CN103977035A - Application of refrigeration technique to drying of cordyceps sinensis - Google Patents

Application of refrigeration technique to drying of cordyceps sinensis Download PDF

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Publication number
CN103977035A
CN103977035A CN201410204825.5A CN201410204825A CN103977035A CN 103977035 A CN103977035 A CN 103977035A CN 201410204825 A CN201410204825 A CN 201410204825A CN 103977035 A CN103977035 A CN 103977035A
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China
Prior art keywords
cordyceps
dissolution
dry
application
refrigeration technique
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CN201410204825.5A
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Chinese (zh)
Inventor
刘金磊
石红艳
李诗标
卢宁
刘圣梅
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Jinan Kangzhong Pharmaceutical Research and Development Co Ltd
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Jinan Kangzhong Pharmaceutical Research and Development Co Ltd
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Priority to CN201410204825.5A priority Critical patent/CN103977035A/en
Publication of CN103977035A publication Critical patent/CN103977035A/en
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Abstract

The invention relates to an application of a refrigeration technique to drying of cordyceps sinensis. Newly-dug out fresh cordyceps sinensis is refrigerated, stacked for 2-5 days and dried; the prepared cordyceps sinensis has high content of main effective components, is applied to auxiliary treatment of cancers and enhancement of immunity, and has a good clinical curative effect.

