CN109011698B - On-line cleaning and storing method for silica gel filler separation column - Google Patents
On-line cleaning and storing method for silica gel filler separation column Download PDFInfo
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- CN109011698B CN109011698B CN201810976703.6A CN201810976703A CN109011698B CN 109011698 B CN109011698 B CN 109011698B CN 201810976703 A CN201810976703 A CN 201810976703A CN 109011698 B CN109011698 B CN 109011698B
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- 238000000926 separation method Methods 0.000 title claims abstract description 174
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 121
- 239000000741 silica gel Substances 0.000 title claims abstract description 121
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 121
- 239000000945 filler Substances 0.000 title claims abstract description 112
- 238000000034 method Methods 0.000 title claims abstract description 52
- 238000004140 cleaning Methods 0.000 title claims abstract description 47
- 239000012156 elution solvent Substances 0.000 claims abstract description 34
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 32
- 230000000694 effects Effects 0.000 claims abstract description 23
- 239000007864 aqueous solution Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 235000019253 formic acid Nutrition 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000012856 packing Methods 0.000 claims abstract description 9
- 238000002791 soaking Methods 0.000 claims abstract description 5
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 33
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 19
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- 238000003860 storage Methods 0.000 claims description 13
- 238000005086 pumping Methods 0.000 claims description 10
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 9
- JLPULHDHAOZNQI-ZTIMHPMXSA-N 1-hexadecanoyl-2-(9Z,12Z-octadecadienoyl)-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCC\C=C/C\C=C/CCCCC JLPULHDHAOZNQI-ZTIMHPMXSA-N 0.000 claims description 8
- 238000001223 reverse osmosis Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000004587 chromatography analysis Methods 0.000 claims description 2
- 229940083466 soybean lecithin Drugs 0.000 claims description 2
- JZNWSCPGTDBMEW-UHFFFAOYSA-N Glycerophosphorylethanolamin Natural products NCCOP(O)(=O)OCC(O)CO JZNWSCPGTDBMEW-UHFFFAOYSA-N 0.000 description 8
- WTJKGGKOPKCXLL-RRHRGVEJSA-N phosphatidylcholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCCC=CCCCCCCCC WTJKGGKOPKCXLL-RRHRGVEJSA-N 0.000 description 7
- 239000008347 soybean phospholipid Substances 0.000 description 7
- 238000004440 column chromatography Methods 0.000 description 6
- 150000008104 phosphatidylethanolamines Chemical class 0.000 description 5
- RYCNUMLMNKHWPZ-SNVBAGLBSA-N 1-acetyl-sn-glycero-3-phosphocholine Chemical compound CC(=O)OC[C@@H](O)COP([O-])(=O)OCC[N+](C)(C)C RYCNUMLMNKHWPZ-SNVBAGLBSA-N 0.000 description 3
- CWRILEGKIAOYKP-SSDOTTSWSA-M [(2r)-3-acetyloxy-2-hydroxypropyl] 2-aminoethyl phosphate Chemical compound CC(=O)OC[C@@H](O)COP([O-])(=O)OCCN CWRILEGKIAOYKP-SSDOTTSWSA-M 0.000 description 3
- HQVFCQRVQFYGRJ-UHFFFAOYSA-N formic acid;hydrate Chemical compound O.OC=O HQVFCQRVQFYGRJ-UHFFFAOYSA-N 0.000 description 3
- 150000003905 phosphatidylinositols Chemical class 0.000 description 3
- 230000002159 abnormal effect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010829 isocratic elution Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
Images
Classifications
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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
- B01D15/42—Selective adsorption, e.g. chromatography characterised by the development mode, e.g. by displacement or by elution
- B01D15/424—Elution mode
- B01D15/426—Specific type of solvent
-
- 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
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
- Silicon Compounds (AREA)
- Detergent Compositions (AREA)
Abstract
The invention discloses an on-line cleaning and storing method of a silica gel filler separation column, which comprises the following steps: a. cleaning the silica gel filler separation column on line; b. and (4) storing the silica gel filler separation column on line. Step a is carried out by the following steps: a1. washing the silica gel filler in the separation column with formic acid aqueous solution; a2. washing the silica gel filler in the separation column with pure water to replace the formic acid aqueous solution therein; a3. the silica gel packing in the separation column is equilibrated with an elution solvent. Step b soaking the separation column which is completely cleaned in an aqueous solution of an elution solvent. According to the online cleaning and storing method for the silica gel filler separation column, the separation column does not need to be detached and the silica gel filler does not need to be taken out, the operation process is simple and easy to control, the silica gel filler is free of loss, the separation effect can be restored, the separation operation of the silica gel filler separation column is optimized, and the separation effect is improved; after the silica gel filler separation column is cleaned and stored by adopting the method, the separation performance of the silica gel filler in the separation column can be completely restored to the original performance.
