CN108254478A - A kind of easy refitting regeneration method for preparing chromatographic column - Google Patents
A kind of easy refitting regeneration method for preparing chromatographic column Download PDFInfo
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- CN108254478A CN108254478A CN201810052177.4A CN201810052177A CN108254478A CN 108254478 A CN108254478 A CN 108254478A CN 201810052177 A CN201810052177 A CN 201810052177A CN 108254478 A CN108254478 A CN 108254478A
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- column
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/50—Conditioning of the sorbent material or stationary liquid
- G01N30/56—Packing methods or coating methods
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/20—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
- B01D15/203—Equilibration or regeneration
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The present invention relates to a kind of easy refitting regeneration method for preparing chromatographic column, used chromatographic column directly discarded the technical issues of leading to waste is mainly solved.Its method is as follows：1. what will be reset prepares column cap opening, dirty filler is removed；2. weighing 2 times of new fillers of removal filler quantity, homogenate is carried out with solvent dissolving；3. taking an old void column pipe with resetting column same size model, inner wall is cleaned and dried, its column tail with resetting the column cap of column is connect, is sealed with sealing ring；4. homogenate is poured into above void column pipe in 2 column tubes connected, column cap is covered later and is tightened；5. choosing high phase liquid chromatogram prepares pump 1 or 2, column tube is connected with preparing pump, according to the selected corresponding leacheate of Fillers selection, turn on pump is prepared by preparing to be pumped into column, can recycle leacheate after leacheate replaces homogenate completely to reduce leacheate usage amount；6. termination of pumping after leacheate rinses 2 hours stands, the connector among 2 pillars is removed, slowly removes void column pipe above, following at this time preparing should fill up filler in column, and column cap is installed after replacing sieve plate.
Description
Technical field
The present invention relates to the refitting regeneration methods for preparing chromatographic column.
Background technology
As people have found that the work of new lead compound is increasingly drawn from microorganism, ocean and land higher organisms
Play extensive interest, it is often necessary to be isolated from a large amount of or a small amount of mixture in effective, quick, inexpensive method pure
Compound.And the purpose of chromatography is prepared, pure material is exactly obtained from mixture.Therefore chromatography extensive use at present is prepared
In pharmaceuticals industry, biotechnology, biomedicine and biochemical research, the energy, food, cosmetics, environmental science, drug and micro-
Many fields such as biology.In chromatography is prepared, in order to accelerate the efficiency that is detached with raising of time of separation, prepare chromatography into
Sample size is very big, causes to prepare the corresponding increasing of the segregational load of chromatography pillar, when chromatography on-column sample, which loads, to be increased,
It often leads to column effect drastically to decline, causes to prepare that the service life of column is often very short with analytical column compared with, and prepare that major gene loads fills out
The more cost of doses is also corresponding higher.Therefore how effective extension prepares the service life of column as the key of cost is reduced.
It is that sample load capacity is big to prepare the main reason for effect decline of column column is fast, so being mainly column in fact when column is imitated and declined
The filler on head point is polluted by sample, and the filler of pillar stage casing and bottom is still clean available, leads to nothing when column effect declines
When method obtains the product purity needed, general company can only buy finished product and prepare column again, still can be used in discarded old pillar
Filler waste.
Invention content
The object of the present invention is to provide a kind of easy refitting regeneration methods for preparing chromatographic column, mainly solve used
Chromatographic column is directly discarded the technical issues of leading to waste.
The technical scheme is that：A kind of easy refitting regeneration method for preparing chromatographic column, includes the following steps：
1. what will be reset prepares column cap opening, dirty part filler is removed；
2. weighing 2 times of new fillers of removal filler quantity, homogenate is carried out with corresponding solvent dissolving；
3. taking an old void column pipe with resetting column same size model, inner wall is cleaned and dried, by its column tail and refitting column
Column cap connection, sealed with sealing ring to ensure no leakage；
4. the homogenate mixed is poured into above void column pipe in 2 column tubes connected, column cap is covered later and is tightened；
5. choosing high phase liquid chromatogram prepares pump 1 or 2, column tube is connected with preparing pump, according to selected Fillers selection
Corresponding leacheate, turn on pump are prepared by preparing to be pumped into column, can be followed leacheate after leacheate replaces homogenate completely
Ring is using to reduce leacheate usage amount；
Termination of pumping after 6. leacheate rinses 0.5-2 hours stands half an hour, the connector among 2 pillars is removed, is slowly removed
Void column pipe above, following at this time preparing should fill up filler in column, column cap is installed after replacing sieve plate.
Column tube inside diameter ranges are in 20mm-50mm.The total flow for preparing pump is related to column tube internal diameter size, and 20mm internal diameters always flow
Speed is best using 50-100ml/min, 30mm internal diameters overall flow rate is less than 150ml/min, with 80-120ml/ less than 100ml/min
Min is best, and 50mm internal diameters overall flow rate is less than 200ml/min, best with 150-180ml/min；Leacheate washing time is excellent
It selects 1.5-2 hours.
