CN200951333Y

CN200951333Y - Chromatographic separation equipment

Info

Publication number: CN200951333Y
Application number: CN 200620046198
Authority: CN
Inventors: 殷翔
Original assignee: FUHUA PHARMALEUTICAL INDUSTRY Co Ltd SHANGHAI
Current assignee: Fudan Shanghai Polytron Technologies Inc; Fuhua Pharmaleutical Industry Co., Ltd., Shanghai
Priority date: 2006-09-22
Filing date: 2006-09-22
Publication date: 2007-09-26
Anticipated expiration: 2016-09-22

Abstract

The utility model relates to a chromatography separating device, which comprises N (N is a positive integer) chromatographic columns (1) and a vacuum concentrator (2); the outflux of the chromatographic columns (1) passes through a first pipeline (3) and is connected with the inlet of the vacuum concentrator (2); the outlet of the vacuum concentrator (2) passes through a second pipeline (4) and is connected with the influx of the chromatographic columns (1); the N chromatographic columns (1) are connected with each other in parallel; a sieve plate (11) which has silicone (12) for blocking the silicone is arranged at the inner bottom part of the chromatographic columns (1); the utility model has the advantages of high producing efficiency, high processing capacity, low solvent consumption, and effective protection of physical health of operators.

Description

The chromatography device

Technical field

The utility model relates to the device that a kind of field of medicaments is used, and relates in particular to chromatography separator in a kind of GTW separation and Extraction.

Background technology

Thunder godvine Tripterygium wilfordii Hook.f is the xylem of Celastraceae plant tripterygium root.Its leaf, flower and fruit also can be used as medicine, and have another name called water thick grass, gelsemium elegan, herba fibraureae recisae, adopt worm medicine etc.Thunder godvine is recorded in Shennong's Herbal the earliest as medicine, has another name called thick grass.The plant that belongs to together still has tripterygium hypoglaucum hutcs T.hypoglacum (Levl.) Hukeda. Cangshan thunder godvine T.forretii Dials. and northeast thunder godvine T.regelli Sprague et Takeda..Thunder godvine has obtained extensive use clinically because of having significant anti inflammatory immunity regulating action.According to incompletely statistics, it has been used for more than 50 kind of treatment of diseases such as rheumatism, skin disease, ephrosis, also has bright prospects aspect antitumor and the anti-rejection of organ transplant.

GTW is the Diterpenes component based on triptolide.The separation-extraction technology of GTW is to form with alcohol extract, chloroform extraction, three steps of chromatography, wherein chromatography is wherein crucial long step consuming time, its principle is the performance by the silica gel selective absorption, cooperate the eluant, eluent of opposed polarity, GTW is separated from the thunder godvine extract.

Be by some opening glass column (H1m in the laboratory with the separating layer analysis system in the prior art, Φ 120mm) and Rotary Evaporators form, silica gel is packed in the opening glass column, thunder godvine extract dissolving back adds, eluant, eluent flows through silica gel, GTW wash-out from silica gel is come out, and Rotary Evaporators concentrates the solution under the wash-out, and the eluant, eluent of recovery can use repeatedly, this system's production efficiency is low, solvent consumption is big, and treating capacity is low, and operating personnel are subjected to solvent easily and poison.

Summary of the invention

The utility model technical issues that need to address have provided a kind of chromatography device, are intended to solve above-mentioned defective.

In order to solve the problems of the technologies described above, the utility model is achieved through the following technical solutions:

The utility model comprises: N chromatographic column and vacuum concentrator, and N is a positive integer; The flow export of described chromatographic column joins by the import of first pipeline and vacuum concentrator; The outlet of vacuum concentrator is joined by the inflow entrance of second pipeline and chromatographic column; It between the described N chromatographic column relation in parallel; Also settle a sieve plate that intercepts silica gel at the inner bottom part of chromatographic column, on the sieve plate 11 that intercepts silica gel, silica gel 12 is arranged.

Compared with prior art, the beneficial effects of the utility model are: the production efficiency height, and treating capacity is big, and solvent consumption is little, can effectively protect health of operators.

Description of drawings

Fig. 1 is the structure chart of a chromatographic column of the utility model;

The specific embodiment

Below in conjunction with the accompanying drawing and the specific embodiment the utility model is described in further detail:

As seen from Figure 1: the utility model comprises: N chromatographic column 1 and vacuum concentrator 2, and N is a positive integer; The flow export of described chromatographic column 1 joins by first pipeline 3 and the import of vacuum concentrator 2; The outlet of vacuum concentrator 2 is joined by the inflow entrance of second pipeline 4 with chromatographic column 1; It between the described N chromatographic column 1 relation in parallel; Also settle a sieve plate 11 that intercepts silica gel at the inner bottom part of chromatographic column 1, on the sieve plate 11 that intercepts silica gel, silica gel 12 is arranged;

The material of described chromatographic column 1, first pipeline 3 and second pipeline 4 is stainless steels.