Description
Technical Field
The invention relates to a cleaning method and a storage method of a separation column, in particular to an on-line cleaning and storage method of a silica gel filler separation column.
Background
Soybean phospholipids are composed of Phosphatidylcholine (PC), Phosphatidylethanolamine (PE), Phosphatidylinositol (PI), Lysophosphatidylcholine (LPC), Lysophosphatidylethanolamine (LPE), and the like, and have properties very close to each other, and it is very difficult to separate them. When high-purity soybean phospholipid (PC ≧ 90%) is produced in large quantities, silica gel separation filler is commonly used for separation and production.
At present, after the preparation of high-purity soybean phospholipid by adopting a silica gel filler separation column chromatography method is finished, the silica gel filler separation column is usually soaked and stored by using an elution solvent (without water), and along with the increase of preparation frequency, the following problems are easy to occur in the process of separating and preparing the high-purity soybean phospholipid by using the existing silica gel filler separation column: 1. the column pressure of the separation column rises; 2. the separation effect of the separation column is obviously reduced, under the condition of the same sample amount and separation conditions, the time for separating each component is moved forward, the whole separation time is shortened, and the separation effect of PC and LPC, PI and LPE is obviously reduced. And the normal state can not be recovered after the washing by the common 50 to 85 percent aqueous elution solvent.
Disclosure of Invention
In view of the defects in the prior art, the invention provides an on-line cleaning and storing method for a silica gel filler separation column, so as to improve the separation effect of the silica gel filler separation column and optimize the separation operation of the silica gel filler separation column.
In order to solve the technical problems, the invention adopts the technical scheme that: the method for cleaning and storing the silica gel filler separation column on line comprises the following steps:
a. the silica gel filler separation column is cleaned on line and is carried out by the following steps:
a1. washing the silica gel filler in the separation column with formic acid aqueous solution;
a2. washing the silica gel filler in the separation column with pure water to replace the formic acid aqueous solution therein;
a3. balancing the silica gel filler in the separation column with an elution solvent;
b. and (3) online storage of the silica gel filler separation column: and soaking the cleaned silica gel filler separation column in an elution solvent water solution.
Furthermore, the silica gel filler separation column is a high pressure liquid chromatography column, and the diameter-height ratio of the silica gel filler separation column is 0.01-3.
Furthermore, in the step a1, 0.45-0.6% formic acid aqueous solution is used for washing the silica gel filler in the separation column for not less than 3 hours, and the flow rate of the formic acid aqueous solution is 30-60 mL/min.
Further, the silica gel packing in the separation column is washed with reverse osmosis pure water at a flow rate of 50mL/min to 70mL/min for not less than 30min in step a2.
Further, the elution solvent is one or a mixture of n-hexane, n-heptane and ethyl acetate.
Further, in step a3, the elution solvent is pumped into the separation column, and other solvents in the separation column are replaced, and the time for pumping the elution solvent is not less than 30 min.
Further, in the step b, the silica gel filler separation column which is balanced is soaked in an elution solvent aqueous solution containing 10 to 20 percent of water.
Further, the method comprises the following steps between step a3 and step b:
a4. detecting the column effect of the silica gel filler separation column: in order to verify the separation effect of the separation column after being cleaned by the online cleaning method for the silica gel filler separation column, the method comprises the following steps:
a4-1, pumping 1.0mL-5.0mL of 1% toluene solution into the separation column;
4-2, using methanol as a mobile phase, eluting the 1% toluene solution in the separation column for 20-30min under the conditions of a flow rate of 40-55 mL/min, a column temperature of 40 ℃ and an ultraviolet wavelength of 254nm, and measuring a liquid chromatogram to obtain an effective column plate number of the separation column, wherein when the effective column plate number is not less than 1500, the separation effect of the silica gel filler separation column is recovered.
