepic acid determination of dissolution rate result of different breaking method processing shows, adopt this method to pulverize the Cordyceps mealworm oxalic acid dissolution that obtains and all be higher than the result that the room temperature pulverizing obtains in the air, and powder particle diameter is more little more obvious, when powder particle diameter is 500 orders, dissolution difference is not obvious, when reaching 2000 orders when thin, the result that the cordycepic acid dissolution of this method is pulverized apparently higher than room temperature in air exceeds 12.4%.
3, the mensuration of cordycepin
3.1. chromatographic condition
Chromatographic column is the C18 of Chinese nation post (4.6mm * 250mm, 5 μ m), 30 ℃ of column temperatures.Detector is diode array UV-detector (DAD), detects wavelength 260nm.Mobile phase: V (acetonitrile): V (water)=80: 20, flow velocity 0.8mL/min.
3.2. standard solution preparation
Accurately take by weighing cordycepin standard substance 2.5mg, to 100mL, be mixed with the standard solution that mass concentration is respectively 25 μ g/mL with methanol constant volume.Accurate absorption reference substance solution 1,4,8,12,16,20 μ L inject high performance liquid chromatograph, the record chromatogram.Be longitudinal and transverse coordinate drawing standard curve with peak area, mass concentration, obtain equation of linear regression: Y=7.38 * 10
5X-1968.1, R=0.9996, the range of linearity is 0.025～0.5 μ g;
3.3. sample pretreatment
The filtrate of will be in the above-mentioned test 1 measuring total dissolution, with centrifuge with the quick centrifugal 5min of 15000rpm/min after, with 0.45 μ m filtering with microporous membrane, filtrate is analyzed for HPLC.
3.4. sample analysis
Draw each 10 μ L of standard sample and sample solution and inject high performance liquid chromatography, the record chromatogram, external standard method is with content of cordycepin in the calculated by peak area sample.
The dissolution (mg/g) of the Cordyceps powder cordycepin of the different breaking method processing of table 3
| The sample title | Normal 500 | Excellent 500 | Normal 1000 | Excellent 1000 | Normal 2000 | Excellent 2000 |
| Dissolution | 0.01173 | 0.01165 | 0.01455 | 0.01554 | 0.01808 | 0.01997 |
The Cordyceps powder cordycepin determination of dissolution rate result of different breaking method processing shows, when powder particle diameter is 500 orders, adopt this method and the cordycepin dissolution that room temperature obtains in air not to have obvious difference, when reaching 2000 orders when thin, the result that the cordycepin dissolution of this method is pulverized apparently higher than room temperature in air exceeds 10.8%.
4, the mensuration of Cordyceps polysaccharide
4.1. reference substance liquid
Precision takes by weighing 105 ℃ of D-anhydrous glucose 0.005g that are dried to constant weight, and adding distil water dissolves and is diluted to scale in the 500mL volumetric flask, shakes up namely.
4.2. for test agent
Accurately take by weighing " normal 500 ", " normal 1000 ", " normal 2000 ", " excellent 500 ", " excellent 1000 ", " excellent 2000 " each 5g (being accurate to 0.00001g), be dissolved in 100mL 80% ethanol, 60 degree water-bath 1h, utilize the lipid component in the water alcohol method removal powder, centrifugal 20 minutes of 4000rpm, collecting precipitation utilizes the protein in sevage isolating protein method (chloroform and n-butyl alcohol) the removal sample, centrifugal 20 minutes of 4000rpm; The crude polysaccharides dissolved in distilled water that obtains concentrating is put standardize solution in the 100mI volumetric flask, shakes up, namely.
4.3. the drafting of phenol sulfuric acid process standard curve
From mother solution precision measure 0.5,3,5.5,8,10.5,13mL, be settled to 20mL with distilled water respectively, thereby obtain the standard glucose Concentraton gradient solution that concentration is 0.25,1.5,2.75,4,5.25,6.5 μ g/mL.Precision is measured above-mentioned gradient solution 2mL and is placed test tube respectively, add 5% phenol solution 2mL successively, concentrated sulphuric acid 8mL shakes up and places 10min, boiling water bath heating 15min, being cooled to room temperature, measuring absorbance A at 490nm wavelength place, is vertical coordinate with the absorbance A, concentration of glucose C is the abscissa coordinate, draw linear equation: (r=0.9993 n=6), has good linear relationship to Y=0.0087X+0.0354 in 0.25-6.5 μ g/mL scope.
