CN101666786A - Method for packing separation column and nozzle needle integrated capillary column and manufacturing stopper - Google Patents
Method for packing separation column and nozzle needle integrated capillary column and manufacturing stopper Download PDFInfo
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- CN101666786A CN101666786A CN200810213432A CN200810213432A CN101666786A CN 101666786 A CN101666786 A CN 101666786A CN 200810213432 A CN200810213432 A CN 200810213432A CN 200810213432 A CN200810213432 A CN 200810213432A CN 101666786 A CN101666786 A CN 101666786A
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Abstract
The invention relates to a method for packing a separation column and a nozzle needle integrated capillary column and manufacturing a stopper, which comprises the following steps: preparing a chromatography packing into a homogenate with a certain concentration; reversely pressing the homogenate into the capillary column to pack by nitrogen under a certain pressure, wherein one end of the capillary column is a tapered taper; sintering the chromatography packing at the mouth of the taper to form the stopper; and during the process of sintering, using a stainless steel tube to control the lengthof the stopper and protect the chromatography packing at the back of the stopper. The method for packing the separation column and the nozzle needle integrated capillary column and manufacturing thestopper is simple and fast to operate without special equipment and high in success ratio. The capillary column packed according to the method has high separation efficiency and good separation reproducibility; and the stopper manufactured according to the invention has small volume, no sample adsorption and no post-column effect. The method for packing the separation column and the nozzle needleintegrated capillary column and manufacturing the stopper has very good application value in the fields of protein sciences, micro environments and biological sample analyses based on capillary liquidchromatography-electrospray ionization mass spectrometry technology.
Description
Technical field
The present invention relates to filling of a kind of separating column and nozzle needle integrated capillary column and stopper method for making, belong to chromatogram, mass spectrophotometry field.
Background technology
In recent years, along with the fast development of protein science research, microscopic capillary liquid chromatography-electro-spray ionization mass spectrum (nano-LC-ESI-MS) obtains application more and more widely.The microscopic capillary liquid chromatography is used the separating column of 20～300 microns of internal diameters, and corresponding mobile phase flow rate is generally received at per minute tens and is raised to hundreds of and receives liter.By electron spray nozzle needle (interior) ionization, be introduced into mass spectrum by electric field from the component of capillary separation column wash-out then through being tens microns tapered tube.For liquid chromatography separating column (comprising capillary liquid chromatography separating column and common liquid chromatography separating column), generally all to stop the chromatograph packing material of filling in the post, prevent its leakage at seben/stopper of the terminal use of post.At present, the stopper that uses in capillary liquid chromatography and capillary electric chromatogram mainly contains sintering stopper, gel one colloidal sol stopper, organic polymer stopper, magnetic particle stopper, single-particle stopper, stainless steel stopper and Teflon film stopper.
In nano-LC-ESI-MS, use one zero dead volume, the two logical microscopic capillary separating column and the electron spray nozzle needles that will have above-mentioned stopper to be linked together usually; Yet, even zero dead volume two is logical, still can introduce extra column effect, cause the chromatographic peak broadening.Separating column and electron spray nozzle needle are integrated (an end drawing-down that is about to the microscopic capillary post is that taper is as the electron spray nozzle needle), the filler that utilization is filled in the kapillary bell is self-assembled into " arch bridge " stopper, stop the filler of filling in the post, can effectively avoid using the connection two logical chromatographic peak broadenings that cause.Yet a shortcoming of this capillary column is: when not having moving phase in the capillary column, the filler of " arch bridge " stopper that forms at the kapillary bell can take place to reset and run off, and causes packing leaking in the capillary separation column.There is the researcher that monolithic silica column and polystyrene integral post and electron spray nozzle needle are integrated, constitute incorporate capillary column, obtained reasonable separating effect, but, this integrated capillary column making step is very loaded down with trivial details, and because the intrinsic low sample charge capacity of integral post has limited their application.
In sum, in order to guarantee that capillary separation column has enough sample charge capacity, should use the capillary separation column of packing chromatography filler, in order to reduce the outer bands of a spectrum broadening of post as far as possible, should use separating column and electron spray nozzle needle integrated capillary column, yet the problem that faces at present is not have very effective separating column and filling of electron spray nozzle needle integrated capillary column and stopper method for making.
