CN1500520A - Lichen bacteriophage and its production method thereof - Google Patents

Lichen bacteriophage and its production method thereof Download PDF

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Publication number
CN1500520A
CN1500520A CNA021525560A CN02152556A CN1500520A CN 1500520 A CN1500520 A CN 1500520A CN A021525560 A CNA021525560 A CN A021525560A CN 02152556 A CN02152556 A CN 02152556A CN 1500520 A CN1500520 A CN 1500520A
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CN
China
Prior art keywords
tinctorum despr
parmelia tinctorum
antibiotics
ethanol
parmelia
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Pending
Application number
CNA021525560A
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Chinese (zh)
Inventor
姚德坤
王秀丽
姚德利
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GREAT XINGAN MOUNTAINS LINGEBEI ORGANIC FOOD CO Ltd
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GREAT XINGAN MOUNTAINS LINGEBEI ORGANIC FOOD CO Ltd
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Application filed by GREAT XINGAN MOUNTAINS LINGEBEI ORGANIC FOOD CO Ltd filed Critical GREAT XINGAN MOUNTAINS LINGEBEI ORGANIC FOOD CO Ltd
Priority to CNA021525560A priority Critical patent/CN1500520A/en
Publication of CN1500520A publication Critical patent/CN1500520A/en
Pending legal-status Critical Current

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  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The present invention is Baishi flower antibiotic and its production process. Through the main technological process of Baishi flower pre-treatment with resin, hot alcohol reflux extraction, decompressing concentration, adsorption, desorption, secondary decompressing concentration and spray drying, Baishi flower antibiotic is produced.