The beneficial effects of the invention are as follows：It is expensive due to preparing column, it is that cost is most in each company's prepare compound link
High easily-consumed products, and most enterprises prepare specification and packing variety difference of column etc. because the product quantity requirement prepared is different
Deng can all have the column for preparing of many variety classes and model, usage amount is also very big, and cost is very high, but these companies are general
All without packing column machine, prepare column once column imitate reduce can only be abandoned once separating effect is deteriorated should not, but filling out in pillar in fact
Material majority can also continue to use, and the present invention is exactly to prepare column using department to fill up the column for preparing of no packing column machine
Column effect decline after how the technology of oneself refitting, the present invention effectively extension can prepare the service life of column, and saving prepares making for column
Use cost.
Description of the drawings
Fig. 1 prepares column for the embodiment of the present invention 1 and resets front pillar effect figure.
Fig. 2 prepares column for the embodiment of the present invention 1 and resets rear pillar effect figure.
Fig. 3 prepares column for the embodiment of the present invention 2 and resets front pillar effect figure.
Fig. 4 prepares column for the embodiment of the present invention 2 and resets rear pillar effect figure.
Specific embodiment
Hereinafter with reference to example, the present invention is described in further detail, but the present invention is not restricted to these specific example
Embodiment 1：A kind of easy refitting regeneration method for preparing chromatographic column, includes the following steps：
1. what will be reset prepares column cap opening, dirty part filler is removed；Prepare column specification：Internal diameter 20mm, length are
250mm；
2. weighing 2 times of new fillers of removal filler quantity, homogenate is carried out with solvent dissolving；
3. taking an old void column pipe with resetting column same size model, the soft brush of inner wall is cleaned up, it is clear with alcohol later
It washes and dries, its column tail is connect with resetting the column cap of column, sealed to ensure no leakage with sealing ring；
4. the homogenate mixed is poured into above void column pipe in 2 column tubes connected, column cap is covered later and is tightened；
5. choosing high phase liquid chromatogram prepares pump 2, the flow velocity for setting every pump is 50ml/min, and column tube is pumped phase with preparing
Even, according to the selected corresponding leacheate of Fillers selection, turn on pump is prepared by preparing to be pumped into column, treats leacheate by homogenate
Leacheate can be recycled to reduce leacheate usage amount after replacing completely；
Termination of pumping after 6. leacheate rinses 2 hours stands half an hour, the connector among 2 pillars is removed, is slowly removed above
Void column pipe, following at this time preparing should fill up filler in column, column cap is installed after replacing sieve plate.
Test pole effect condition be：Mobile phase A：The TFA of+0.1% mass percentage concentration of acetonitrile of 100% mass percentage concentration
（Trifluoroacetic acid）, Mobile phase B：The TFA of+0.1% mass percentage concentration of pure water, flow velocity：20ml/mim, wavelength：254nm, sample：
Naphthalene.
The column effect of this root pillar is before refitting：474（Theoretical cam curve）, see Fig. 1, qualified product can not have been prepared,
Pillar column effect reaches 11384 after refitting（See Fig. 2）, it is entirely capable of reaching the requirement for preparing column, the preparation available for product.
Embodiment 2：An internal diameter 50mm is reset according to 1 step of embodiment, length prepares column for 250mm's, with 2 flow velocitys
Preparation for 200ml/min pumps connection, and the flow velocity of every pump is set to be reset for 180ml/min.Leacheate rinses 1.5 hours
Termination of pumping afterwards, the condition of test pole effect are：Mobile phase A：The TFA of+0.1% mass percentage concentration of acetonitrile of 100% mass percentage concentration
（Trifluoroacetic acid）, Mobile phase B：The TFA of+0.1% mass percentage concentration of pure water, flow velocity：80ml/mim, wavelength：254nm, sample：
Naphthalene.
The column effect of this root pillar is before refitting：490（See Fig. 3）, qualified product, pillar column after refitting can not have been prepared
Effect reaches 9448（See Fig. 4）, it is entirely capable of reaching the requirement for preparing column, the preparation available for product.
Embodiment 3 prepares column internal diameter as 30mm, and the flow velocity of every pump is set to be reset for 100ml/min.Leacheate rushes
Termination of pumping after washing 1.7 hours, remaining is the same as embodiment 1.
Embodiment 4 prepares column internal diameter as 30mm, and the flow velocity of every pump is set to be reset for 80ml/min.Leacheate rushes
Termination of pumping after washing 2 hours, remaining is the same as embodiment 1.
Embodiment 5 prepares column internal diameter as 20mm, and the flow velocity of every pump is set to be reset for 70ml/min.Leacheate rushes
Termination of pumping after washing 1.8 hours, remaining is the same as embodiment 1.
Embodiment 6. prepares column internal diameter as 20mm, and the flow velocity of every pump is set to be reset for 100ml/min.Leacheate rushes
Termination of pumping after washing 1.5 hours, remaining is the same as embodiment 1.