Further, in step a4-2, the 1% toluene solution in the separation column was eluted isocratically using 100% methanol as a mobile phase at a flow rate of 50mL/min, a column temperature of 40 ℃ and an ultraviolet wavelength of 254 nm.
According to the online cleaning and storing method for the silica gel filler separation column, the separation column does not need to be detached and the silica gel filler in the separation column does not need to be taken out, the operation process is simple and easy to control, the silica gel filler is not lost, the separation effect can be recovered, the separation operation of the silica gel filler separation column is optimized, and the separation effect is improved; after the silica gel filler separation column is cleaned and stored by adopting the cleaning and storing method, the separation performance of the silica gel filler in the separation column can be completely recovered to the original state (when the column is initially loaded).
Drawings
FIG. 1 is a liquid chromatogram obtained by column chromatography in example 1 of the present invention.
Detailed Description
The invention provides an on-line cleaning and storage method for a silica gel filler separation column, which is characterized in that in the process of separating and preparing high-purity PC and PE products by taking soybean phospholipid as a raw material and adopting a silica gel filler separation column chromatography, when the pressure of the silica gel filler separation column is abnormal or the separation degree is reduced, the silica gel filler separation column is cleaned by adopting the on-line cleaning method, the cleaning refers to cleaning of the silica gel filler in the silica gel filler separation column, after the cleaning is qualified, the storage method is adopted to store the separation column for the next column chromatography operation, the column chromatography separation operation can also be carried out after the cleaning is qualified, and after the separation is finished, the separation column is stored by adopting the storage method.
The silica gel filler separation column is a high-pressure liquid chromatography column, the diameter-height ratio of the silica gel filler separation column is 0.01-3, and preferably, the height of the separation column is not more than 1000 mm.
The invention provides an on-line cleaning and storing method of a silica gel filler separation column, which comprises the following steps:
a. the method comprises the following steps of (1) cleaning a silica gel filler separation column on line, specifically, cleaning the silica gel filler separation column on line by the following steps:
a1. washing the silica gel filler in the separation column with formic acid aqueous solution;
a2. washing the silica gel filler in the separation column with pure water to replace the formic acid aqueous solution therein;
a3. balancing the silica gel filler in the separation column with an elution solvent;
b. and (3) online storage of the silica gel filler separation column: and soaking the cleaned silica gel filler separation column in an elution solvent water solution.
Further, in the step a1, washing the silica gel filler in the separation column with 0.45% -0.6% formic acid water solution for not less than 3 hours, wherein the flow rate of the formic acid water solution is set to be 30-60 mL/min; in step a2, washing the silica gel packing in the separation column with reverse osmosis pure water for not less than 30min, wherein the flow rate of the reverse osmosis pure water is set to be 50 mL/min-70 mL/min, so as to ensure that the formic acid aqueous solution in the silica gel packing is completely replaced; in step a3, pumping the elution solvent into the separation column, and displacing other solvents in the separation column, wherein the time for pumping the elution solvent is not less than 30min, the other solvents refer to formic acid water solution or reverse osmosis pure water which may remain in steps a1 and a2, and preferably, the elution solvent is one or a mixture of n-hexane, n-heptane and ethyl acetate.
The silica gel filler on-line cleaning method is used for directly cleaning the silica gel filler in the separation column, the separation column does not need to be disassembled, the silica gel filler is taken out and then cleaned, and compared with the existing operation of taking the silica gel filler out and cleaning in a container, the operation process is simple and easy to control, the silica gel filler is not lost, the cleaning cost is reduced, and the cleaning efficiency of the silica gel filler is improved.
In the step b, the silica gel filler separation column cleaned in the step a is soaked in an elution solvent aqueous solution containing 10 to 20 percent of water, and as can be understood, the silica gel filler in the separation column is soaked in the elution solvent aqueous solution. It should be noted that the elution solvent in this step is the same as the elution solvent in step a3, except that the aqueous solution of the elution solvent is used to soak the silica gel filler separation column in this step, and the elution solvent in step a3 is 100% of the equilibrium silica gel filler.
The online storage method of the silica gel filler separation column enables the silica gel filler in the separation column to be effectively and safely stored, and can effectively avoid reduction of the separation effect of the silica gel filler separation column.
