CN101598712A - Trace distillate collector - Google Patents
Trace distillate collector Download PDFInfo
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- CN101598712A CN101598712A CNA2009100542201A CN200910054220A CN101598712A CN 101598712 A CN101598712 A CN 101598712A CN A2009100542201 A CNA2009100542201 A CN A2009100542201A CN 200910054220 A CN200910054220 A CN 200910054220A CN 101598712 A CN101598712 A CN 101598712A
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- trace
- kapillary
- distillate collector
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Abstract
The invention provides the trace distillate collector that a kind of liquid chromatography that can be used for complex biological sample and electro spraying ionization-mass spectrometry are analyzed, this trace distillate collector is made up of kapillary, threeway (or four-way), air Bubble generating apparatus and kapillary protective device.Utilize bubble to separate the cut of liquid phase chromatographic resolution gained.A kind of trace distillate collector of the present invention, apparatus is simple, and price is low; Can solve the complex sample cut is collected the sample loss problem, simultaneously when LC-MS, electron spray does not carry out at the gas place, be equivalent to the mass spectrum that stopped, can give and search the ion that the longer selection of time of library software needs, the thrust unit that can stop at any time, mass spectrum has long time to select ion like this, can identify more material not increasing under the situation that sample uses than present LC-MS more.Solved the problem that mass spectral analysis speed does not catch up with liquid-phase chromatographic analysis speed.
Description
Technical field
The present invention relates to a kind of liquid treatment equipment that is used for liquid chromatography and mass spectrometry, in particular, relate to the trace distillate collector that the liquid chromatography that is used for complex biological sample such as protein and electro spraying ionization-mass spectrometry are analyzed.
Background technology
Fraction collector (fraction collector) is the servicing unit of liquid chromatograph and gas chromatograph, is mainly used in preparation and enrichment pure component.When needs provide the standard pure sample or certain component are done further evaluation, usually collect required component in the chromatographic column exit with fraction collector, the moving phase of removing in the cut promptly obtains pure component.Gatherer can cut with craft or automatic control mode by the signal of chromatographic peak outflow.In gas chromatography,, can adopt methods such as solvent absorbing or cold-trap to collect cut because the component boiling point is lower.
Fraction collector is from broadly being divided into two classes.The first kind comprises fraction collector, in this fraction collector, is equipped with a plurality of collection containers on common round turntable.These fraction collectors are commonly referred to as " turntable collectors ", and rotating disk that turntable collectors is generally installed by rotation and rotation are installed and the combination that has an arm of dispensing head is operated to fill a plurality of collection containers.The second class fraction collector comprises the gatherer with a plurality of collection containers and a dispensing head, these collection containers are aligned to lattice on fixed station, this dispensing head is joined and is arranged in two dimensional surface or on all three dimension scales, thereby distributes the liquid to selectively in each collection container.The second class fraction collector is collectively referred to as " X-Y " gatherer.
This two classes fraction collector all has tangible advantage.For example, when handling a large amount of liquid collecting container, the fraction collector with rectangular grid patterns can more effectively hang down and utilize work space.The X-Y gatherer also is more suitable for handling large-scale collection container than the rotating disk that rotation is installed.The X-Y gatherer can be suitable for the universal standard female receptacle as microtiter plate and so in addition, device perhaps other standard or customization.
No matter fraction collector is X-Y type gatherer or carousel-type gatherer, instrument is all complicated, cost an arm and a leg, be difficult to adjusting and maintenance and dispensing head and the collection container volume is all bigger, have bigger dead volume, in the efficient liquid phase chromatographic analysis of complex biological sample, sample size is considerably less, as collecting with above-mentioned fraction collector, sample loss is very big, has brought very big obstruction for ensuing mass spectrophotometry.
On the other hand, when the liquid chromatography of biological sample and electro spraying ionization-mass spectrometry were analyzed now, the analysis speed of liquid chromatography was faster than mass spectral, caused a lot of sample mass spectrums to have little time to analyze and fail evaluation.
