CN1393443A

CN1393443A - Process for preparing dihydromyricetin from porcelain ampelopsis

Info

Publication number: CN1393443A
Application number: CN 01114564
Authority: CN
Inventors: 张友胜
Original assignee: 张友胜
Current assignee: Guangzhou Baidi Bio-technology Co., Ltd.
Priority date: 2001-06-29
Filing date: 2001-06-29
Publication date: 2003-01-29

Abstract

A process for prparing dihydromyricetin from bigdentate ampelopsis includes such steps as providing the dried stems and leaves of bigdentate ampelopsis, immersion extracting in water or alcohol at 50-100 deg.c for 0.5-3 hr, vacuum-filtering, concentrating the filtrate to obtain coarse dihydromyricatin, drying, purifying and refining. The resultant dihydromyricatin is a medicine for arrhythmia, myocardial ischemia, hypertension, obesity, etc.

Description

Produce the method for dihydromyricetin with porcelain ampelopsis

The present invention relates to a kind of method of producing dihydromyricetin with porcelain ampelopsis.

Showing tooth snake plant Ampelopsis grossedentata (Hand.-Mazz.) W.T.Wang. is a kind of wild vine of Vitaceae Ampelopsis.Mainly be distributed in provinces and regions such as China Guangdong, Guangxi, Yunnan, Guizhou, Hunan, Hubei, Jiangxi, Fujian.Mutation A.cantoniesis (H.et.A.) Pl.var.grossedentata Hand-Mazz for ampelopsis cantoniensis.The provinces and regions Zhuang such as China Guangxi, Hunan and the people of the Yao nationality its young young stem and leaf commonly used is gone into tea, and make tea summer do not turn sour a few days, has " title of refreshing tea ", also claims " vine tea ", " white tea ", " Maoyanmei tea ".Complete stool is medicinal, flavor is sweet, light, cool in nature, have effects such as clearing heat and detoxicating, wind-damp dispelling, strengthening the bones and muscles.Among the people its young stem and leaf is made health tea, be used for the treatment of diseases such as heating, swelling and pain in the throat, icterohepatitis, blister furuncle, the use history in existing hundreds of years.Ampelopsis grossedentata mainly is distributed in 400-1300 rice above sea level, concentrates or scattered wild reserves are big in the mixing in the woods of hillside, distribute and growth rhythm more clear, make wild change man plant the expansion stock number easily in addition.Be the wild plant resource that can directly utilize.

Studies confirm that, mainly contain dihydromyricetin isoreactivity composition in the porcelain ampelopsis body, wherein contain dihydromyricetin in the young leaflet tablet that pluck March to September and reach 35% (dry weight).

Dihydromyricetin (dihydromyricetin) has another name called Ampelopstin (ampelopsin), holds back element (ampelopsin), dihydromyricetin flavones (dihydromyricetin), ampelopsin (ampelopsin) in vain.Traditionally, people are called for short dibydro myricetrin (dihydromyricetin), and it comprises multiple isomers, and chemical structural formula is as follows:

In recent years, pharmacological evaluation both domestic and external shows: it has obvious antagonism norepinephrine and high K ⁺Due to rabbit thoracic aorta bar contractile response and calcium antagonism, and toxicity is low, can be used as anti-arrhythmia, resist myocardial ischemia, antihypertensive newtype drug; Tool significantly eliminates the phlegm, anti-inflammatory, cough-relieving, lipopenicillinase, liver protection function; Tool is significantly removed the effect of alcoholism; The formation of tool obvious suppression extracorporeal platelet aggregation and thrombus in vivo, blood fat reducing and glucose level, SOD activity improving is expected to be developed as one, two national kind new medicines.

In the plant of having found that contains this composition, this component content is very low, let alone industrialization extraction, purified problem.So this composition fails to be used widely always.

Purpose one of the present invention is to extract dihydromyricetin from porcelain ampelopsis, the 2nd, with the thick dihydromyricetin that extracts purify, refining be dihydromyricetin 90% or more, a kind of method with porcelain ampelopsis production dihydromyricetin promptly is provided

The objective of the invention is to realize with the following methods.