Description

Parmelia tinctorum Despr. antibiotics and production technology thereof
Parmelia tinctorum Despr. antibiotics and production technology belong to a kind of Chinese medicinal plant extract and production technology thereof, Parmelia tinctorum Despr., another name Parmelia saxatilis Ach., stone clothing, Dermis Rana limnocharis, the prunus mume (sieb.) sieb.et zucc. clothing, Latin Parmeliatinctorum Desper.and NYL, thallus wrinkles more, about 30 centimetres of diameter, above canescence, the edge branch is attacked into most irregular lobes, sliver tip circle, the edge the fecula bud, and is level and smooth, little glossy, the close life of central authorities' pin bud, black, more coarse, the lower edge part is level and smooth, and tarnish has rhizoid.Sub-device is few, cup-shaped, and about 1 centimetre of diameter has short handle; The oval Room 1 of spore, colourless, produce on rock and the bark, be distributed in Daxing'an Mountainrange, Parmelia tinctorum Despr. is rich in sekikaic acid, and (Lecanoric acid is Parmelialic acid, C 16H 14O 7), 22%-24%, (atranorin is Parmelin to the Parmelia saxatilis Ach. element, C 19H 18O 8) 0.4%-1.1%, nor-Corii Bovis seu Bubali folic acid (norstictinic acid, C 19H 12O 9) 1%, Sa La Qin acid (Salazinic acid) 1%-1.2%.Still contain black phenol carboxylate methyl ester etc. in addition.Have heat-clearing and toxic substances removing, removing heat from blood, effects such as hemostasis are as the antibiotics raw material.
Daxing'an Mountainrange Parmelia tinctorum Despr. raw material resources are very abundant, its year reserves more than 10,000 tons, it is carried out rational exploitation and utilization, the forest zone new growth engines is significant for cultivating.
Purpose of the present invention be exactly utilize Parmelia tinctorum Despr. extract through technology of the present invention after and a kind of Parmelia tinctorum Despr. antibiotics atranorin of making is parmelin, molecular formula is C 19H 18O 8, its effective component content 〉=25% is used for the treatment of innominate toxic swelling, traumatic hemorrhage, anti-secondary tumor.
Advantage of the present invention is the Parmelia tinctorum Despr. antibiotics effective component content height of producing by Technology of the present invention, and therapeutic effect is obvious, has the effect of heat clearing away preferably, detoxifcation, pathogenic fire purging, antiinflammatory.Do not find as yet up till now to utilize Parmelia tinctorum Despr. to extract the report of antibiotics.Its development success reduces the side effect to the patient for changing the situation mostly present clinical application is synthetic antibiotic, has profound significance.This antibiotics production technology is simple simultaneously, product harvest rate height, and raw material is easy to get.
The present invention relates to the natural Parmelia tinctorum Despr. of a kind of usefulness is the method for the natural Parmelia tinctorum Despr. antibiotics of raw material production, comprises following main contents:
1. resin pretreatment: get commercially available macroporous adsorbent resin, use the alcohol heating reflux eluting, be washed till noresidue behind the eluent evaporate to dryness.After the resin that ethanol is cleaned is flung to solvent, preserve standby.
2. resin dress post: with ethanol wet method dress post, continue on post, to flow and clean, check effusive ethanol frequently, to mix (getting 1ml ethanol liquid 5ml water) till the muddiness that is not white in color with water with ethanol.With a large amount of distilled water flush away ethanol, standby then.There is the absorption affinity that will reduce resin greatly in small amount of ethanol.
3. resin regeneration: when the ethanol elution with 95% was extremely colourless, resin column was promptly regenerated, removes alcohol with massive laundering then, can carry out extraction separation next time.After using repeatedly, adsorbent resin darkens, and when adsorption effect descended, available 2-4%NaOH solution soaking foam 24 hours was washed till neutrality with clear water then, and reuse 2-4%HCl solution soaking 12 hours is washed till neutrality with clear water then, and resin is promptly regenerated.
4, alcohol reflux
Learnt from else's experience and selected Parmelia tinctorum Despr. after the cleaning, slightly broken, with 95% alcohol reflux 8--12 time, 1.5h at every turn, the solvent consumption is 8--10 times, extracting liquid filtering, merging filtrate.
5, concentrating under reduced pressure
Filtrate after merging is concentrated under 60--70 ℃ of condition, and striking point is 5 Baumes.
6, absorption
Add on 3m * 0.5m macroporous adsorptive resins that suitable quantity of water heating is added to dissolving, sucking filtration, filtrate to have handled well, adsorption rate is 5BV/H, till saturated.
7, desorbing
After having adsorbed, wash with water earlier to reducing sugar reaction and be negative (Molish reaction), use 30% ethanol instead and be washed till the whole eluting of Parmelia tinctorum Despr. antibiotics and detect with the Rp-HPLC method fully, detect the chromatographic peak of no Parmelia tinctorum Despr. antibiotics in the liquid.
8, decompression secondary concentration
Merge 30% ethanol elution, decompression recycling ethanol, temperature is controlled at 60-65 ℃, and striking point is the 5-10 Baume.
9, spray drying
Carry out spray drying with concentrating good Parmelia tinctorum Despr. extracting solution.Baking temperature: inlet temperature is controlled at 200-250 ℃, and outlet temperature is controlled at 60-80 ℃, and air-pressure controlling is at 0.45mPa, and obtaining the silver gray powder is Parmelia tinctorum Despr. antibiotics.
The invention still further relates to by production method of the present invention and obtain natural Parmelia tinctorum Despr. antibiotics, its every index is as follows:
Physical and chemical index:
Color and luster: silver gray
Shape: Powdered
Dissolubility: be dissolved in water fully
Degree of purity: do not have precipitation, free from admixture
Parmelia tinctorum Despr. antibiotics content: 25-98%
Moisture % :≤5
Ash % :≤0.05
Arsenic (As) % :≤0.0001
Plumbous (Pb) % :≤0.0003
Microbiological indicator:
Total number of bacteria:＜100/g
Mycete:＜100/g
Salmonella: must not detect
Escherichia coli: must not detect
Following most preferred embodiment further specifies the present invention.
1. resin pretreatment: get 500 kilograms of commercially available macroporous adsorbent resins, use the alcohol heating reflux eluting, be washed till noresidue behind the eluent evaporate to dryness.After the resin that ethanol is cleaned is flung to solvent, preserve standby.
2. resin dress post: with ethanol wet method dress post, continue on post, to flow and clean, check effusive ethanol frequently, to mix (getting 1ml ethanol liquid 5ml water) till the muddiness that is not white in color with water with ethanol.With a large amount of distilled water flush away ethanol, standby then.There is the absorption affinity that will reduce resin greatly in small amount of ethanol.
3. resin regeneration: when the ethanol elution with 95% was extremely colourless, resin column was promptly regenerated, removes alcohol with massive laundering then, can carry out extraction separation next time.After using repeatedly, adsorbent resin darkens, and when adsorption effect descended, available 2-4%NaOH solution soaking foam 24 hours was washed till neutrality with clear water then, and reuse 2-4%HCl solution soaking 12 hours is washed till neutrality with clear water then, and resin is promptly regenerated.
4, alcohol reflux
Learnt from else's experience and select 1000 kilograms of Parmelia tinctorum Despr. after the cleaning, slightly broken, with 95% alcohol reflux 12 times, each 1.5h, solvent consumption are that 8--10 doubly is 8000 kilograms, extracting liquid filtering, merging filtrate.
5, concentrating under reduced pressure
Filtrate after merging is concentrated under 65 ℃ of conditions for 7500 kilograms, and striking point is 5 Baumes.
6, absorption
Add on 3m * 0.5m macroporous adsorptive resins that suitable quantity of water heating is added to dissolving, sucking filtration, filtrate to have handled well, adsorption rate is 5BV/H, till saturated.
7, desorbing
After having adsorbed, wash with water earlier to reducing sugar reaction and be negative (Molish reaction), using 1000 kilograms of 30% ethanol instead, to be washed till the whole eluting of Parmelia tinctorum Despr. antibiotics complete, detects with the Rp-HPLC method, detects the chromatographic peak of no Parmelia tinctorum Despr. antibiotics in the liquid.
8, decompression secondary concentration
Merge 1000 kilograms of 30% ethanol elution, decompression recycling ethanol, temperature is controlled at 60-65 ℃, and striking point is the 5-10 Baume.
9, spray drying
Carry out spray drying with concentrating good Parmelia tinctorum Despr. extracting solution.Baking temperature: inlet temperature is controlled at 200-250 ℃, and outlet temperature is controlled at 60-80 ℃, and air-pressure controlling is at 0.45mPa, and obtaining 10 kilograms in silver gray powder is Parmelia tinctorum Despr. antibiotics.
Following dried powder is carried out vacuum packaging, every bag of 0.5-5kg/ bag, or the sealing of paper loading plate bucket.

