CN101508715A - Extraction and purification process for cordycepin in cordyceps militaris link - Google Patents
Extraction and purification process for cordycepin in cordyceps militaris link Download PDFInfo
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- CN101508715A CN101508715A CNA2009100261138A CN200910026113A CN101508715A CN 101508715 A CN101508715 A CN 101508715A CN A2009100261138 A CNA2009100261138 A CN A2009100261138A CN 200910026113 A CN200910026113 A CN 200910026113A CN 101508715 A CN101508715 A CN 101508715A
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- KQLDDLUWUFBQHP-UHFFFAOYSA-N Cordycepin Natural products C1=NC=2C(N)=NC=NC=2N1C1OCC(CO)C1O KQLDDLUWUFBQHP-UHFFFAOYSA-N 0.000 title claims abstract description 57
- OFEZSBMBBKLLBJ-BAJZRUMYSA-N cordycepin Chemical compound C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](CO)C[C@H]1O OFEZSBMBBKLLBJ-BAJZRUMYSA-N 0.000 title claims abstract description 57
- OFEZSBMBBKLLBJ-UHFFFAOYSA-N cordycepine Natural products C1=NC=2C(N)=NC=NC=2N1C1OC(CO)CC1O OFEZSBMBBKLLBJ-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 241001264174 Cordyceps militaris Species 0.000 title claims abstract description 37
- 238000000605 extraction Methods 0.000 title claims abstract description 22
- 238000000746 purification Methods 0.000 title claims abstract description 19
- 239000011347 resin Substances 0.000 claims abstract description 26
- 229920005989 resin Polymers 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 20
- 238000000926 separation method Methods 0.000 claims abstract description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 239000003480 eluent Substances 0.000 claims abstract description 5
- 238000002137 ultrasound extraction Methods 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 239000012488 sample solution Substances 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 238000005352 clarification Methods 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 7
- 150000004676 glycans Chemical class 0.000 abstract description 5
- 229920001282 polysaccharide Polymers 0.000 abstract description 5
- 239000005017 polysaccharide Substances 0.000 abstract description 5
- 102000004169 proteins and genes Human genes 0.000 abstract description 5
- 108090000623 proteins and genes Proteins 0.000 abstract description 5
- 238000011161 development Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 239000000654 additive Substances 0.000 abstract description 3
- 230000000996 additive effect Effects 0.000 abstract description 3
- 235000013376 functional food Nutrition 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 239000012141 concentrate Substances 0.000 abstract 1
- 238000010828 elution Methods 0.000 abstract 1
- 239000000178 monomer Substances 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 239000000523 sample Substances 0.000 description 6
- 239000003814 drug Substances 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 4
- 230000004071 biological effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 241001248610 Ophiocordyceps sinensis Species 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000003809 water extraction Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 240000001307 Myosotis scorpioides Species 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 241000382353 Pupa Species 0.000 description 1
- 150000003838 adenosines Chemical class 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000003013 cytotoxicity Effects 0.000 description 1
- 231100000135 cytotoxicity Toxicity 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000007365 immunoregulation Effects 0.000 description 1
- 238000010829 isocratic elution Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- SPOMEWBVWWDQBC-UHFFFAOYSA-K tripotassium;dihydrogen phosphate;hydrogen phosphate Chemical compound [K+].[K+].[K+].OP(O)([O-])=O.OP([O-])([O-])=O SPOMEWBVWWDQBC-UHFFFAOYSA-K 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 239000012224 working solution Substances 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
Abstract
The invention provides an extraction and purification method of cordycepin from Cordyceps militaris, and belongs to the deep-processing technical field of agricultural products. The method comprises the following steps: crushing Cordyceps militaris raw material, mixing the raw material with water at 1:20 raw material/water ratio, performing ultrasonic extraction, and performing centrifugal filtration on obtained extracting solution and pouring in a macroporous resin column at the adsorption flow of 1.8BV/hr; taking 15% methanol aqueous solution as an eluant to perform resin column elution, and decompressing and condensing obtained eluent at the temperature of 60 DEG C by a rotary evaporator to obtain Cordyceps militaris cordycepin concentrate. The method can help realize aqueous solution extraction of the cordycepin from the Cordyceps militaris raw material at low temperature, and the extraction rate reaches 85%; and polysaccharide and protein can be removed from the extract by macroporous resin separation and purification, thus the content of the cordycepin in the extract can reach 10%. The cordycepin in the Cordyceps militaris product has high activity, can be taken as a raw material for producing cordycepin monomer and can also be directly taken as an additive of health products and functional food, thus the cordycepin has wide market development prospect.
Description
One, technical field
The invention provides extraction and purification process for cordycepin in a kind of Cordyceps militaris (L.) Link., belong to deep-processing technical field of agricultural products.