Summary of the invention:
At the problems referred to above, the purpose of this invention is to provide filling of a kind of separating column and nozzle needle integrated capillary column and stopper method for making.
1. separating column and nozzle needle integrated capillary column packing method, as shown in Figure 1.This packing method belongs to low pressure homogenate method, and being suitable for an end drawing-down is the filling of taper quartz capillary column.With organic solvent chromatograph packing material is made into certain density homogenate, the centrifuge tube that fills homogenate places in the homogenate jar; Capillary column one end is passed homogenate cover insert homogenate, homogenate jar and homogenate cover are sealed with four screws; Open reduction valve, under the nitrogen pressure effect, homogenate slowly enters capillary column, and finally is full of capillary column; Nitrogen pressure is slowly reduced to zero, unload capillary column, logical capillary column is connected on the liquid chromatography pump by one little two, utilize high-pressure flow that liquid chromatography pump produces with the chromatograph packing material compacting in the capillary column, as shown in Figure 2.
Above-mentioned chromatograph packing material is a kind of in normal-phase chromatography filler, reverse-phase chromatography filler, the ion-exchange chromatography filler, and the particle diameter of filler is 3～10 microns.In order to prevent chromatograph packing material sedimentation in the filling process, in homogenate, place a stirrer, whole homogenate jar is placed on the magnetic stirring apparatus, the speed control of stirrer is at 100～200r/min.
Under nitrogen pressure, homogenate slowly moves to capillary column bell direction, and when arriving the capillary column bell, the homogenate solvent flows out from bell, and chromatograph packing material forms " arch bridge " stopper under bell stops, stop that the filler of back moves forward.Because homogenate does not stop to move up in the homogenate jar, chromatograph packing material is full of capillary column gradually.When just beginning to load, use less nitrogen pressure, prevent that filler from moving that too fast to cause kapillary bell chromatograph packing material to be filled undesirable, after this, along with the increase of filling length, nitrogen pressure is increased to 1MPa gradually.
When using nitrogen pressure that chromatograph packing material is pressed into capillary column, can use a kind of disposable of filler described in the claim 3 that capillary column is filled up, also can segmentation fill, be that leading portion is filled the reverse-phase chromatography filler, back segment is filled the ion-exchange chromatography filler, perhaps leading portion is filled the reverse-phase chromatography filler, and interlude is filled the ion-exchange chromatography filler, and back segment is filled the reverse-phase chromatography filler; Filler selection can be the combination in any between described 3 kinds of fillers, thereby obtains to have the capillary column of different separating properties.
When using in the high-pressure flow phase compacting capillary column that liquid chromatography pump produces chromatograph packing material, maximum pressure between 15MPa and 20MPa, both guaranteed with filler press closely, solid, obtain Gao Zhuxiao, prevent the excessive damage chromatograph packing material of pressure again.
2. separating column and electron spray nozzle needle integrated capillary column stopper method for making, as shown in Figure 3.This method belongs to sintering chromatograph packing material legal system and makes stopper, and being suitable for an end drawing-down is the quartz capillary column of taper.A stainless-steel tube is enclosed within on the capillary column of packing chromatography filler, with a stainless steel threeway capillary column and liquid chromatography pump is connect, pump keeps the moving phase of certain flow rate; The kapillary bell is stretched out certain-length from stainless-steel tube, and the chromatograph packing material with flame sintering kapillary bell place forms the sintering stopper.
During packed capillary column, filler can form a self assembly stopper (because arch bridge effect) at the kapillary bell to chromatograph packing material under the nitrogen effect, stops that the filler of back is revealed, but this stopper instability.By the chromatograph packing material at sintering bell place, can make the self assembly stopper become a highly stable sintering stopper.For the length of control sintering stopper with prevent to damage chromatograph packing material in the capillary column when the sintering, use a stainless steel protection pipe box on capillary column.Simultaneously, when the sintering chromatograph packing material,, keep the moving phase of certain flow rate in the capillary column in order to prevent excessive sintering.
Separating column of the present invention and nozzle needle integrated capillary column packing method have the following advantages: (1) filling process is simple, and the nitrogen pressure that comes out from reduction valve is 1MPa to the maximum, handling safety; (2) filling process does not need specific apparatus, equipment, implements very easy; (3) success ratio of filling capillary column is very high, more than 90%; (4) capillary column of filling separates favorable reproducibility; (5) the capillary column post of filling is imitated high.