Given this, in order to overcome the above problems, now propose a kind of simple in structure, cheap and can be used in the trace distillate collector that the liquid chromatography of complex biological sample such as protein and electro spraying ionization-mass spectrometry are analyzed.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of trace distillate collector, being used to solve LC-MS mass spectrum speed when analytic sample does not on the one hand have liquid-phase chromatographic analysis speed fast, selected complex sample cut is carried out this problem of more deep analysis for the time of mass spectrum abundance.On the other hand, the complex sample cut is collected the sample loss problem.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: a kind of trace distillate collector, it comprises communication apparatus, and this communication apparatus is provided with three interfaces at least, the 3rd interface that is respectively first interface, second interface and connects by kapillary with liquid chromatography;
The collection kapillary of both ends open, described collection kapillary one end is communicated with first interface of communication apparatus, other end emptying or connect mass ion source;
Air Bubble generating apparatus, an end is communicated with second interface of communication apparatus, is used to produce bubble.
As one of preferred version of the present invention, described air Bubble generating apparatus is the syringe that is preset with gas.
As one of preferred version of the present invention, described air Bubble generating apparatus is a solenoid valve, and described solenoid valve one end is communicated with second interface of communication apparatus, and the other end is communicated with the gas source that is equiped with gas.
As one of preferred version of the present invention, described syringe is installed in and is used to inflate the generation bubble on the syringe pump.
As one of preferred version of the present invention, described trace distillate collector further comprises being used to accommodate collects kapillary protective device capillaceous.
As one of preferred version of the present invention, described kapillary protective device comprises being used to accommodate to be collected plastic casing capillaceous and places the interior absorbing matter of plastic casing.
As one of preferred version of the present invention, described collection kapillary center section is wound in annular and is positioned in the kapillary protective device.
As one of preferred version of the present invention, described gas source is the inert gas source of the gas.
As one of preferred version of the present invention, described communication apparatus is stainless steel threeway or four-way.
A kind of trace distillate collector of the present invention, apparatus is simple, and price is low; Can solve the complex sample cut is collected the sample loss problem, simultaneously when LC-MS, electron spray does not carry out at the gas place, be equivalent to the mass spectrum that stopped, can give and search the ion that the longer selection of time of library software needs, the thrust unit that can stop at any time, mass spectrum has long time to select ion like this, can identify more material not increasing under the situation that sample uses than present LC-MS more.Solved the problem that mass spectral analysis speed does not catch up with liquid-phase chromatographic analysis speed.
Description of drawings
Fig. 1 is a trace distillate collector structural representation of the present invention;
Fig. 2 collects form synoptic diagram in the kapillary for the present invention, and wherein A represents cut, and B represents bubble.
The main element symbol description
Collect kapillary 1 kapillary 11
12 communication apparatus 2 are adorned in the kapillary protection
Put
First interface, 21 second interfaces 22
The 3rd interface 23 air Bubble generating apparatus 3
Liquid chromatography 4 gas sources 5
Embodiment
Further specify concrete implementation step of the present invention below in conjunction with accompanying drawing.
A kind of trace distillate collector, be used for the liquid chromatography and the mass spectrometry analysis of complex biological sample, it comprises collection kapillary 1, air Bubble generating apparatus 3, kapillary 11 (quartz capillary), gas source 5 and the liquid chromatography 4 of communication apparatus 2, both ends open, this communication apparatus 2 is provided with three interfaces at least, the 3rd interface 23 that is respectively first interface 21, second interface 22 and connects by kapillary 11 with liquid chromatography; Described communication apparatus 2 can be stainless steel threeway or four-way.
Described collection kapillary 1 one ends are communicated with first interface 21 of communication apparatus 2, other end emptying or connect mass ion source 6, if emptying can be after cut stores any time analyze, be to can be implemented in line analysis if directly connect ion gun.
Kapillary 11 connects liquid chromatography and is used to draw the sample cut, collects kapillary 1 connection first interface 21 and is used for the cut storage.