4.4. the mensuration of chromogenic reaction and Cordyceps polysaccharide
Smart amount takes by weighing the above-mentioned test agent 2mL that supplies in test tube, adds 5% phenol solution 2mL successively, and concentrated sulphuric acid 8mL shakes up and places 10min, and boiling water bath 15min is cooled to room temperature, measures absorbance at 490nm wavelength place, and the substitution linear equation calculates concentration of glucose.Following formula calculates the percentage composition that each order of Cordyceps gets polysaccharide in the powder.Formula: ((C is concentration of glucose μ g/ml in the sample solution to the W% of C * D * f) to polysaccharide %=; D is the dilution factor of sample solution; F is conversion factor; W is example weight (μ g).
The dissolution (%) of the Cordyceps powder polysaccharide of the different breaking method processing of table 4
| The sample title | Normal 500 | Excellent 500 | Normal 1000 | Excellent 1000 | Normal 2000 | Excellent 2000 |
| Dissolution | 0.92 | 0.91 | 1.31 | 1.37 | 1.42 | 1.52 |
The Cordyceps powder polysaccharide determination of dissolution rate result of different breaking method processing shows, when powder particle diameter is 500 orders, adopt this method and the polysaccharide dissolution that room temperature obtains in air not to have obvious difference, when reaching 1000 orders and 200 orders when thin, the result that the cordycepin dissolution of this method is pulverized apparently higher than room temperature in air exceeds 4.5% and 7.0% respectively.
5, the mensuration of adenosine
5.1. chromatographic condition
Chromatographic column: chromatographic column is the C18 of Chinese nation post (4.6mm * 250mm, 5 μ m), 30 ℃ of column temperatures.Detector is diode array UV-detector (DAD), detects wavelength 260nm.
Mobile phase: phosphate buffer (0.125% dipotassium hydrogen phosphate mixes with potassium dihydrogen phosphate): methanol=92: 8; Flow: 1.0mL/min.
5.2. standard solution preparation
Precision takes by weighing the adenosine standard that is dried to constant weight and shines product 10mg in the 25ml volumetric flask, adds 90% dissolve with methanol and is mixed with the stock solution that contains 0.4mg/mL adenosine reference substance; The accurate absorption 0.5,1.5,2,2.5,3 of difference, 3.5mL stock solution, become with 90% methanol constant volume that adenosine concentration is 0.2,0.6,0.8,1,1.2, the reference substance solution of 1.4mg/mL, draw reference substance solution 10 μ L sample introductions, press condition determination and measure peak area, be vertical coordinate with the peak area, concentration is that abscissa carries out regression analysis, gets regression equation: Y=391.99X-198.7, r=0.9993, the range of linearity is 0.2～0.504ug/mL.
5.3. the processing of sample
Get and pulverize uniform sample an amount of (being accurate to 0.00001g) in the 50mL volumetric flask, add about 40mL water, supersound extraction 30min takes out and is cooled to room temperature, and water is settled to scale again.Get 2mL sample liquid, behind the quick centrifugal 5min of 15000rpm/min, with 0.45 μ m filtering with microporous membrane, filtrate is analyzed for HPLC.
5.4. sample analysis
Draw each 10 μ L of standard sample and sample solution and inject high performance liquid chromatography, the record chromatogram, external standard method is with content of cordycepin in the calculated by peak area sample.
The dissolution (mg/g) of the Cordyceps powder adenosine of the different breaking method processing of table 5
| The sample title | Normal 500 | Excellent 500 | Normal 1000 | Excellent 1000 | Normal 2000 | Excellent 2000 |
| Dissolution | 0.14604 | 0.14584 | 0.17359 | 0.17420 | 0.19319 | 0.19208 |
This method does not have obvious difference with the adenosine dissolution that room temperature obtains in air, be 500 orders and 2000 orders when thin at powder particle diameter, the result that the cordycepin dissolution of this method is pulverized a little less than room temperature in air is when powder particle diameter is 1000 orders when thin, then slightly high, but difference is not obvious.Illustrate that this method is little to the dissolution rate influence of adenosine.
Above experimental result shows, the Cordyceps powder that adopts this method to obtain is compared the result that room temperature is pulverized in air at the dissolution of total leachable, cordycepic acid, cordycepin, Cordyceps polysaccharide and is improved a lot, illustrate that this method can effectively avoid nutrient loss, improve the quality of products.