Get the dry cauline leaf of porcelain ampelopsis, water or ethanol are pressed solid-liquid ratio 1: (1-20) under 50-100 ℃ temperature, lixiviate 0.5-3 hour, filtration under diminished pressure, concentrated filtrate, the crude extract of dihydromyricetin, the dry raw extract, the dry thing of thick dihydromyricetin, again it is purified and makes with extra care.

The purification of thick dihydromyricetin, refining: two kinds of methods are arranged:

A: the hot water that is soluble in that utilizes dihydromyricetin, can be dissolved in the characteristics of cold water again, put the crude extract of dihydromyricetin cold, or with (70-100 ℃) dissolving in hot water of thick dihydromyricetin, it is cold that lysate is put, just separate out a large amount of dihydromyricetin crystal in the solution, filtration under diminished pressure, filtrate reenter extractor, filter residue leaves standstill, filters with hot water dissolving and cooling again, continue preceding step,, can add small amount of activated with among the hot water dissolving, purification speed is accelerated in the decolouring impurity elimination.Through 4-10 time the circulation, can be with the rough monomer that is purified to purity＞90% of thick dihydromyricetin, its technological process of production as shown in Figure 1, that is:

Fig. 1 is a kind of technological process of production figure of the present invention

Produce the gained filter residue by technological process shown in Figure 1 and use the hot water dissolving, heavy Multiple process flow steps shown in Figure 1.

With cocycle the 7-8 time the dihydromyricetin list more than＞90% Body, the 9-10 time dihydromyricetin monomer more than＞95%.

B method: the dihydro that utilizes uniform temperature (50 ℃ more than-100 ℃) When the myricetin crude extract passes through macroporous absorbent resin, the macroporous absorption tree Fat mainly adsorb the characteristics of impurity and make with extra care, the purification dihydromyricetin.

The water-soluble liquid of dihydromyricetin crude extract or dry thing, insulation Or heating makes solution 50 ℃ of temperature more than-100 ℃, and solution insulation is logical Cross first large pore resin absorption column, speed 2-3 column volume/hour, mistake Filtrate is continued under keeping warm mode by second, the 3rd macroporous absorption Resin column. The number of times that solution is crossed post requires the purity of product to decide on manufacturer, Crossing for the first time behind the large pore resin absorption column product purity can be more than 70%, Cross for the second time that the large pore resin absorption column product can reach more than 80%, cross the 3rd Inferior large pore resin absorption column product can reach more than 90%. Such as need high-purity more Product (more than 95%), then can make for the third time large pore resin absorption column The post liquid cooling of crossing but leave standstill, filtration under diminished pressure, dry filter residue namely get 95% with The dihydromyricetin of upper purity.

The technical problem that the invention solves: the one, in the minimum feelings of cost Extract to greatest extent dihydromyricetin in the aobvious tooth mattae under the condition; The 2nd, under simple scenario, purify, refining dihydromyricetin.

Below be non-limiting examples of the present invention:

Embodiment 1: get the dry cauline leaf of porcelain ampelopsis, water is pressed solid-liquid ratio 1: 10 under 100 ℃ temperature, lixiviate 1 hour, filtration under diminished pressure, concentrated filtrate, the crude extract of dihydromyricetin, the dry raw extract, the dry thing of the thick dihydromyricetin of purity about 40%, again it is purified and makes with extra care.

The purification of thick dihydromyricetin, refining: the hot water that is soluble in that utilizes dihydromyricetin, be insoluble in the characteristics of cold water, put the crude extract of dihydromyricetin cold, or with (80 ℃) dissolving in hot water of the dry thing of thick dihydromyricetin, it is cold that lysate is put, just separate out a large amount of dihydromyricetin crystal in the solution, filtration under diminished pressure, filtrate reenter extractor, filter residue leaves standstill, filters with hot water dissolving and cooling again, continue preceding step,, can add small amount of activated with among the hot water dissolving, purification speed is accelerated in the decolouring impurity elimination.Through 8 circulations, thick dihydromyricetin can be purified to the monomer of purity＞90%.