Two, background technology
Cordyceps militaris (L.) Link. (Cordyceps militaris) has another name called Cordyceps militaris (L.) Link., with China rare traditional Chinese medicine Cordyceps sinensis (Cordyeeps sinensis) for belonging to xenogenesis together, its cordycepin (cordycepin) content is (3.089 ± 0.046) ‰, than high about 3 to 6 times of the cordycepin in the Cordyceps sinensis. cordycepin is a kind of adenosine class formation analogue in the Chinese caterpillar fungus, molecular formula C
10H
130
3N
5. cordycepin has proved to have effects such as antitumor, antiviral, antibiotic, has cytotoxicity and immunoregulation effect.At present, the pure product price of cordycepin is 25000 dollars/g in the international market.China's Cordyceps militaris (L.) Link. cultivation is general, but how to be used as medicine with the form of mycelium or sporophore, and therefore, the extraction process of research cordycepin has important economic value and vast market application potential.
Macroporous adsorbent resin is the isolation technique of new development both at home and abroad in recent years, and in field of medicaments (particularly natural drug is refining), widely use, be fit to suitability for industrialized production, but the separation and purification aspect that this technology is applied in cordycepin yet there are no report, and the present invention adopts the macroporous adsorbent resin isolation technique to separate
Three, summary of the invention
Technical problem
The object of the present invention is to provide extraction and purification process for cordycepin in a kind of Cordyceps militaris (L.) Link., cordycepin content can reach 10%. and can make the cordycepin in the Cordyceps militaris (L.) Link. obtain enrichment by macroporous resin after the separation and purification, and it is low to have a production cost, characteristics such as technology maturation.
Extraction and purification process for cordycepin in the technical scheme Cordyceps militaris (L.) Link. provided by the invention comprises:
1) extraction of cordycepin in the Cordyceps militaris (L.) Link.: Cordyceps militaris (L.) Link. raw material pulverizing, cross 40~100 mesh sieves, adding deionized water with material-water ratio 1:20 ratio then mixes, under ultrasonic frequency 90kHz, carry out ultrasonic extraction, 60 ℃ of temperature, extraction time 30-60 minute, extracting solution with 4000 rev/mins of centrifugings, is made pale brown look Cordyceps militaris (L.) Link. extracting solution.
2) separation and purification of cordycepin in the Cordyceps militaris (L.) Link.: with macroporous resin column on the extracting solution, the resin model is AB-8, and pH value is 5~5.5, and the sample solution amount is 5~6 times of resin column volumes, absorption flow velocity 1.8BV/hr; Wait to adsorb saturated back with deionized water towards post, after the effluent liquid clarification, be eluent wash-out resin column with 15% methanol aqueous solution, elutriant is 2.0~2.5 times of resin column volumes, during flow velocity 1BV/hr.
3) concentrating under reduced pressure elutriant: 60 ℃ of temperature, concentrating under reduced pressure elutriant under the vacuum tightness 0.09MP makes Cordyceps militaris (L.) Link. cordycepin enriched material with rotatory evaporator.
Extraction and purification process for cordycepin in above-mentioned a kind of Cordyceps militaris (L.) Link., used resin are that Cangzhou precious grace chemical industry company limited produces, and model is AB-8; Used eluent is 15% methanol aqueous solution; With deionized water as extraction agent and washing fluid.
Beneficial effect the present invention can keep the biological activity of cordycepin to greatest extent with the cordycepin extract at low temperature in the Cordyceps militaris (L.) Link. raw material; Utilize polysaccharide and the protein ingredient that to remove after the macroporous resin separation and purification in the extract, the cordycepin content in the extract is reached more than 10%.Cordycepin enriched material impurity is few in the product Cordyceps militaris (L.) Link., and is active high, as reducing separating difficulty as separating the monomeric raw material of cordycepin, improves separation efficiency, reduces separation costs; As also can directly adding in healthcare products and the functional food, has the vast market development prospect as additive.
Major advantage of the present invention and positively effect are as follows:
1. the present invention adopts the low-temperature ultrasonic water extraction to extract cordycepin, has kept the biological activity of cordycepin to greatest extent, extraction rate reached to 85%;
2. utilize polysaccharide and the protein ingredient that to remove after the macroporous resin separation and purification in the extract, the cordycepin content in the extract is reached more than 10%.
3. cordycepin enriched material impurity is few in the product Cordyceps militaris (L.) Link., and is active high, as reducing separating difficulty as separating the monomeric raw material of cordycepin, improves separation efficiency, reduces separation costs; Cordycepin enriched material impurity is few in the product Cordyceps militaris (L.) Link., and is active high,
4. as separating the monomeric raw material of cordycepin can reduce separating difficulty, improve separation efficiency, reduce separation costs; As also can directly adding in healthcare products and the functional food, has the vast market development prospect as additive.