Embodiment 7. prepares column internal diameter as 30mm, and the flow velocity of every pump is set to be reset for 120ml/min.Leacheate rushes
Termination of pumping after washing 1.5 hours, remaining is the same as embodiment 1.
Embodiment 8. prepares column internal diameter as 50mm, and the flow velocity of every pump is set to be reset for 150ml/min.Leacheate rushes
Termination of pumping after washing 1.7 hours, remaining is the same as embodiment 1.
Embodiment 9. prepares column internal diameter as 50mm, and the flow velocity of every pump is set to be reset for 165ml/min.Leacheate rushes
Termination of pumping after washing 2 hours, remaining is the same as embodiment 1.
Claims (5)
1. a kind of easy refitting regeneration method for preparing chromatographic column, it is characterized in that：Include the following steps：
1. what will be reset prepares column cap opening, dirty part filler is removed；
2. weighing 2 times of new fillers of removal filler quantity, homogenate is carried out with corresponding solvent dissolving；
3. taking an old void column pipe with resetting column same size model, inner wall is cleaned and dried, by its column tail and refitting column
Column cap connection, sealed with sealing ring to ensure no leakage；
4. the homogenate mixed is poured into above void column pipe in 2 column tubes connected, column cap is covered later and is tightened；
5. choosing high phase liquid chromatogram prepares pump 1 or 2, column tube is connected with preparing pump, according to selected Fillers selection
Corresponding leacheate, turn on pump are prepared by preparing to be pumped into column, can be followed leacheate after leacheate replaces homogenate completely
Ring uses；
Termination of pumping after 6. leacheate rinses 0.5-2 hours stands half an hour, the connector among 2 pillars is removed, is slowly removed
Void column pipe above, following at this time preparing should fill up filler in column, column cap is installed after replacing sieve plate.
2. a kind of easy refitting regeneration method for preparing chromatographic column according to claim 1, it is characterized in that：Column tube internal diameter
Range is in 20mm-50mm.
3. a kind of easy refitting regeneration method for preparing chromatographic column according to claim 1, it is characterized in that：Prepare pump
Total flow is related to column tube internal diameter size, and 20mm internal diameters overall flow rate is less than 100ml/min, and 30mm internal diameters overall flow rate is less than 150ml/
Min, 50mm internal diameter overall flow rate are less than 200ml/min.
4. a kind of easy refitting regeneration method for preparing chromatographic column according to claim 3, it is characterized in that：Column tube internal diameter
Overall flow rate is 50-100ml/min during 20mm, and overall flow rate is 80-120ml/min during column tube internal diameter 30mm, during column tube internal diameter 50mm
Overall flow rate is 150-180ml/min.
5. a kind of easy refitting regeneration method for preparing chromatographic column according to claim 1, it is characterized in that：Leacheate follows
Ring rinses 1.5-2 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810052177.4A CN108254478A (en) | 2018-01-19 | 2018-01-19 | A kind of easy refitting regeneration method for preparing chromatographic column |
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| CN201810052177.4A CN108254478A (en) | 2018-01-19 | 2018-01-19 | A kind of easy refitting regeneration method for preparing chromatographic column |
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| CN201810052177.4A Pending CN108254478A (en) | 2018-01-19 | 2018-01-19 | A kind of easy refitting regeneration method for preparing chromatographic column |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111249771A (en) * | 2020-02-24 | 2020-06-09 | 中国科学院长春应用化学研究所 | Preparation method and regeneration method of chromatographic column for purifying gram-grade mechanical functional protein on large scale |
| CN112843789A (en) * | 2020-12-29 | 2021-05-28 | 上海赛梵科分离技术有限公司 | Regeneration method of chromatographic packing and chromatographic medium in cannabidiol purification |
| CN112933660A (en) * | 2020-09-11 | 2021-06-11 | 石家庄新奥环保科技有限公司 | Regeneration method of ion chromatography protective column |
| CN113318483A (en) * | 2020-02-28 | 2021-08-31 | 内蒙古伊利实业集团股份有限公司 | Regeneration method of chromatographic column |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111249771A (en) * | 2020-02-24 | 2020-06-09 | 中国科学院长春应用化学研究所 | Preparation method and regeneration method of chromatographic column for purifying gram-grade mechanical functional protein on large scale |
| CN113318483A (en) * | 2020-02-28 | 2021-08-31 | 内蒙古伊利实业集团股份有限公司 | Regeneration method of chromatographic column |
| CN112933660A (en) * | 2020-09-11 | 2021-06-11 | 石家庄新奥环保科技有限公司 | Regeneration method of ion chromatography protective column |
| CN112843789A (en) * | 2020-12-29 | 2021-05-28 | 上海赛梵科分离技术有限公司 | Regeneration method of chromatographic packing and chromatographic medium in cannabidiol purification |
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Application publication date: 20180706 |