Description

The application of Refrigeration Technique in Cordyceps is dry
Invention field
The present invention relates to medicine preparation method, the particularly application of Refrigeration Technique in Cordyceps is dry, belongs to medical technical field.
Background technology
Cordyceps is that section ergot fungus cordyceps sinensis bacterium colonizes in Stroma on Hepialidae insect larvae and the dry composite body of larva corpse.Early summer Stroma is unearthed, spore does not take while dispersing, and shines to 6 seventy percent dry, removes quasi-fibrous attachment and impurity, dries or cold drying.Cordyceps is a kind of rare Chinese medicine of China, classifies China's three large tonics together with Radix Ginseng, Cornu Cervi Pantotrichum as, have the title of soft gold.Cordyceps enters lung, kidney channel, can the kidney invigorating lung benefiting, and hemostasis and phlegm, has immunomodulating, antitumor, protection Liver and kidney and calmness, antifatigue effect.Cordyceps contains various active material, comprise ucleosides, polysaccharide, amino acid polypeptide class and various trace elements, wherein nucleosides material is main active, in nucleoside, with adenosine, there is obvious pharmacological action again, so working standard is using adenosine content as the leading indicator of investigating Cordyceps quality.
Quality and the bioavailability of curative effect of medication are closely related, although bioavailability height is finally to weigh with clinical efficacy, also can evaluate by dissolution in vitro.Dissolution refers to that medicine is from speed and the degree of solid preparation stripping regulation solvent.Dissolution is an important indicator of quality control of solid dosage forms.Medicine in vivo infiltration rate is usually determined by the speed dissolving, medicine in solid preparation is before being absorbed, must be through dissolving the process that then transfers solution to, if medicine is difficult for discharging from preparation or the dissolution velocity of medicine is very slow, the infiltration rate of said preparation Chinese medicine or degree just likely have problems.
The prepared slices of Chinese crude drugs there is no the concept of dissolution at present.Cordyceps is as costly medicine, conventionally directly beats powder and takes, so reference solid preparation dissolution method, the dissolution of the Cordyceps of mensuration, can be used as an index of evaluation quality.This being applied in previously also has relevant report in document.Liang Juchun etc., have studied the Cordyceps dissolution in vitro of nanometer particle size, and result shows that smashing fineness increase can improve the dissolution (Liang Juchun etc. of Cordyceps, Cordyceps study in vitro dissolution, Chengdu University journal, the 32nd the 1st phase of volume in 2013,15-19 page).The document does not relate to the freezing impact on dissolution.
At a kind of processing method of Cordyceps (application number: 200310110734.7) disclose in patent that to utilize vacuum lyophilization to prepare moisture content low, long shelf-life, is easy to the Cordyceps storing.As well known to those skilled in the art, freeze drying technology is for processing and the active fresh-keeping of Chinese crude drug, the activity that can preserve to greatest extent effective medicinal components, the exterior quality that keeps preferably medical material, dehydration thoroughly, is easily preserved, and has the unrivaled superiority of other dry technologies.Prior art does not relate to the report that can further improve effective ingredient after freezing processing, more without application Refrigeration Technique, prepares the report of the Cordyceps that active component content is high.
Li Shao equality, content and variation (Li Shao equality at Cordyceps Nucleosides, content and the variation of natural and fermentation culture Cordyceps Nucleosides, Acta Pharmaceutica Sinica, the 36th the 6th phase of volume of calendar year 2001,436-439 page) in research, show that in the Cordyceps of fresh collection, adenosine class content of material is extremely low, and gather with the passing of time, person's gradient elution content is higher, prompting natural cordyceps Nucleosides may derive from the degraded of macromole nucleoside in storage process, and result of study shows the damp and hot content that increases nucleosides material in Cordyceps.
Existing document does not have the freezing report on dissolution impact.
Summary of the invention
The drying means that the object of this invention is to provide a kind of Cordyceps, the dry active ingredients of cordyceps sinensis ucleosides content of the method is high, and for auxiliary treatment and the enhancing immunity of cancer, clinical efficacy is good.
The present invention is achieved in that
The application of Refrigeration Technique in Cordyceps is dry, is characterized in that: get the fresh Cordyceps newly digging out, and freezing, the 2-5 days that banks up at dark and damp place is dry.
The application of Refrigeration Technique of the present invention in Cordyceps is dry, is characterized in that: freezing is to be refrigerated to freeze.
The application of Refrigeration Technique of the present invention in Cordyceps is dry, is characterized in that: freezing is to be refrigerated to-5 ℃ to freeze below.
The application of Refrigeration Technique of the present invention in Cordyceps is dry, is characterized in that: dry is that heap postpone is dried or dries or dries.
Of the present inventionly being refrigerated to subzero certain ℃, is to be refrigerated to and to freeze at this subzero certain ℃.
The method of preparing Cordyceps by Refrigeration Technique of the present invention, has same effect for the Cordyceps fungus powder that ferments.
Above-mentioned fermentation Cordyceps fungus powder refers to from Cordyceps what separated strain was prepared by the method for industrial fermentation, as hundred raw materials that make capsule, JINSHUIBAO, Cordyceps militaris (L.) Link. sheet.
So far completed the present invention, the active ingredients of cordyceps sinensis content of preparing by drying means of the present invention is high, and active component dissolution is high, and for auxiliary treatment and the enhancing immunity of cancer, clinical efficacy is good.
Test example is intended to further illustrate substantive progress of the present invention below, but not limitation of the present invention.
Active constituent content and the Comparative Study on Dissolution of Cordyceps of the present invention and common Cordyceps and Cordyceps nano powder
1, instrument and material
The semi-automatic digestion instrument of Switzerland SOTAX; Waters high performance liquid chromatograph.Adenosine reference substance is purchased from Nat'l Pharmaceutical & Biological Products Control Institute, for assay.
Cordyceps: be purchased from Jinan Bai Weitang decoction pieces factory, decoction pieces is up to the standards through hundred taste halls.
Cordyceps nano powder: be purchased from Jinan Bai Weitang decoction pieces factory Cordyceps decoction pieces, pulverize, cross 325 mesh sieves.
Cordyceps 1: get the fresh Cordyceps coming from place of production air transport, be refrigerated to-5 ℃ to freezing, bank up 3 days at dark and damp place, 50 ℃ of following oven dry.
2, Determination of Adenosine: measure according to method under 2010 editions (one) Cordyceps items of < < Chinese Pharmacopoeia > >.
Chromatographic condition and system suitability be take octadecylsilane chemically bonded silica as filling chaste tree; Phosphate buffer (the pH6.5)-methanol (85:15) of take is mobile phase; Detection wavelength is 260nm.Number of theoretical plate calculates and should be not less than 2000 by adenosine peak.
It is appropriate that adenosine reference substance is got in the preparation of reference substance solution, accurately weighed, adds 90% methanol and make every 1m1 containing the solution of 20 μ g, obtains.
The preparation of need testing solution is got respectively Cordyceps (pulverizing sieve No. three), Cordyceps nano powder, worm summer in winter 1(and was pulverized sieve No. three) each about 0.5g, accurately weighed, put in tool plug conical flask, precision adds 90% methanol 10ml, and close plug, shakes up, weighed weight, reflux 30 minutes, lets cool, weighed weight again, the weight of supplying less loss with 90% methanol, shakes up, and filters, get subsequent filtrate, obtain.Algoscopy is accurate reference substance solution and each l0 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and obtains.
Result: in dry product, three kinds of Cordyceps sample adenosine contents are in Table 1.
Three kinds of Cordyceps sample adenosine contents of table 1 (%)
Decoction pieces Cordyceps decoction pieces Cordyceps nano powder Cordyceps decoction pieces 1
Adenosine content 0.0299 0.0301 0.0498
Presentation of results, the Cordyceps of preparing by method of the present invention, active constituent content is obviously high, good product quality.
3, Their Dissolution Test in vitro
Sample thief, pulverize, cross sieve No. 6, get respectively 6 parts, every part of 2g, according to Their Dissolution Test in vitro method, with pH1.2(sodium chloride 2.0g, adding water dissolves in right amount, add hydrochloric acid 7ml, thin up becomes 1000ml again, obtain) solution 400ml be solvent, rotating speed is 50 r/ min, through 5, 10, 15, 30, 45, 60, 90, during 120 min, get respectively solution 5ml, with 0.45 μ m microporous filter membrane, filter, get subsequent filtrate as need testing solution, and immediately in process container, supplement dissolution medium, according to Determination of Adenosine method, measure, take sample size as 100%, by external standard method, with calculated by peak area, go out sample at the stripping quantity of different time.The results are shown in Table 2.
Three kinds of Cordyceps sample dissolution comparisons of table 2 (%, min, n=6)
Time Cordyceps decoction pieces Cordyceps nano powder Cordyceps 1
5 16.23 4.32 17.32
10 40.51 30.72 79.56
15 64.21 80.11 99.12
20 67.05 98.33 98.02
30 67.65 99.01 97.36
40 67.78 98.14 98.19
60 68.02 99.45 98.79
80 68.28 98.36 99.13
Quality and the bioavailability of curative effect of medication are closely related, although bioavailability height is finally to weigh with clinical efficacy, also can evaluate by dissolution in vitro.Dissolution refers to that medicine is from speed and the degree of solid preparation stripping regulation solvent.Dissolution is an important indicator of quality control of solid dosage forms.Medicine in vivo infiltration rate is usually determined by the speed dissolving, medicine in solid preparation is before being absorbed, must be through dissolving the process that then transfers solution to, if medicine is difficult for discharging from preparation or the dissolution velocity of medicine is very slow, the infiltration rate of said preparation Chinese medicine or degree just likely have problems.
According to table 2 data, make three kinds of Cordyceps sample dissolution curves, see accompanying drawing 1.
From dissolution curve, Cordyceps is part stripping when 10min, and dissolution 40% left and right, reaches the highest scope at 15min, changes afterwards little; Cordyceps nano powder is part stripping when 10min, and dissolution 30% left and right, reach the highest scope, and dissolution reaches 100% at 20min; Cordyceps decoction pieces of the present invention part stripping when 10min, dissolution 80% left and right, reach the highest scope, and dissolution reaches 100% at 15min; Show that Cordyceps dissolution prepared by the present invention, higher than commercially available Cordyceps, compares with Cordyceps nano powder, stripping is faster, and can avoid pulverizing in nano powder preparation process the loss causing.
To sum up state test, active ingredients of cordyceps sinensis content prepared by the present invention is high, and dissolution rate is high, has higher activity.
Accompanying drawing explanation
Accompanying drawing 1 is Cordyceps (Cordyceps 1) dissolution curve comparison figure prepared by Cordyceps decoction pieces, Cordyceps nano powder, the inventive method.
the specific embodiment
embodiment 1
Get the fresh Cordyceps newly digging out, put in freeze dryer, be refrigerated to-5 ℃ to freezing, banking up 2 days in dark and damp place, dries.
Measure adenosine content in Cordyceps, containing adenosine (C10H13N5O4) O.0481%.
Measure Cordyceps dissolution, dissolution is in slurry method, and rotating speed 50 r/ min and commercially available Cordyceps compare, and dissolution is higher.
embodiment 2
Get the fresh Cordyceps newly digging out, put in freeze dryer, be refrigerated to-10 ℃, at dark and damp place, bank up 3 days, dry.
embodiment 3
Get the fresh Cordyceps newly digging out, put in freeze dryer, be refrigerated to-20 ℃, at dark and damp place, bank up 4 days, dry.
embodiment 4
Get the Hirsutlla sinensis mycelium of the new tank that ferments, put in freeze dryer, be refrigerated to-32 ℃ to freezing, at dark and damp place, bank up 3 days, dry.
embodiment 5
Get the Paecilomyces hepiali Chen et Dai Mycelia of the new tank that ferments, put in freeze dryer, be refrigerated to-15 ℃, at dark and damp place, bank up 5 days, dry.
embodiment 6
Get the cordyceps mycelium of the new tank that ferments, put in freeze dryer, be refrigerated to-25 ℃, at dark and damp place, bank up 3 days, dry.