Described bubble generator 3 can be formed (syringe) by the special-purpose sample introduction needle of chromatogram.One end is communicated with second interface 22 of communication apparatus 2, during use, prepares the gas (nitrogen or other inert gases) that some need, and extracts a part with syringe then.Select the chromatogram sample introduction needle of different volumes for use according to required bubble volume amount difference, manually push required gas flow.
In another embodiment, bubble generator 3 can be made of solenoid valve, solenoid valve one end is communicated with gas source, the other end is communicated with second interface 22 of communication apparatus 2, this solenoid valve has enough little dead volume, thereby can utilize the switch control of circuit controling electromagnetic valve to flow into the gas volume of threeway to reach the demand that satisfies the complex biological sample analysis.
In another embodiment, bubble generator 3 can be made up of mechanical pump (as syringe pump) and syringe, mechanical pump links to each other with gas source (gas in the gas source is nitrogen or other inert gas), thereby regulates the volume that mechanical pump control enters gas in the kapillary at every turn.
Above-mentioned connection is all adopted standard interface to realize connecting and is got final product, and can adopt hickey or other modes to couple together and get final product.
Described trace distillate collector further comprises accommodates the kapillary protective device 12 of collecting kapillary 1.Described kapillary protective device 12 comprises accommodates the plastic casing of collecting kapillary 1 and places the interior absorbing matter of plastic casing.As cotton, sponge etc.Described collection kapillary 1 center section is wound in annular and is positioned in the kapillary protective device 12.Described gas source 5 is source nitrogen or other inert gas sources of the gas.
During use, according to the employed high performance liquid chromatograph flow rate of analysis of biological samples with roughly calculate the cut approximate volume analysis time, according to keeping liquid and bubble is relatively stable and easily be viewed as principle determines used internal diameter capillaceous, determine length capillaceous by internal diameter.As shown in Figure 1 kapillary, threeway, air Bubble generating apparatus etc. are connected, kapillary is wound in annular and is positioned in the kapillary protective device, other end emptying.When needs carried out mass spectrophotometry to sample, then emptying end capillaceous being linked to each other with mass spectral ion source interface got final product.
If operating personnel want directly to analyze stored cut, just can directly insert mass spectral ion gun with collecting an other end capillaceous, the gas that utilizes air Bubble generating apparatus to produce is cut apart liquid, when cut is complete from the chromatographic column wash-out, the chromatogram pump that itself is provided with in the chromatographic apparatus works on, use moving phase rate setting flow velocity as required, the liquid of collecting in the kapillary is pushed mass spectrum, owing to stop at gas section electron spray, in the gas section pump of liquid chromatography is stopped, allowing mass spectrum search library software has the sufficient time to select ion, open the chromatogram pump then and continue to push cut, mass spectrum just can detect and need the material that detects more, when whole bubble cuts at interval that have are all pushed mass spectrum and just finished later on once and analyze.
If will analyze again after a while, collect the other end emptying of kapillary, when needs are analyzed, just can using gases or liquid will collect the interior material of kapillary and push mass spectrum.
If sample is very complicated, want much more as much as possible some things that detect, time that may just stop and more so is not if the sample simple simon says just need.
If the words that using gases pushes, gas comes out from gas source, it generally is steel cylinder, by decompression, flow rate adjustment device, enter air Bubble generating apparatus, if it is just passable to use syringe just to utilize syringe that gas is pushed, use electroceramics valve gauge tap just passable, the injection pump also is the same.If use liquid is connected by coupling arrangement one section open capillaries of kapillary gatherer with the moving phase output pipe of liquid chromatography, utilize the control device of liquid chromatography just can control flow velocity and when stop.
If preferably use solenoid valve when using gases is as thrust unit among the present invention, the relative bubble of gas flow that needs because thrust unit produces and Yan Yaoda many many, it is cumbersome that the words of use syringe will often be got gas, still syringe pump is much better inflating in the bubble, and precision is more better than solenoid valve.