Further, the online cleaning and storing method of the silica gel filler separation column further comprises the following steps between the step a3 and the step b:
a4. detecting the column effect of the silica gel filler separation column: in order to verify the separation effect of the separation column after being cleaned by the online cleaning method for the silica gel filler separation column, the method comprises the following steps:
a4-1, pumping 1.0mL-5.0mL of 1% toluene solution into the separation column;
4-2, using methanol as a mobile phase, eluting the 1% toluene solution in the separation column for 20-30min under the conditions of a flow rate of 40-55 mL/min, a column temperature of 40 ℃ and an ultraviolet wavelength of 254nm, and measuring a liquid chromatogram to obtain an effective column plate number of the separation column, wherein when the effective column plate number is not less than 1500, the separation effect of the silica gel filler separation column is recovered.
Preferably, in step a4-2, 100% methanol is used as mobile phase, and the 1% toluene solution in the separation column is eluted isocratically at a flow rate of 50mL/min, a column temperature of 40 ℃ and an ultraviolet wavelength of 254 nm.
After the separation effect of the separation column is verified, the separation performance of the silica gel filler is reduced and the original performance can be restored (when the column is initially installed) after the silica gel filler separation column is cleaned by the method for cleaning the silica gel filler separation column.
The invention is further illustrated by the following specific examples:
example 1:
the embodiment provides an online cleaning and storage method for a silica gel filler separation column, which is used for online cleaning and storage of the silica gel filler separation column which takes soybean lecithin as a raw material and adopts a chromatography to prepare high-purity PC and PE products. In the embodiment, the silica gel filler separation column is a dynamic axial compression column (DAC), the inner diameter of the column is 50mm, the column length is 650mm, and the effective packing height is less than or equal to 450 mm.
Specifically, in the process of separating and preparing high-purity PC and PE products, when the pressure of the silica gel filler separation column is abnormal or the separation degree is decreased, the silica gel filler separation column is cleaned by the online cleaning method provided by the embodiment, and the online cleaning method for the silica gel filler separation column includes the following steps:
s1, washing a silica gel filler in a separation column by using 0.5% formic acid aqueous solution, wherein the flow rate of the formic acid aqueous solution is set to be 50mL/min, and washing for 4 hours;
s2, washing the silica gel filler in the separation column for 40min by using reverse osmosis pure water, wherein the flow rate of the reverse osmosis pure water is set to be 50mL/min, so as to ensure that the formic acid aqueous solution in the silica gel filler is completely replaced;
s3, balancing the silica gel filler in the separation column by using an elution solvent, pumping the elution solvent into the separation column, displacing other solvents in the separation column, wherein the pumping time of the elution solvent is 45min, so that the elution solvent completely displaces other solvents in the separation column, and the baseline of the measured liquid chromatogram is a straight line, wherein the elution solvent is ethyl acetate.
In this embodiment, the online cleaning method for the silica gel filler separation column further includes a step of performing column effect detection on the silica gel filler separation column after the cleaning step is completed:
s4, pumping 1% toluene solution into the separation column, wherein the sample volume is 2 mL; and (3) using 100% methanol as a mobile phase, carrying out isocratic elution on the 1% toluene solution in the separation column for 30min under the conditions that the flow rate of the 100% methanol is 50mL/min, the column temperature is 40 ℃ and the ultraviolet wavelength is 254nm, and measuring a liquid chromatogram, wherein the theoretical plate number of the separation column is 6625 and the effective plate number is 6716, and the separation effect is recovered, referring to the attached drawing 1.
And S5, after the column chromatography separation operation of the soybean phospholipid PC50 is carried out by using the silica gel filler separation column with the column effect detection completed in the step S4, soaking the silica gel filler separation column into an aqueous solution of an elution solvent containing 15% of water, wherein the elution solvent is ethyl acetate.
After the silica gel filler is cleaned and stored by the online cleaning and storing method, the silica gel separation column is used for separating the soybean phospholipid PC50 for more than 7 months and more than 150 times, the column pressure is kept between 1.5MPa and 3.0MPa, and the separation effect is still kept as the effect of primary column packing.