Separating column of the present invention and nozzle needle integrated capillary column stopper method for making have the following advantages: (1) operation is very simple, quick, and on average the Production Time of each stopper was less than 3 minutes; (2) do not need specific apparatus, equipment and reagent, common liquid-phase chromatographic analysis laboratory just can be realized; (3) cost of manufacture is very low, and the volume of (4) stopper is very little, to separating not influence; (5) stopper does not have suction-operated to sample, can not introduce the outer chromatographic peak broadening of post.
Description of drawings:
Fig. 1. the filling synoptic diagram of separating column and electron spray nozzle needle integrated capillary column.(a), capillary column inserts the homogenate jar and prepares filling; (b) chromatograph packing material soon loads full capillary column.11. the capillary column bell, 12. capillary columns, 13. sealing screws, 14. homogenate cover, 15. the centrifuge tube of shipment slurries, 16. chromatograph packing material homogenates, 17. magnetons, 18. homogenate jar, 19. magnetic stirring apparatus, 110. nitrogen transfer tubes, 111. nitrogen cylinders, 112. the chromatograph packing material of filling in the kapillary, the filler at 113. kapillary bell places.
Fig. 2. use the synoptic diagram of the capillary column of liquid chromatography pump compacting filling.21. the liquid chromatography pump woven hose, 22. moving phases, 23. little threeways, the chromatograph packing material of filling in 24. capillary columns, 25. capillary columns, the chromatograph packing material of 26. capillary column bells, 27. little distributing T-pipe kapillaries.
Fig. 3. separating column and nozzle needle integrated capillary column stopper manufacturing process synoptic diagram.31. liquid chromatography pump woven hose, 32. moving phase, 33. little threeway, the chromatograph packing material of filling in 34. capillary columns, 35. capillary columns, 36. stainless-steel tube, 37. the chromatograph packing material of capillary column bell, 38. butane spray guns, 39. butane spray gun internal flames, 310. butane spray gun flame envelope, 311. little distributing T-pipe kapillaries.
Fig. 4. separating column and nozzle needle integrated capillary column stopper picture that the present invention makes.41. stopper, 42. chromatograph packing materials, 43. capillary walls.
Fig. 5. use the separating column of the present invention's filling/making and nozzle needle integrated capillary column analysis bovine serum albumin(BSA) (BSA) trypsase to cut the chromatogram (three parallel analysiss) of peptide section.
Fig. 6. the capillary column of self assembly stopper is analyzed bovine serum albumin(BSA) (BSA) trypsase and is cut the chromatogram (three parallel analysiss) of peptide section.The same Fig. 5 of condition.
Embodiment
Embodiment 1
The filling of separating column and electron spray nozzle needle integrated capillary column: with the C of 5mL centrifuge tube 15 preparation 2mL-5mg/mL-5 μ m
18Reverse phase filler-methyl alcohol homogenate, interior placement magneton 17; Centrifuge tube is put into 18 li in homogenate jar, and the homogenate jar is placed on the magnetic stirring apparatus 19, keeps the rotating speed of 200r/min; Internal diameter 75 μ m, bell internal diameter 15 μ m, length 12cm capillary column 12 seals up the homogenate jar with sealed screw 13 by in the insertion homogenate 16 shown in Figure 1; Open the nitrogen reduction valve, the adjusting nitrogen pressure is 0.1MPa; Under nitrogen pressure, filler slowly moves to capillary column bell direction, and after 2 hours, filler is full of capillary column, in this process, increases nitrogen pressure gradually to 1MPa; Capillary column is taken off from the homogenate jar, with little threeway 23 capillary column is connected on the liquid chromatography pump, little threeway one end is connected with the long shunting kapillary of internal diameter 250 μ m, 50cm; The moving phase of liquid chromatography pump keeps 0.001mL/min, 0.002mL/min, and 0.005mL/min, 0.01mL/min, 0.02mL/min, 0.03mL/min each 30 minutes, in this process, the liquid chromatography pump pressure is 15MPa to the maximum; Flow rate of mobile phase is reduced to zero, unload capillary column, obtain separating column and electron spray nozzle needle integrated capillary column from little threeway.