Four, description of drawings
The liquid chromatogram of Fig. 1 cordycepin standard specimen
Five, embodiment
The extraction of cordycepin in the Cordyceps militaris (L.) Link.: Cordyceps militaris (L.) Link. raw material Su Ke pupa No. 1 (commercially available) is pulverized, cross 40~100 mesh sieves, mixed with solid-liquid ratio 1:20 ratio and extracting solution deionized water then, upward carry out ultrasonic extraction at KQ5200E type Ultrasonic Cleaners (Kunshan ultrasonic instrument company limited) with ultrasonic frequency 90kHz, extract 60 ℃ of temperature, 30 minutes extraction times, 60 ℃ of temperature, extracting solution is centrifugal with 4000 rev/mins of centrifugings with TD5A-WS type whizzer (Shanghai Lu Xiang instrument whizzer instrument company limited), make pale brown look Cordyceps militaris (L.) Link. extracting solution.The present invention adopts the low-temperature ultrasonic water extraction to extract cordycepin, has kept the biological activity of cordycepin to greatest extent, extraction rate reached to 85%.
The separation and purification of cordycepin in the Cordyceps militaris (L.) Link.: with macroporous resin column on the extracting solution, the resin model is AB-8 (the precious grace chemical industry in a Cangzhou company limited), and pH value is 5~5.5, and the sample solution amount is 5~6 times of resin column volumes, absorption flow velocity 1.8BV/hr; Wait to adsorb saturated back with deionized water towards post, after the effluent liquid clarification, be eluent wash-out resin column with 15% methanol aqueous solution, elutriant is 2~2.5 times of resin column volumes, during flow velocity 1BV/hr.
Concentrating under reduced pressure elutriant: 60 ℃ of temperature, under the vacuum tightness 0.09MP elutriant is concentrated to 10ml with RE52A type rotatory evaporator (Shanghai Yarong Biochemical Instrument Plant), makes Cordyceps militaris (L.) Link. cordycepin enriched material.
Measuring method: utilize high performance liquid chromatography to carry out the mensuration of cordycepin content. measuring method is as follows:
1 reagent and material
Potassium primary phosphate: analytical pure.Dipotassium hydrogen phosphate: analytical pure.Tetrahydrofuran (THF): chromatographically pure. dehydrated alcohol: analytical pure.4 experimental waters: should meet the requirement of GB/T6682-1992 one-level water.Cordycepin standard substance: purity 〉=98%.
2 cordycepin standard reserving solutions: accurately take by weighing cordycepin standard substance 15mg, fixed molten with the dissolving of 50% aqueous ethanolic solution ultra-sonic oscillation to 100mL, place-18 ℃ of refrigerators to preserve, preservation period is 2 months.
3 moving phases: accurately take by weighing 1.36gKH2PO4,2.28gK2HPO43H2O in the 1L volumetric flask, be dissolved in water, constant volume, add the 10mL tetrahydrofuran (THF) again, mixing is standby.
4 instrument and equipments
Liquid chromatograph has UV-detector, 0.22 μ m filter membrane.The ultrasonoscope supercentrifuge, rotating speed is not less than 10000rpm.Air dry oven.
5 test procedures
5.1 the preparation of sample
With 60 ℃ of oven drying at low temperatures 1 hour, pulverizing the back, to cross the aperture be that 60 mesh sieves are standby with sample.Precision takes by weighing powder 0.1g, puts into reagent bottle, adds 10.00mL distilled water, supersound extraction 30 minutes, and 0.22 μ m millipore filtration filters, and extracting solution is as need testing solution.
5.2 chromatographic condition
5.2.1 typical curve
The dilute with water standard reserving solution, the standard operation solution of preparation series concentration: 3 μ g/mL, 6 μ g/mL, 30 μ g/mL, 75 μ g/mL, 150 μ g/mL.0.22 μ m membrane filtration is got filtrate, draws 10 μ L sample detection (n=3) successively with microsyringe under chromatographic condition.With the peak area is ordinate zou, and corresponding standard working solution concentration is X-coordinate.The high-efficient liquid phase chromatogram of cordycepin standard specimen (Fig. 1), the present invention utilizes polysaccharide and the protein ingredient that can remove after the macroporous resin separation and purification in the extract, and the cordycepin content in the extract is reached more than 10%.
5.2.2 chromatographic column:
C18 post (3.9mm * 300mm, 4 μ m).
5.2.3 moving phase:
The KH2PO4-K2HPO4 damping fluid (pH=6.86,0.01mol/L), isocratic elution; Flow velocity: 1.00mL/min.
5.2.4 detection wavelength: 260nm.
