CN1048403C - Photosensitizer of traditional herb medicines and its production technology - Google Patents

Photosensitizer of traditional herb medicines and its production technology Download PDF

Info

Publication number
CN1048403C
CN1048403C CN93103432A CN93103432A CN1048403C CN 1048403 C CN1048403 C CN 1048403C CN 93103432 A CN93103432 A CN 93103432A CN 93103432 A CN93103432 A CN 93103432A CN 1048403 C CN1048403 C CN 1048403C
Authority
CN
China
Prior art keywords
photosensitizer
ethanol
chinese medicine
mentioned
production technology
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
CN93103432A
Other languages
Chinese (zh)
Other versions
CN1092981A (en
Inventor
金秀莲
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dalian auretech Technology Co. Ltd.
Original Assignee
Zhejiang Academy of Traditional Chinese Medicine
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Zhejiang Academy of Traditional Chinese Medicine filed Critical Zhejiang Academy of Traditional Chinese Medicine
Priority to CN93103432A priority Critical patent/CN1048403C/en
Publication of CN1092981A publication Critical patent/CN1092981A/en
Application granted granted Critical
Publication of CN1048403C publication Critical patent/CN1048403C/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Abstract

The present invention relates to a traditional Chinese medicine photosensitizer and preparation method thereof, particularly to a traditional Chinese medicine photosensitizer for photosensitization therapy and preparation technology thereof. The present invention is characterized in that the photosensitizer contains chlorine 6 and 60 to 80 % of polymer; silkworm droppings are used as raw material; the preparation technology comprises the steps that the raw material and acetone are mixed to be extracted; then NaOH is added to the mixture to be saponified by ethanol; then magnesium is removed by acidification; the mixture is mixed and stirred with silica gel G; then the mixture is eluted, and impurities are removed respectively by petroleum ether and ethanol; then the mixture is dissolved by distilled water and vaporized to prepare the finished product. The prepared finished product is black brown loose powder, is easy to be dissolved into water, is not dissolved into an organic solvent and is sensitive to light. The photosensitizer has the advantages of good treatment effect, convenient clinical application, simple preparation technology, easy operation, and low cost and easy acquirement of the raw material.

Description

A kind of production technology of Chinese medicine photosensitizer
The present invention relates to be used for the Chinese medicine photosensitizer and the production technology of photosensitization therapy.
Photosensitization therapy is a kind of quick, the new technique of non-invasive diagnosis and treatment cancer, the external in recent years tumor bound pair step is attached great importance to, and obtained faster and made progress, but the research of photosensitizer and selection are the important steps of this photosensitization therapy always, the photosensitizer that uses clinically both at home and abroad is hematoporphyrin derivative (HPD) at present, hemoporphyrin is taken from animal blood, the retention time is long in the body, the photosensitive side effect of skin is strong, take 30 day time lucifuge, therefore make troubles to extensive use diagnosis and treatment, seek a kind of new, the curative effect height, drain fast, the photosensitizer that toxicity is low, significant.
The objective of the invention is to overcome the defective of above-mentioned existence, make every effort to use the Bombyx mori L. feedstock production that is easy to get that a kind of Chinese medicine photosensitizer is provided, and provide the production technology of this photosensitizer.
Described photosensitizer is characterized in that containing chlorin e (CHLORINe6) and polymer 60-80% thereof, is raw material with the Bombyx mori L., through acetone separation extract crude extract, then through saponification, acidify, remove impurity, refining obtaining.
Above-mentioned Chinese medicine photosensitizer is characterized in that containing chlorin e (CHLORINe6) and polymer 60-65% thereof.
Above-mentioned Chinese medicine photosensitizer is characterized in that containing the xanthein 20-40% based on carotin.
The production technology of above-mentioned Chinese medicine photosensitizer is a raw material with the Bombyx mori L., and presses following processing step:
1) gets Bombyx mori L. and mix, under 90-100 ℃ of temperature reflux 1-3 hour, filter waste and also reclaim acetone with the acetone that 3-7 doubly measures.
2) the above-mentioned crude extract that obtains is mixed with 95% ethanol that 1-5 doubly measures, heating for dissolving under agitation is incorporated as crude extract 1-3 10%NaOH doubly then, and under 90-100 ℃ of temperature reflux 12-20 hour, and to keep pH value be 9-10.
3) after above-mentioned mixed liquor reclaims ethanol, dilution, static, remove the thick thing in upper strata, filter waste.
4) above-mentioned solution neutralization and adjusting pH value are 4-6, and be static, abandons supernatant, and precipitate is repeated to be washed to neutrality, and filtration is drained.
5) impurity removal and purification.
The production technology of above-mentioned a kind of Chinese medicine photosensitizer is characterized in that by following technological parameter:
A) above-mentioned 1) Bombyx mori L. is doubly measured acetone with 4-6 and is mixed reflux 1.5-2.5 hour.
B) above-mentioned 2) crude extract that obtains and 2-4 doubly measure 95% ethanol and mix, and 10%NaOH is that the 1.5-2.5 of crude extract doubly measures, reflux 15-17 hour.
The production technology of above-mentioned a kind of Chinese medicine photosensitizer is characterized in that described impurity removal and purification, mixes and stirs absorption with silica gel G earlier, with the petroleum ether eluting, volatilize the back and take out granum, reuse 95% ethanol elution again, and recovery ethanol, be dissolved in water at last and evaporate anhydrate refining finished product.
Described Chinese medicine photosensitizer is dark brown loose powder, and is soluble in water, is insoluble to organic solvent, sees photaesthesia, keeps in Dark Place.It is good that fruit is treated in these photosensitizer diagnosis and treatment, and clinical practice is convenient, can alleviate the side effect of skin photosensitizer, and toxicity is low, drains fast.And production technology is simple, and raw material is cheap and easy to get, has application value widely.
Below provide specific embodiment of the present invention, simultaneously the present invention is further described.
(1) thick chlorophyllous extraction
Get the Bombyx mori L. pulverize, cross the distiller sieve No. 20, take by weighing 200g and place the 2000ml round-bottomed flask, add 5 times of amount acetone, add condenser reflux in water bath with thermostatic control, each two hours, about four times, filter, reclaim acetone, promptly get thick chlorophyll 10g (containing chlorophyll 10-15%).
(2) phytyl is gone in saponification
Get thick chlorophyll 200g, add 95% ethanol triplication, heating in water bath 20 minutes, the about 400ml of dissolving back agitation and dropping 10%NaOH, the adjusting pH value is 9-10, and heating in water bath refluxed about 16 hours, surveyed PH at any time, after reclaiming ethanol, add 20 times of about 4000ml of amount of distilled water, at a static night, remove the thick thing in upper strata, filter, filtrate keeps.
(3) magnesium is removed in acidify
Getting that above-mentioned solution adds 10%HCl neutralization and regulate pH value is 5, and at a static night, precipitate is on the bottom, and supernatant inclines to discard and repeats to be washed to neutrality then, and filtration is drained.
(4) impurity removal and purification
Get the silica gel that above-mentioned solid adds about one times of amount, mix thoroughly, be loose shape, with petroleum ether eluting (200g uses petroleum ether 6000ml approximately), till not having xanthein to eluent, volatilize the back and take out granum, place round-bottomed flask to add the about triplication of 95% ethanol, transferring PH is 9, same operation eluting 6 times, merge eluent, filtered and recycled ethanol gets the about 5g of chlorin e.Add about 10 times of water gagings dissolving at last, the water-bath evaporation is anhydrated, and must make with extra care finished product, and test dissolubility 100mg/ml should clarify, and survey content must be measured and be Bombyx mori L. 0.1-0.08%.