Embodiment 2
The making of separating column and nozzle needle integrated capillary column stopper: the stainless-steel tube of a long 3cm, internal diameter 0.5mm, external diameter 1.6mm is enclosed within on the capillary column of embodiment 1 filling, use little threeway 33 that capillary column 34 and liquid chromatography pump are connect, little threeway one end connects the shunting kapillary of internal diameter 250 μ m, 50cm; The moving phase of liquid chromatography pump keeps 0.01mL/min; The capillary column bell is stretched out 0.25 millimeter from stainless-steel tube, and with the filler of flame sintering kapillary bell, forming length is the sintering stopper of 0.25mm; Flow rate of mobile phase is reduced to zero, unload capillary column.
Embodiment 3
Be used for the actual sample analysis according to the separating column of implementing 1 and 2 preparations with nozzle needle integrated capillary column and stopper, the result as shown in Figure 5.As a comparison, under similarity condition, use the same sample of self assembly stopper capillary column analysis, the result as shown in Figure 6.Contrast two figure, as can be seen, the separating column and the incorporate sintering stopper of the nozzle needle capillary column of the present invention's preparation have better separating effect.
Chromatographic condition: mobile phase A, 0.1% formic acid-2% acetonitrile, Mobile phase B, 0.1% formic acid-80% acetonitrile; Mobile phase B is increased to 50% from 5% linearity in the 90min, and Mobile phase B is linear in the 10min then increases by 100%, flow velocity 200nL/min.Mass spectrum condition: m/z=400～1600 full scans selects 6 highest peaks to carry out secondary scanning after a full scan is finished.Instrument: the nano-LC-Packing of the Dai An company chromatogram thermoelectric linear ion hydrazine mass spectrum (LTQ) that is coupled.The trypsase of the bovine serum albumin(BSA) of sample: 1pmol (BSA) is cut the peptide section.
Claims (16)
1. separating column and nozzle needle integrated capillary column packing method may further comprise the steps:
(1) the chromatograph packing material homogenate of preparation 5mg/mL places in the homogenate jar;
(2) homogenate is put into a magneton in the homogenate jar;
(3) under stirring state, use the nitrogen of 0.1～1MPa that homogenate oppositely is pressed into capillary column;
(4) capillary column is connected on the liquid chromatography pump, with the chromatograph packing material in the moving phase compacting capillary column.
2. packing method according to claim 1 is characterized in that: described capillary column is the quartz capillary column of 20～300 microns of internal diameters, and capillary column one end is tapered bell, and the bell internal diameter is 10～30 microns; Described bell is as the nozzle needle of capillary column.
3. packing method according to claim 1 is characterized in that: described chromatograph packing material is a kind of in normal-phase chromatography filler, reverse-phase chromatography filler, the ion-exchange chromatography filler, and the particle diameter of filler is 3～10 microns.
4. packing method according to claim 1 is characterized in that: the solvent of described homogenate be methyl alcohol, ethanol, isopropyl alcohol, acetonitrile, acetone and chloroform etc. approaching with packing density, to filler do not have the infringement organic solvent.
5. packing method according to claim 1, it is characterized in that: homogenate oppositely is pressed into the capillary column step at the nitrogen that uses 0.1～1MPa, can use disposable capillary column is filled of a kind of filler in the claim 3 to expire, also can segmentation fill, leading portion is filled the reverse-phase chromatography filler, and back segment is filled the ion-exchange chromatography filler, and perhaps leading portion is filled the reverse-phase chromatography filler, interlude is filled the ion-exchange chromatography filler, and back segment is filled the reverse-phase chromatography filler; Filler selection can be the combination in any between described 3 kinds of fillers.
6. packing method according to claim 1 is characterized in that: described liquid chromatography pump operation flow rate of mobile phase step gradient, and each step gradient keeps 30～60min, chromatograph packing material in the compacting capillary column; The maximum column head pressure that described flow rate of mobile phase step gradient obtains is greater than 15MPa, less than 20MPa; Described moving phase is a kind of in methyl alcohol, acetonitrile, the ethanol.
7. packing method according to claim 1 is characterized in that: use a little threeway that capillary column is connected with liquid chromatography pump; Described little threeway one end is connected with the shunting kapillary, is used for the fast pressure relief of liquid chromatography pump.
8. press the capillary column that claim 1 is loaded for one kind, it is characterized in that: described capillary column is a quartz capillary column, and internal diameter is 20～300 microns, and an end is the bell of 10～30 microns of internal diameters, fills 3～10 microns chromatograph packing material in the post; Described capillary column is mainly used in capillary liquid chromatography-electrospray ionization mass spectrum analysis.