The flow rate that is used for liquid chromatography is known, and the working time is also set, and the cumulative volume of liquid is the product of flow rate and time.The total length of liquid is that cumulative volume is divided by sectional area capillaceous.The volume of bubble and interval time can be set numerical value according to individual demand, and the cumulative volume of bubble is the product of bubble number and bubble volume.The length of bubble be volume of gas divided by the kapillary sectional area, dutycycle is most important one, roughly remains on dutycycle and is about 50% and be optimum condition.
Concrete, the flow velocity C of liquid chromatography is 1ul/min, working time T is 60min, then the cumulative volume V1=C * T=1 * 60=60ul of liquid;
Selecting inside diameter D for use is the kapillary of 250um, sectional area S=∏ then capillaceous * 1/4 (D)
2/ 1000000=0.0490874mm
2, the total length L 1=V1/S/10=122.23cm of liquid then;
Each 30s injects the gas of 0.4ul, the volume V3=0.4u l of bubble then, and be t=30s interval time, the number N=T/t of bubble * 60=60 * 60/30=120;
Cumulative volume V4=V3 * N=0.4 * the 120=48ul of bubble, the volume V2=C * t/60=1ul/min * 30s/60=0.5ul of each liquid;
The length L 2=V2/S/10=0.5/0.0490874/10=1.02cm of each drop, the length of each bubble is L3=V3/S/10=0.4/0.049087/10=0.81cm;
The total length L 4=V4/S/10=48/0.04897/10=97.78cm of bubble;
Dutycycle V=V1/V4+V1=60/60+48=55.56%, because the bubble cumulative volume is 48ul so can select the chromatogram sample introduction needle of 50ul for use, perhaps bigger sample introduction needle all can, as long as just passable, select bubble length and liquid length relatively near like this than being easier to observation greater than 48ul.
Dutycycle is best about 50%, but in fact what it be not special impact effect at, and used length capillaceous can be saved cost under just will taking all factors into consideration.
Therefore, select for use the kapillary of 250mm to get final product as fraction collection.Select the stainless steel threeway for use, kapillary is connected by joint and stainless steel threeway, kapillary is wound in circle and puts into plastic casing, puts absorbing matters such as cotton in the plastic casing in advance well in order to the protective hair tubule, and plastic casing is drawn in outlet capillaceous, emptying.
When cut is carried out mass spectrophotometry, kapillary emptying end is linked to each other with mass spectral ion source interface, utilize air Bubble generating apparatus in collecting kapillary, inflate (or using moving phase liquid) make distillate flow to mass spectrum, because bubble is separated the biological sample cut, missed the sample that to analyze when analyzing during with regard to unnecessary worry screening sample owing to the chromatogram flow velocity is too fast carrying out the mass spectrum selectivity, come the cut of complex biological sample one or more are judged screening for the mass spectrum time enough, can better finish the Analysis and Identification of sample, be adapted to the demand for analysis of present proteomics and genomics more.
The foregoing description is the unrestricted technical scheme of the present invention in order to explanation only.Any technical scheme that does not break away from spirit and scope of the invention all should be encompassed in the middle of the patent claim of the present invention.
Claims (9)
1. trace distillate collector is used for the liquid chromatography and the electro spraying ionization-mass spectrometry analysis of complex biological sample,
It is characterized in that: described trace distillate collector comprises
Communication apparatus (2), this communication apparatus (2) is provided with three interfaces at least, the 3rd interface (23) that is respectively first interface (21), second interface (22) and connects by kapillary (11) with liquid chromatography;
The collection kapillary (1) of both ends open, described collection kapillary (1) one end is communicated with first interface (21) of communication apparatus (2), other end emptying or connect mass ion source;
Air Bubble generating apparatus (3), an end is communicated with second interface (22) of communication apparatus (2), is used to produce bubble.
2. trace distillate collector as claimed in claim 1 is characterized in that: described air Bubble generating apparatus (3) is for being preset with the syringe of gas.
3. trace distillate collector as claimed in claim 1 is characterized in that: described air Bubble generating apparatus (3) is a solenoid valve, and described solenoid valve one end is communicated with second interface (22) of communication apparatus (2), and the other end is communicated with the gas source that is equiped with gas.
