CN104535699B - Prolong suppressor, the efficient liquid phase chromatographic analysis device and method using it before peak shape - Google Patents
Prolong suppressor, the efficient liquid phase chromatographic analysis device and method using it before peak shape Download PDFInfo
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- CN104535699B CN104535699B CN201510005647.8A CN201510005647A CN104535699B CN 104535699 B CN104535699 B CN 104535699B CN 201510005647 A CN201510005647 A CN 201510005647A CN 104535699 B CN104535699 B CN 104535699B
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Abstract
The invention discloses a kind of for prolonging suppressor before the peak shape of efficient liquid phase chromatographic analysis device and analysis method, device core including cutting ferrule and inside the cutting ferrule, the device core is hollow structure and inside is provided with cavity, the end of the device core inner is provided with sieve plate, and the sieve plate connects with the cavity.Also disclose using the efficient liquid phase chromatographic analysis device and method for prolonging suppression before the peak shape so that when flowing through the cavity with the sample solvent of sample, the sample solvent can be by the flowing phase dilution.Advantages of the present invention：Prolong phenomenon before peak shape caused by " sample solvent mismatches with mobile phase " can effectively be suppressed, solve because what " sample solvent " was brought bothers, improve peak shape, add post effect, improve separating degree.The interference that sample solvent is brought when analysis, preparation and method are developed is greatly reduced, is greatly saved human and material resources.
Description
Technical field
The present invention relates to technical field of chromatographic analysis, more particularly to efficient liquid phase chromatographic analysis and preparation, and in particular to one
Prolong suppressor, the efficient liquid phase chromatographic analysis device and method using it before kind peak shape.
Background technology
High performance liquid chromatography is that the industries such as current biology, pharmacy, medical treatment, food, chemical industry carry out production supervision and quality
Most important means and method in control process, the whole world include bio-pharmaceuticals, medical diagnosis, food security and chemical industry quality inspection etc.
In thousands of kinds of compounds more than 80% analyzed with high performance liquid chromatography in field, relate generally to national economy
Every field.With the development in epoch, the improvement of people's living standards, the concern to quality of life and physical and mental health is increasingly
It is more, after the requirement more and more higher to drug quality, medical diagnosis and food security, particularly melamine poison milk powder case, food
Product security fields have become focus of concern, and the national standard of varieties of food items safety is put into effect in succession, major food producer
Numerous and confused purchase high performance liquid chromatograph carries out quality control, and the application of high performance liquid chromatography has arrived further promotion
And popularization.
High performance liquid chromatography may not only be applied to analytical scale, and be widely used in the separation of medicine, the system of purifying
Standby scale field.Complicated in Chinese herbal medicine, impurity content is more, therefrom to extract effective pharmaceutical compositions and make injection and dense
The formulations such as contracting ball, traditional extracting mode often do not reach the purity of modern medicines science requirements, preparation scale high performance liquid chromatography
Application of the method in this field is more and more common；Meanwhile the biologically purifying of active ingredient also be unable to do without high performance liquid chromatography
The application of method.
High performance liquid chromatography is a chromatographic important branch,, will using high pressure transfusion system using liquid as mobile phase
The mobile phases such as the mixed solvent of single solvent or different proportion with opposed polarity, buffer solution are pumped into the chromatogram equipped with stationary phase
Post, after each composition is separated in post, detected into detector, so as to realize the analysis to sample.
As the most important analysis of organic compound, separation means, high performance liquid chromatography is widely used in pharmacy, doctor
The fields such as treatment, food, chemical industry.
A kind of parabola shaped high-efficient liquid phase color is disclosed in the Chinese patent of Application No. 201110071563.6 to compose
Standby post, the capillary liquid chromatography preparation post include：Column cap, parabola shaped tubular cylinder positioned at cylinder top and under cylinder
The post tail in portion；Wherein, the arrival end of parabola shaped tubular cylinder and the port of export respectively there is a special sealing to stretch into part, with
And cylinder is parabola shaped design, and parabolic equation is corresponding with flow velocity, can obtain perfect plug shape chromatographic band, greatly improve
Chromatographic column post is imitated；Cylinder internal diameter is gradually reduced, and adds chromatographic column volume containing the sample, and has a certain amount of enrichment effect to sample, can
Preparation cost is greatly lowered.
The Chinese patent of Application No. 200910219901.9 discloses a kind of tapered high-performance liquid chromatogram preparation column
Column cap structure, including upper lid, seal washer, distribution plate, porous sieve plate with injection port, described chromatogram prepare post cylinder
Intake section is provided with annular inner stopper, and distribution plate is placed in above porous sieve plate, in distribution plate and porous sieve plate embedding sealing packing ring；
Seal washer carries annular male half coupling, and seal washer is embedded into cylinder inner stopper, and seal washer male half coupling is placed in cylinder entrance
Place top；The diameter of circular distribution plate and porous sieve plate is identical and is slightly larger than the inlet inside diameter and seal washer of conical column cylinder
Internal diameter matches；Upper lid is connected with preparing post cylinder by flange.The column cap knot of this tapered high-performance liquid chromatogram preparation column
Structure is adapted to the preparation chromatographic column that inlet diameter is more than 35 millimeters, can improve the post effect of chromatographic column and the symmetry of chromatographic peak.