5.3 accurate respectively reference substance solution and each the 10 μ L of need testing solution of drawing of sample introduction inject liquid chromatograph, measure.On typical curve, calculate the concentration of garlicin in the sample solution with peak area.
The result calculates:
By (1) formula calculation result.
In the formula:
X---cordycepin content in the sample, unit is every kilogram (mg/g) of gram;
C---the concentration of cordycepin in the sample solution, unit is every milliliter of microgram (μ g/mL);
V---sample solution volume, unit are milliliter (mL);
M---sample mass, unit is gram (g).
Calculation result keeps two position effective digitals.
5 precision
The absolute difference of the twice independent measurement result that obtains under repeated condition must not surpass 10% of arithmetical av.
The result
Utilize polysaccharide and the protein ingredient that to remove after the macroporous resin separation and purification in the extract, the cordycepin content in the extract is reached more than 10%.
Claims (2)
1, extraction and purification process for cordycepin in a kind of Cordyceps militaris (L.) Link. comprises:
1) extraction of cordycepin in the Cordyceps militaris (L.) Link.: Cordyceps militaris (L.) Link. raw material pulverizing, cross 40~100 mesh sieves, mixed with feed liquid mass ratio 1:20 ratio and extracting solution deionized water then, under ultrasonic frequency 90kHz, carry out ultrasonic extraction, extract 60 ℃ of temperature, extraction time 30-60 minute, extracting solution with 4000 rev/mins of centrifugings, is made pale brown look Cordyceps militaris (L.) Link. extracting solution;
2) separation and purification of cordycepin in the Cordyceps militaris (L.) Link.: with macroporous resin column on the extracting solution, the resin model is AB-8, and pH value is 5~5.5, and the sample solution amount is 5~6 times of resin column volumes, absorption flow velocity 1.8BV/hr; Waiting to adsorb saturated back and use the washing fluid deionized water towards post, after the effluent liquid clarification, is eluent wash-out resin column with volume ratio 15% methanol aqueous solution, and elutriant is 2~2.5 times of resin column volumes, during flow velocity 1BV/hr;
3) concentrating under reduced pressure elutriant: 60 ℃ of temperature, concentrating under reduced pressure elutriant under the vacuum tightness 0.09MP makes Cordyceps militaris (L.) Link. cordycepin enriched material with rotatory evaporator.
2, the product that extraction and purification process for cordycepin obtained in the described a kind of Cordyceps militaris (L.) Link. of claim 1.
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CN102060898A (en) * | 2011-01-10 | 2011-05-18 | 中山大学 | Extraction method of cordycepin |
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CN102746355B (en) * | 2012-06-19 | 2014-08-13 | 吉林省起泰科技有限公司 | Method for extracting and separating cordycepin |
CN102746355A (en) * | 2012-06-19 | 2012-10-24 | 吉林省起泰科技有限公司 | Method for extracting and separating cordycepin |
CN102936271B (en) * | 2012-11-14 | 2015-04-22 | 石家庄藏诺生物股份有限公司 | Method for extracting cordycepin |
CN102936271A (en) * | 2012-11-14 | 2013-02-20 | 石家庄藏诺生物股份有限公司 | Method for extracting cordycepin |
CN104072559A (en) * | 2014-05-08 | 2014-10-01 | 宁波广发文博生物科技有限公司 | Method for extracting cordycepin from cordyceps militaris |
CN104926903B (en) * | 2015-05-30 | 2018-05-01 | 北京汇林思生物科技有限公司 | A kind of method for extracting active ingredient in cordyceps sinensis |
CN104926903A (en) * | 2015-05-30 | 2015-09-23 | 吴爱群 | Method for extracting effective components in cordyceps sinensis |
CN105585639A (en) * | 2015-12-08 | 2016-05-18 | 泰山医学院 | Cordyceps militaris sporocarp heteropolysaccharide and application thereof |
CN105585639B (en) * | 2015-12-08 | 2017-10-27 | 泰山医学院 | Cordyceps militaris fruiting body heteropolysaccharide and application thereof |
CN107266513A (en) * | 2017-07-10 | 2017-10-20 | 浙江理工大学 | A kind of isolation and purification method of Cordyceps militaris active component |
CN107266513B (en) * | 2017-07-10 | 2020-06-09 | 浙江理工大学 | Separation and purification method of active ingredients of cordyceps militaris |
CN108815205A (en) * | 2018-09-14 | 2018-11-16 | 徐州工程学院 | Cordyceps militaris extract and the preparation method and application thereof |
CN108815205B (en) * | 2018-09-14 | 2022-02-01 | 徐州工程学院 | Cordyceps militaris extract and preparation method and application thereof |
CN110754436A (en) * | 2019-10-31 | 2020-02-07 | 青岛农业大学 | Method for collecting larvae of cryptocaryon irritans |
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