Claims (8)

  1. The present invention relates to a kind of production method of Parmelia tinctorum Despr. antibiotics and the Parmelia tinctorum Despr. antibiotics that obtains thus, be primarily characterized in that:
    1, resin pretreatment: get commercially available macroporous adsorbent resin, use the alcohol heating reflux eluting, be washed till noresidue behind the eluent evaporate to dryness, with ethanol wet method dress post, the reuse clear water dashes to there not being the alcohol flavor then.
  2. 2, alcohol heat reflux extracts
    Learnt from else's experience and selected Parmelia tinctorum Despr. after the cleaning, slightly broken, with 95% alcohol reflux 8--12 time, 1.5h at every turn, temperature is controlled in 80 ℃, and the solvent consumption is 8--10 times, extracting liquid filtering, merging filtrate.
  3. 3, concentrating under reduced pressure
    Filtrate after merging is concentrated under 60--70 ℃ of condition, and striking point is 5 Baumes.
  4. 4, absorption
    Add on 3m * 0.5m macroporous adsorptive resins that suitable quantity of water heating is added to dissolving, sucking filtration, filtrate to have handled well, adsorption rate is 5BV/H, till saturated.
  5. 5, desorbing
    After having adsorbed, wash with water earlier to reducing sugar reaction and be negative (Molish reaction), using 30% ethanol instead, to be washed till the whole eluting of Parmelia tinctorum Despr. antibiotics complete.
  6. 6, decompression secondary concentration
    Merge 30% ethanol elution, decompression recycling ethanol, temperature is controlled at 60-65 ℃, and striking point is the 5-10 Baume.
  7. 7, the Parmelia tinctorum Despr. extracting solution after above-mentioned the concentrating is added the aseptic distillation water of 10-30% and can obtain Parmelia tinctorum Despr. liquid antibiotic element, effective component content 25-28%.
  8. 8, spray drying
    The Parmelia tinctorum Despr. extracting solution of aforesaid right 6 gained is carried out spray drying.Baking temperature: inlet temperature is controlled at 200-250 ℃, and outlet temperature is controlled at 60-80 ℃, and air-pressure controlling can obtain the Powdered Parmelia tinctorum Despr. antibiotics of silver gray at 0.45mPa.
CNA021525560A 2002-11-18 2002-11-18 Lichen bacteriophage and its production method thereof Pending CN1500520A (en)

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CNA021525560A CN1500520A (en) 2002-11-18 2002-11-18 Lichen bacteriophage and its production method thereof

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Application Number Priority Date Filing Date Title
CNA021525560A CN1500520A (en) 2002-11-18 2002-11-18 Lichen bacteriophage and its production method thereof

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CN1500520A true CN1500520A (en) 2004-06-02

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103044258A (en) * 2012-12-13 2013-04-17 大兴安岭林格贝有机食品有限责任公司 Novel technology method for extracting lichen parmeliae tinctori atranorine from wild lichen parmeliae tinctori

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103044258A (en) * 2012-12-13 2013-04-17 大兴安岭林格贝有机食品有限责任公司 Novel technology method for extracting lichen parmeliae tinctori atranorine from wild lichen parmeliae tinctori
CN103044258B (en) * 2012-12-13 2015-09-30 大兴安岭林格贝寒带生物科技股份有限公司 A kind of novel technological method extracting white parmelia saxatilis tea stain element from wild white parmelia saxatilis

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