Note: the percentage of formic acid solution indicated in the invention is mass percent, and the others are volume percent.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (9)
1. A silica gel filler separation column on-line cleaning and storage method is used for on-line cleaning and storage of a silica gel filler separation column which takes soybean lecithin as a raw material and adopts a chromatography to prepare high-purity PC and PE products, and is characterized by comprising the following steps:
a. the silica gel filler separation column is cleaned on line and is carried out by the following steps:
a1. washing the silica gel filler in the separation column with formic acid aqueous solution;
a2. washing the silica gel filler in the separation column with pure water to replace the formic acid aqueous solution therein;
a3. balancing the silica gel filler in the separation column with an elution solvent;
b. and (3) online storage of the silica gel filler separation column: and soaking the cleaned silica gel filler separation column in an elution solvent water solution.
2. The on-line cleaning and storing method for the silica gel filler separation column according to claim 1, wherein the silica gel filler separation column is a high pressure liquid chromatography column, and the diameter-height ratio thereof is 0.01-3.
3. The on-line cleaning and storing method for the silica gel filler separating column as claimed in claim 1, wherein the silica gel filler in the separating column is washed with 0.45% -0.6% formic acid solution at a flow rate of 30 mL/min-60 mL/min for not less than 3 hours in step a1.
4. The on-line cleaning and storing method for the silica gel packing separation column according to claim 1, wherein the silica gel packing in the separation column is washed with reverse osmosis pure water at a flow rate of 50mL/min to 70mL/min for not less than 30min in step a2.
5. The on-line cleaning and storing method for the silica gel filler separation column according to claim 1, wherein the elution solvent is one or more of n-hexane, n-heptane and ethyl acetate.
6. The on-line cleaning and storing method for the silica gel filler separation column as claimed in claim 1, wherein in step a3, the elution solvent is pumped into the separation column to displace other solvents in the separation column, and the time for pumping the elution solvent is not less than 30 min.
7. The on-line cleaning and storing method for the silica gel filler separation column according to claim 1, wherein in the step b, the silica gel filler separation column which is balanced is soaked in an aqueous solution of an elution solvent with 10-20% of water.
8. The on-line cleaning and storing method for silica gel packed separation column according to claim 1, wherein the method further comprises the following steps between step a3 and step b:
a4. detecting the column effect of the silica gel filler separation column: in order to verify the separation effect of the separation column after being cleaned by the online cleaning method for the silica gel filler separation column, the method comprises the following steps:
a4-1, pumping 1.0mL-5.0mL of 1% toluene solution into the separation column;
4-2, using methanol as a mobile phase, eluting the 1% toluene solution in the separation column for 20-30min under the conditions of a flow rate of 40-55 mL/min, a column temperature of 40 ℃ and an ultraviolet wavelength of 254nm, and measuring a liquid chromatogram to obtain an effective column plate number of the separation column, wherein when the effective column plate number is not less than 1500, the separation effect of the silica gel filler separation column is recovered.
9. The on-line cleaning and storing method for the silica gel packing separation column according to claim 8, wherein in step a4-2, 100% methanol is used as a mobile phase, and the 1% toluene solution in the separation column is eluted isocratically at a flow rate of 50mL/min, a column temperature of 40 ℃ and an ultraviolet wavelength of 254 nm.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1284981A1 (en) * | 1985-03-21 | 1987-01-23 | Московский институт тонкой химической технологии им.М.В.Ломоносова | Method of isolating anion phospholipides |
| CN1771080A (en) * | 2003-04-08 | 2006-05-10 | 诺沃挪第克公司 | Regeneration of Chromatographic Stationary Phases |
| CN101838285A (en) * | 2010-05-07 | 2010-09-22 | 南昌大学 | Method for separating phospholipids in purified oil material |
| US8759753B1 (en) * | 2013-03-14 | 2014-06-24 | Thermo Finnigan Llc | Methods and apparatus for improved immunosuppressant drug monitoring |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150190733A1 (en) * | 2014-01-03 | 2015-07-09 | Ironstone Separations, Inc. | Chromatography methods |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1284981A1 (en) * | 1985-03-21 | 1987-01-23 | Московский институт тонкой химической технологии им.М.В.Ломоносова | Method of isolating anion phospholipides |
| CN1771080A (en) * | 2003-04-08 | 2006-05-10 | 诺沃挪第克公司 | Regeneration of Chromatographic Stationary Phases |
| CN101838285A (en) * | 2010-05-07 | 2010-09-22 | 南昌大学 | Method for separating phospholipids in purified oil material |
| US8759753B1 (en) * | 2013-03-14 | 2014-06-24 | Thermo Finnigan Llc | Methods and apparatus for improved immunosuppressant drug monitoring |
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