Claims (3)

1, a kind of production technology that contains the Chinese medicine photosensitizer of chlorin e and polymer thereof is characterized in that with the Bombyx mori L. being raw material, and presses following processing step:
1) get Bombyx mori L. and mix with the acetone that 3-7 doubly measures, under 90-100 ℃ of temperature reflux 1-3 hour, filter waste and also reclaim acetone,
2) the above-mentioned crude extract that obtains is mixed with 95% ethanol that 1-5 doubly measures, heating for dissolving under agitation is incorporated as crude extract 1-3 10%NaOH doubly then, and under 90-100 ℃ of temperature reflux 12-20 hour, and to keep pH value be 9-10,
3) after above-mentioned mixed liquor reclaimed ethanol, dilution, static, the thick thing in removal upper strata filtered waste,
4) above-mentioned solution neutralization and adjusting pH value are 4-6, and be static, abandons supernatant, and precipitate is repeated to be washed to neutrality, and filtration is drained,
5) impurity removal and purification.
2, the production technology of a kind of Chinese medicine photosensitizer as claimed in claim 1 is characterized in that by following technological parameter:
A) above-mentioned 1) Bombyx mori L. is doubly measured acetone with 4-6 and is mixed, and reflux 1.5-2.5 hour,
B) above-mentioned 2) crude extract that obtains and 2-4 doubly measure 95% ethanol and mix, and 10%NaOH is that the 1.5-2.5 of crude extract doubly measures, reflux 15-17 hour.
3, the production technology of a kind of Chinese medicine photosensitizer as claimed in claim 1, it is characterized in that described impurity removal and purification, earlier mix and stir absorption with silica gel G, again with the petroleum ether eluting, volatilize the back and take out granum, reuse 95% second jealous woman eluting, and reclaim ethanol, be dissolved in water at last and evaporate anhydrate refining finished product.
CN93103432A 1993-03-26 1993-03-26 Photosensitizer of traditional herb medicines and its production technology Expired - Lifetime CN1048403C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN93103432A CN1048403C (en) 1993-03-26 1993-03-26 Photosensitizer of traditional herb medicines and its production technology