Claims (5)

1. the application of Refrigeration Technique in Cordyceps is dry, is characterized in that: the fresh Cordyceps newly digging out, and freezing, the 2-5 days that banks up is dry.
2. the application in Cordyceps is dry according to the Refrigeration Technique of claim 1, is characterized in that: freezing is to be refrigerated to freeze.
3. the application in Cordyceps is dry according to the Refrigeration Technique of claim 1, is characterized in that: freezing is to be refrigerated to-5 ℃ to freeze below.
4. the application in Cordyceps is dry according to the Refrigeration Technique of claim 1, is characterized in that: dry is that heap postpone is dried or dries or dries.
5. the application in Cordyceps is dry according to the Refrigeration Technique of claim 1, is characterized in that: for the Cordyceps fungus powder that ferments, have same effect.
CN201410204825.5A 2014-05-15 2014-05-15 Application of refrigeration technique to drying of cordyceps sinensis Pending CN103977035A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102178226A (en) * 2011-04-15 2011-09-14 常州市炉奇虫草行 Fresh processing technique for Cordyceps sinensis

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102178226A (en) * 2011-04-15 2011-09-14 常州市炉奇虫草行 Fresh processing technique for Cordyceps sinensis

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
南京中医药大学: "《中药大辞典》", 31 March 2006, article "冬虫夏草" *
李绍平等: "天然与发酵培养冬虫夏草中核苷类成分的含量及其变化", 《药学学报》, vol. 36, no. 6, 31 December 2001 (2001-12-31) *
黄小丹等: "蛹虫草保健饮料的研制", 《食品工业》, 31 December 2010 (2010-12-31) *

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