9. separating column and nozzle needle integrated capillary column stopper method for making may further comprise the steps:
(1) stainless-steel tube is enclosed within on the capillary column of filling according to claim 1;
(2) use a little threeway, capillary column is connected with the liquid chromatography infusion pump, moving phase keeps the flow velocity of 0.01～0.02mL/min;
(3) the capillary column bell is stretched out 0.2～0.5 millimeter from stainless-steel tube, the filler with flame sintering kapillary bell forms stopper.
10. stopper method for making according to claim 9 is characterized in that: described stainless-steel tube is used for controlling the length of stopper and the chromatograph packing material of protection stopper back as protection tube, and the internal diameter of stainless-steel tube is equal to or slightly greater than the external diameter of capillary column.
11. stopper method for making according to claim 9 is characterized in that: the internal diameter of described capillary column bell is for being 10～30 microns.
12. stopper method for making according to claim 9 is characterized in that: described chromatograph packing material is a kind of in normal-phase chromatography filler, reverse-phase chromatography filler, the ion-exchange chromatography filler, and the particle diameter of filler is 3～10 microns.
13. stopper method for making according to claim 9 is characterized in that: the chromatograph packing material that is filled in the capillary column bell with the flame sintering forms, and forms stopper.
14. stopper method for making according to claim 9 is characterized in that: described flame is the flame envelope of butane flame, also can be other temperature other flame in butane flame envelope temperature range.
15. stopper method for making according to claim 9 is characterized in that: during with flame sintering kapillary bell chromatograph packing material, moving phase keeps the flow velocity of 0.01～0.02mL/min, prevents the excessive sintering of filler; Described moving phase is a kind of in methyl alcohol, ethanol, the acetonitrile.
16. the capillary column stopper by claim 9 preparation, it is characterized in that: described stopper is the sintering stopper, is positioned at the bell of capillary column, and length is 0.2～0.5mm; Stopper has inertia, to not absorption of sample, can not introduce the post aftereffect.
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| CN103399109A (en) * | 2013-08-15 | 2013-11-20 | 宋家玉 | Special apparatus for coating gas-phase capillary column |
| CN104548663A (en) * | 2013-10-21 | 2015-04-29 | 天津汉荣生物技术有限公司 | Flow-dividing baffle for homogenate tank for filling chromatographic column |
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| CN110568086A (en) * | 2018-06-05 | 2019-12-13 | 深圳华大生命科学研究院 | Capillary chromatographic column device and liquid chromatographic separation method |
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| CN103399109A (en) * | 2013-08-15 | 2013-11-20 | 宋家玉 | Special apparatus for coating gas-phase capillary column |
| CN104548663A (en) * | 2013-10-21 | 2015-04-29 | 天津汉荣生物技术有限公司 | Flow-dividing baffle for homogenate tank for filling chromatographic column |
| CN106525955A (en) * | 2017-01-03 | 2017-03-22 | 山东省分析测试中心 | Device and method for dispersive solid-phase extraction- magnetic needle desorption electricity rising atomizing ionized mass spectrometry of magnetic nanoparticles |
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| CN110568086A (en) * | 2018-06-05 | 2019-12-13 | 深圳华大生命科学研究院 | Capillary chromatographic column device and liquid chromatographic separation method |
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| CN111323527A (en) * | 2018-12-13 | 2020-06-23 | 湖南德米特仪器有限公司 | Method for simultaneously measuring multiple psychotropic drugs by using composite two-dimensional liquid chromatography |
| CN111323527B (en) * | 2018-12-13 | 2022-12-02 | 湖南德米特仪器有限公司 | Method for simultaneously measuring various psychotropic drugs by using composite two-dimensional liquid chromatography |
| CN111855877A (en) * | 2019-04-30 | 2020-10-30 | 中国科学院上海微系统与信息技术研究所 | MEMS-based multi-stationary-phase miniature packed column structure and preparation method thereof |
| CN113406227A (en) * | 2021-06-15 | 2021-09-17 | 上海君谊生物科技有限公司 | Novel capillary analytical column and method for realizing ultrahigh-sensitivity protein mass spectrum detection |
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Open date: 20100310 |