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN93103432A CN1048403C (en) 1993-03-26 1993-03-26 Photosensitizer of traditional herb medicines and its production technology

Publications (2)

Publication Number Publication Date
CN1092981A CN1092981A (en) 1994-10-05
CN1048403C true CN1048403C (en) 2000-01-19

Family

ID=4984655

Family Applications (1)

Application Number Title Priority Date Filing Date
CN93103432A Expired - Lifetime CN1048403C (en) 1993-03-26 1993-03-26 Photosensitizer of traditional herb medicines and its production technology

Country Status (1)

Country Link
CN (1) CN1048403C (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100387240C (en) * 2003-06-16 2008-05-14 北京中亚深蓝生物技术开发有限公司 An extract of faeces bombycis and the preparation method thereof, use and device for diagnosing or treating malignant tumours

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102936423B (en) * 2012-10-25 2014-07-02 常州美胜生物材料有限公司 Brown pigment, and preparation method and application thereof
GB2558809B (en) 2013-01-09 2018-11-07 International Moisture Analysers Ltd Optical chemical analyser

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
中国药学杂志 1993.1.8 钟济秀等,蚕少光敏剂的皮肤光毒反应及毒性研究 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100387240C (en) * 2003-06-16 2008-05-14 北京中亚深蓝生物技术开发有限公司 An extract of faeces bombycis and the preparation method thereof, use and device for diagnosing or treating malignant tumours

Also Published As

Publication number Publication date
CN1092981A (en) 1994-10-05

Similar Documents

Publication Publication Date Title
CN103393780B (en) Extraction method of high-purity coptis total alkaloid
DE1935751A1 (en) New quinuclidinol derivatives, processes for their production and their use for the production of medicinal preparations
AT391315B (en) METHOD FOR PRODUCING ISOSILYBINE-FREE SILIBININE
CN1048403C (en) Photosensitizer of traditional herb medicines and its production technology
CN101838266A (en) Citric acid tropisetron raw material medicine and preparation technology of raw material medicine and injection liquid
CN109602693A (en) Mometasone furoate gel and preparation method thereof
CN101260138B (en) Highly effective separation purification method for polygalic acid and tenuigenin
CN103804207B (en) The preparation method of sinapic acid choline ester chlorate and medical applications thereof
CN102477041B (en) Preparation method of cepharanthine hydrochloride
CN105832814A (en) General flavone with effect of treating diabetic mellitus, as well as preparation method and application thereof
CN1241930C (en) Shaddock glycoside extracting and refining process from shaddock
CN1438237A (en) Echinocystic acid preparation, medicinal preparation and new use as medicine
Dudley et al. Improvements in the preparation of insulin. Alkaline extraction of pancreas
CN1178799A (en) Method for extracting solomonscal polyose from Chinese drug solomonseal rhizome
CN108997509B (en) Diaphragma juglandis polysaccharide, preparation method and application thereof
CN102614457A (en) Preparation method of breast recovering tablet
CN1047598C (en) Dammarane-type saponin ginseng lowhydric alcohol derivative and preparation method
IE54425B1 (en) A process for obtaining laxative compounds from senna drug
CN106749437A (en) A kind of recovery method of Glucosamine Sulphate sodium chloride double salt mother liquor
CN1109044C (en) Potassium glycyrrhetate and its preparing process and use
CN1640484A (en) Chinese medicine soft capsule Naodesheng and its preparing method
DE1518199C3 (en)
CN106913650A (en) The preparation method of almond extract and the almond extract prepared with it
CN110526999B (en) Extraction method and application of makallidan crude polysaccharide
CN1537573A (en) Extraction of active ingredient of Zuanshanfeng, and method for preparing its prepn.

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
ASS Succession or assignment of patent right

Owner name: ELLEN BIOTECHNOLOGY CO., LTD.

Free format text: FORMER OWNER: INST. OF TRADITIONAL CHINESE MEDICINE, ZHEJIANG PROV.

Effective date: 20040806

C41 Transfer of patent application or patent right or utility model
TR01 Transfer of patent right

Effective date of registration: 20040806

Address after: Queensland, Australia

Patentee after: Ireland biotech Co

Address before: 310007 No. 26 Tianmu Mountain Road, Zhejiang, Hangzhou

Patentee before: Zhejiang Traditional Chinese Medicine Research Institute

ASS Succession or assignment of patent right

Owner name: DALIAN AORUI SCIENCE CO., LTD.

Free format text: FORMER OWNER: ELLEN BIOTECHNOLOGY CO., LTD.

Effective date: 20050304

C41 Transfer of patent application or patent right or utility model
TR01 Transfer of patent right

Effective date of registration: 20050304

Address after: 116023 No. 3, Gaoxin street, hi tech park, Liaoning, Dalian

Patentee after: Dalian auretech Technology Co. Ltd.

Address before: Queensland, Australia

Patentee before: Ireland biotech Co

C17 Cessation of patent right
CX01 Expiry of patent term

Expiration termination date: 20130326

Granted publication date: 20000119