Embodiment 2: get the dry cauline leaf of porcelain ampelopsis, water is pressed solid-liquid ratio 1: 10 under 100 ℃ temperature, lixiviate 1 hour, filtration under diminished pressure, concentrated filtrate, the crude extract of the dihydromyricetin of purity about 40%, the dry raw extract, the dry thing of thick dihydromyricetin, again it is purified and makes with extra care.

The purification of thick dihydromyricetin, refining: the dihydromyricetin crude extract that utilizes certain temperature (50-100 ℃) is during by NKA-9 (department of chemistry of Nankai University product) macroporous adsorbent resin, macroporous adsorbent resin mainly adsorb the characteristics of impurity and make with extra care, the purification dihydromyricetin.

The water-soluble liquid of dihydromyricetin crude extract or dry thing, insulation or heating make solution in the insulation of the temperature more than 50-100 ℃ → solution by first NKA-9 (department of chemistry of Nankai University product) macroporous adsorptive resins, speed 2 column volumes/hour → filtered liquid continues under keeping warm mode by second, the 3rd NKA-9 macroporous adsorptive resins.The number of times that solution is crossed post requires the purity of product to decide on manufacturer, product purity can be more than 70% after crossing the NKA-9 macroporous adsorptive resins first time, crossing for the second time behind the NKA-9 macroporous adsorptive resins product purity can be more than 80%, can reach more than 90% after macroporous adsorptive resins product for the third time.As the more highly purified product of need (more than 95%), the post liquid cooling of crossing of macroporous adsorptive resins was for the third time but left standstill, filtration under diminished pressure, dry filter residue promptly gets the dihydromyricetin of 95% above purity.

Claims

1, a kind of method of producing dihydromyricetin with porcelain ampelopsis, it is characterized in that getting the dry cauline leaf of porcelain ampelopsis, water or ethanol are pressed solid-liquid ratio 1: (1-20) under 50-100 ℃ temperature, lixiviate 0.5-3 hour, filtration under diminished pressure, concentrated filtrate, get the crude extract of dihydromyricetin, the dry raw extract, the dry thing of the thick dihydromyricetin of purity about 40%, again it is purified and makes with extra care.

2, according to the described method of producing dihydromyricetin with porcelain ampelopsis of claim 1, it is characterized in that the purification of thick dihydromyricetin, refining is the hot water that is soluble in that utilizes dihydromyricetin, be insoluble in the characteristics of cold water, put the crude extract of dihydromyricetin cold, or with (70-100 ℃) dissolving in hot water of thick dihydromyricetin, it is cold that lysate is put, just separate out a large amount of dihydromyricetin crystal in the solution, filtration under diminished pressure, filtrate reenters extractor, filter residue leaves standstill with hot water dissolving and cooling again, filter, continue preceding step, in using the hot water dissolving, can add small amount of activated, purification speed is accelerated in the decolouring impurity elimination.Through 4-10 circulation, can be with the rough monomer that is purified to purity＞90% of thick dihydromyricetin.

3, according to the described method of producing dihydromyricetin with porcelain ampelopsis of claim 1, it is characterized in that the purification of thick dihydromyricetin, refining is the dihydromyricetin crude extract during by macroporous adsorbent resin that utilizes certain temperature (more than 50-100 ℃), macroporous adsorbent resin mainly adsorbs the characteristics of impurity and makes with extra care, the purification dihydromyricetin, the water-soluble liquid of dihydromyricetin crude extract or dry thing, insulation or heating make solution in the insulation of the temperature more than 50-100 ℃ → solution by first macroporous adsorptive resins, speed 2-3 column volume/hour → filtered liquid continues under keeping warm mode by second, the 3rd macroporous adsorptive resins.The number of times that solution is crossed post requires the purity of product to decide on manufacturer, product purity can be more than 70% after crossing the macroporous adsorptive resins first time, crossing for the second time behind the macroporous adsorptive resins product purity can be more than 80%, can reach more than 90% after macroporous adsorptive resins product purity for the third time.As the more highly purified product of need (more than 95%), the post liquid cooling of crossing of macroporous adsorptive resins was for the third time but left standstill, filtration under diminished pressure, dry filter residue promptly gets the dihydromyricetin of 95% above purity.