4. trace distillate collector as claimed in claim 2 is characterized in that: described syringe is installed in and is used to inflate the generation bubble on the syringe pump.
5. trace distillate collector as claimed in claim 1 is characterized in that: described trace distillate collector further comprises the kapillary protective device (12) that is used to accommodate collection kapillary (1).
6. trace distillate collector as claimed in claim 2 is characterized in that: described kapillary protective device (12) comprises accommodates the plastic casing of collecting kapillary (1) and places the interior absorbing matter of plastic casing.
7. as claim 2 or 3 described trace distillate collectors, it is characterized in that described collection kapillary (1) center section is wound in annular and is positioned in the kapillary protective device (12).
8. trace distillate collector as claimed in claim 1 is characterized in that: described gas source (5) is the inert gas source of the gas.
9. trace distillate collector as claimed in claim 1 is characterized in that: described communication apparatus (2) is stainless steel threeway or four-way.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100542201A CN101598712A (en) | 2009-06-30 | 2009-06-30 | Trace distillate collector |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100542201A CN101598712A (en) | 2009-06-30 | 2009-06-30 | Trace distillate collector |
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| CN101598712A true CN101598712A (en) | 2009-12-09 |
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| CNA2009100542201A Pending CN101598712A (en) | 2009-06-30 | 2009-06-30 | Trace distillate collector |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2506147A (en) * | 2012-09-21 | 2014-03-26 | Univ Bristol | Sampling apparatus providing a series of discrete fluid samples in a tube |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3708948A (en) * | 1971-01-11 | 1973-01-09 | Beckman Instruments Inc | Automatic fraction collector |
| JPS5979157A (en) * | 1982-10-28 | 1984-05-08 | Shimadzu Corp | Thin tube column holder of chromatograph |
| JPH04204375A (en) * | 1990-11-30 | 1992-07-24 | Shimadzu Corp | Fraction collector |
| US5674388A (en) * | 1993-12-20 | 1997-10-07 | Biologica Co. | Apparatus for fractionating components in liquid chromatography |
| US6106710A (en) * | 1999-09-10 | 2000-08-22 | Agilent Technologies, Inc. | Fraction collection delay calibration for liquid chromatography |
| CN101014396A (en) * | 2004-09-10 | 2007-08-08 | 吉尔森公司 | Fraction collector with adjustable tray |
| CN2938091Y (en) * | 2006-08-10 | 2007-08-22 | 北京丰杰华信科学仪器有限公司 | Automatic fraction collector |
-
2009
- 2009-06-30 CN CNA2009100542201A patent/CN101598712A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3708948A (en) * | 1971-01-11 | 1973-01-09 | Beckman Instruments Inc | Automatic fraction collector |
| JPS5979157A (en) * | 1982-10-28 | 1984-05-08 | Shimadzu Corp | Thin tube column holder of chromatograph |
| JPH04204375A (en) * | 1990-11-30 | 1992-07-24 | Shimadzu Corp | Fraction collector |
| US5674388A (en) * | 1993-12-20 | 1997-10-07 | Biologica Co. | Apparatus for fractionating components in liquid chromatography |
| US6106710A (en) * | 1999-09-10 | 2000-08-22 | Agilent Technologies, Inc. | Fraction collection delay calibration for liquid chromatography |
| CN101014396A (en) * | 2004-09-10 | 2007-08-08 | 吉尔森公司 | Fraction collector with adjustable tray |
| CN2938091Y (en) * | 2006-08-10 | 2007-08-22 | 北京丰杰华信科学仪器有限公司 | Automatic fraction collector |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2506147A (en) * | 2012-09-21 | 2014-03-26 | Univ Bristol | Sampling apparatus providing a series of discrete fluid samples in a tube |
| GB2506147B (en) * | 2012-09-21 | 2015-04-29 | Univ Bristol | Sampling apparatus providing a series of discrete fluid samples in a tube |
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Application publication date: 20091209 |