The utility model is by stainless steel chromatography post, and vacuum concentrator and stainless steel pipes are formed.Wherein, chromatographic column is made up of the tube and the lower end sieve plate of hollow type, the purpose of sieve plate is to allow flow of solution to cross but prevent that chromatographic silica gel runs off, sieve plate also can be by the nylon mesh screen, ceramic wafer, the other materials that glass fibre etc. can reach identical function substitutes, the lower end of chromatographic column is the flow of solution outlet, link to each other with vacuum concentrator by the stainless steel pipes system, solution enters vacuum concentrator and goes out solvent by concentrating and separating, return chromatographic column by stainless steel pipes again, form the industrial production device of a sealing and circulating, chromatographic silica gel is packed into promptly forms the separation and Extraction tomographic system in the chromatography.

The vacuum concentrator that adopts in the utility model is a prior art products, form by vaporization chamber and recovery chamber, solution is separated into solvent gas and highly concentrated solution in vaporization chamber, solvent gas enters the recovery chamber and is condensed into solvent liquid, recyclable, can concentrate solution by vacuum concentrator.

The separation and Extraction tomographic system that can form all size according to the quantity of chromatographic column and inspissator.Application of the present utility model can alleviate the labour intensity that the GTW chromatography is produced significantly, reduces solvent consumption, improves disposal ability.

The glass column tomographic system that the utility model and laboratory are used is compared as follows:

(dropping into the medicinal material amount is 7.2 tons)

Glass types column chromatography system the utility model

Used chromatographic column 90 6

28 tons 5 tons of solvent consumptions

Required artificial/days 30 days 4 days

The production environment difference is good

The utility model is compared with the glass column tomographic system and is had the following advantages:

1. disposal ability is big: stainless steel chromatography post is 15 times of a glass column loading.

2. concentrating capacity is strong: the concentrating capacity of vacuum concentrator is 400kg/h, and the concentrating capacity 20kg/h of rotary concentrator is 20 times of the latter.

3. solvent consumption is little: the utility model is closed conduit production, compares with the uncovered production of glass column tomographic system, and solvent evaporates is reduction significantly, and solvent consumption is also few a lot.

4. production environment is good: the utility model is closed conduit production, compares with the uncovered production of glass column tomographic system, and solvent evaporates is reduction significantly, and solvent gas content is very low in the whole production surrounding air.

5. required artificial few: be semi-automatic production system, required manually need only 4 people, and the glass column tomographic system is used a large amount of chromatographic columns and rotary concentrator, manually significantly increases.

Embodiment

1. assembling

(1) 100-200 order chromatographic silica gel can be ordered from the Qingdao Haiyang special silica-gel.

(2) select stainless steel chromatography post for use, specification is 200*40cm.

(3) equilibrium liquid (chloroform)

Use is rinsed well and dry chromatographic column, adds chloroform to 1/3 height, pours chromatographic silica gel then into and also stirs, and makes and silica gel natural subsidence in post must not leave bubble in the post bed, closes loam cake, and goes up the stainless steel pipes system continuously.

2. the preparation of thunder godvine spice

The thunder godvine meal is put in the extraction pot, divided to add ethanol heating extraction for three times, the merging extract concentrates, and must extract medicinal extract.

Extract medicinal extract and change in the extraction pot, divide secondary to add chloroform soln, extraction, combining extraction liquid concentrates, and must extract medicinal extract.

Add extraction medicinal extract in the silica gel, stir evenly, dry, pulverize the thunder godvine spice.

3. chromatographic step

Add chromatographic silica gel 65KG in the chromatographic column (200*40cm), thunder godvine spice 50KG adds chloroform to silica gel and just is submerged, and stablizes 4 hours, uses the chloroform wash-out then, and the flow velocity of post is controlled at about 2ml/ second.The silica G thin plate is checked, disappears to before prolonging place's blue-fluorescence spot.

Change solvent (10% methyl alcohol chloroform soln) and carry out the chromatography wash-out, the flow velocity of post is controlled at about 2ml/ second, and the silica G thin plate is checked, to the disappearance of standard point spot, stop chromatography, merge concentrated (thickening temperature 40-60 ℃, vacuum 0.04-0.06MPa), get GTW.

The evaluation of GTW:

Isolated GTW can adopt chromogenic reaction, and high performance liquid chromatography can be done qualitative and quantitative detection.

Claims

1. chromatography device comprises: N chromatographic column (1) and vacuum concentrator (2), and N is a positive integer; It is characterized in that: the flow export of described chromatographic column (1) joins by first pipeline (3) and the import of vacuum concentrator (2); The outlet of vacuum concentrator (2) is joined by the inflow entrance of second pipeline (4) with chromatographic column 1; It between the described N chromatographic column (1) relation in parallel; Also settle a sieve plate (11) that intercepts silica gel at the inner bottom part of chromatographic column (1), on the sieve plate (11) that intercepts silica gel, silica gel (12) is arranged.

2. chromatography device according to claim 1 is characterized in that: the material of described chromatographic column (1), first pipeline (3) and second pipeline (4) is a stainless steel.