Claims (6)
1. the pulverize at low temperature method of a nitrogen protection Cordyceps is characterized in that may further comprise the steps:
A puts into the crushing cylinder of pulverizer with the Cordyceps raw material, feeds nitrogen as protection gas, and makes nitrogen be full of whole crushing cylinder;
B opens fridge, and crushing cylinder is pre-chilled to subzero low temperature;
C opens pulverizer, begins to pulverize, and keeping in the crushing process in the crushing cylinder is that malleation is to prevent air admission; Cut in crushing process, open nitrogen intake valve and return valve, make nitrogen under the air compressor machine effect, from pulverizer, get back to drying system through filter, reuse as protection gas after the dried, form closed cycle.
2. according to the pulverize at low temperature method of the Cordyceps of nitrogen protection described in the claim 1, it is characterized in that described nitrogen is 99.9% nitrogen for carry out dry purity by drying system, dry back nitrogen moisture content should be lower than 1%.
3. according to the pulverize at low temperature method of the Cordyceps of nitrogen protection described in the claim 1, it is characterized in that, described
Feeding the nitrogen steps concrete operations among the step a is: the speed feeding drying nitrogen with 2L/min is full of whole crushing cylinder, continues the logical about 1min of nitrogen, discharges residual air in the cylinder, detect oxygen content with the oxygen detection instrument and be lower than 1% when following, close air bleeding valve earlier, close intake valve again, stop logical nitrogen.
4. according to the pulverize at low temperature method of the Cordyceps of nitrogen protection described in the claim 1, it is characterized in that, described
The temperature that the crushing cylinder pre-cooling reaches among the step b is-20 ℃.
5. according to the pulverize at low temperature method of any described nitrogen protection Cordyceps among the claim 1-4, it is characterized in that described pulverizing is micronizing.
6. the pulverize at low temperature method of nitrogen protection Cordyceps according to claim 5 is characterized in that: the micronizing particle diameter is 500 orders to 2000 orders with carefully.
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| CN104177506A (en) * | 2014-07-18 | 2014-12-03 | 上海天嵩生物科技有限公司 | Preparation method of Hirsutella sinensis mycelia polysaccharide |
| CN104543257A (en) * | 2015-02-04 | 2015-04-29 | 彭正中 | Health tea and making process thereof |
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| CN102784174A (en) * | 2012-08-19 | 2012-11-21 | 陈玉龙 | Process for preparing Chinese caterpillar fungus micropowder and preparation thereof |
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| CN102784174A (en) * | 2012-08-19 | 2012-11-21 | 陈玉龙 | Process for preparing Chinese caterpillar fungus micropowder and preparation thereof |
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| CN104177506A (en) * | 2014-07-18 | 2014-12-03 | 上海天嵩生物科技有限公司 | Preparation method of Hirsutella sinensis mycelia polysaccharide |
| CN104177506B (en) * | 2014-07-18 | 2016-09-28 | 上海天嵩生物科技有限公司 | A kind of preparation method of Hirsutlla sinensis mycelium polysaccharides |
| CN104543257A (en) * | 2015-02-04 | 2015-04-29 | 彭正中 | Health tea and making process thereof |
| CN106165894A (en) * | 2016-07-20 | 2016-11-30 | 吉林农业大学 | One reconstitutes instant type multiple eating bacterium composite nutrition powder and production method thereof |
| CN106174548A (en) * | 2016-07-20 | 2016-12-07 | 吉林农业大学 | Reconstitute instant type Auricularia Semen Euryales composite nutrition powder and production method thereof |
| CN106174455A (en) * | 2016-07-20 | 2016-12-07 | 吉林农业大学 | Reconstitute instant type Tremella Semen Coicis composite nutrition powder and production method thereof |
| CN107929114A (en) * | 2017-12-21 | 2018-04-20 | 隐纱化妆品有限公司 | The extracting method of Cordyceps extract used for cosmetic |
| CN108851030A (en) * | 2018-08-24 | 2018-11-23 | 江西济民可信药业有限公司 | A kind of preparation method for the ergosterol and adenosine dissolution rate improving double capsules that escape |
| CN108851030B (en) * | 2018-08-24 | 2021-12-14 | 江西济民可信药业有限公司 | Preparation method for improving dissolution rates of ergosterol and adenosine of Shuangyi capsule |
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Application publication date: 20130807 |