Often required that when being analyzed and being prepared using liquid chromatography using mobile phase come sample dissolution, so can be with
Obtain symmetrical peak shape and optimal separative efficiency.During development approach, many samples dissolubility in mobile phase is poor,
Yet with the limitation of some objective condition, it is difficult to mobile phase come sample dissolution, have no alternative but that difference need to be used in many cases
Carry out sample dissolution in the solvent of mobile phase, thus cause liquid-phase chromatographic analysis and usually easily occur what is prolonged before peak shape when preparing
Phenomenon, the accuracy of integrating peak areas is had a strong impact on, under causing when being analyzed and being prepared using liquid chromatogram post effect drastically
Drop, separating degree significantly reduces, and separative efficiency is deteriorated, and cubage is very inaccurate, and will be directly affected on liquid phase is prepared point
From purity.
So great influence causes some methods to have to make a change, and the process changed can increase process with before
The cost of processing, some are even had to abandon all work above done, grope method from the beginning, waste substantial amounts of people
Power, material resources.
Efficient liquid-phase chromatography method in current national standard and pharmacopeia, much all because " sample solvent " and the group of mobile phase
Too big into difference and perplex the more, this allows many analysis workers greatly heads for needing to detect their products with these methods
Pain, because method has authority, it is impossible to change easily, and " sample solvent " mismatches with mobile phase in these methods, is this
People have under conditions of original method is not changed, and new pillar are constantly tried out, to a magical chromatogram occur
Post can solve the problems, such as them, but this is not easy very much, even if last problem is resolved, it is a large amount of that them will be also lost in this process
Time, the solvent etc. of energy and costliness, but also will expend it is many be used for chromatographic columns on probation, cause huge resource wave
Take.
In the research process analyzed using high performance liquid chromatography, it has been found that the solvent used in sample dissolution
The reason for having a significant impact to chromatographic isolation, sample was reached in the of short duration time of chromatographic column filler after sample introduction, sample dissolution
Solvent plays double action simultaneously：First effect is the effect of the effect, i.e. sample dissolution of its basis；Second effect is to make
For the effect of mobile phase, because sample size is smaller (generally in 10~20ul), the conduct in the case where flow velocity is 1.0ml/min
The time of mobile phase is very of short duration, will soon be fallen by flowing phase dilution.
Influence main cause of the sample solvent to chromatographic isolation is just used from its second, i.e., sample solvent is entering
Play a part of of short duration mobile phase during sample, although this action time is very short, because the concentration of now sample is very big,
Therefore its influence to chromatographic peak profile is very huge, and the quality of peak shape further causes pole to chromatographic isolation result
Big influence, so this negative effect for eliminating or suppressing solvent is extremely important.
Why " sample solvent " can have an impact to chromatographic peak profile, to find out its cause, being that " sample solvent " conduct is of short duration
Mobile phase differs larger caused with the eluting power of the work " mobile phase " when analysis, preparation.Solves the method for this problem
It is best come sample dissolution with mobile phase, because now " sample solvent " and the chemical analysis of " mobile phase " they are identicals.Study table
Bright, for the chemical analysis of " sample solvent " closer to " mobile phase ", the eluting power of the two is also more close, is caused by sample solvent
Peak shape before prolong phenomenon and also can not possibly more occur.Therefore, the negative effect to caused by chromatographic peak profile in order to avoid " sample solvent ",
Chromatogram workers usually take dilutes the method for raw sample solution with mobile phase come sample dissolution or with mobile phase, makes " sample
Product solvent " and the composition of " mobile phase " are same or like, to have the function that to improve peak shape, and then improve post effect and separating degree.
The content of the invention
The invention aims to make up the deficiencies in the prior art, there is provided one kind can improve peak shape, improve separating degree, increase
Prolong suppressor before the peak shape of strutting effect.
In order to reach the purpose of the present invention, technical scheme is as follows：
Prolong suppressor before a kind of peak shape, it is characterised in that the device core including cutting ferrule and inside the cutting ferrule, institute
State device core and be provided with cavity for hollow structure and inside.
Further, the cavity is any one or a few in circle, ellipse, polygon.
Further, the quantity of the cavity is 1~100.
Further, the cutting ferrule includes intermediate member and the left part part and right members located at the intermediate member both sides,
The device core is fixed in the cutting ferrule by the left part part and right members by way of screw threads for fastening.
Further, the cutting ferrule is quadrangle, pentagon, hexagon, octagon or cylindrical structural.
Further, it is equipped with direction indicating structure on the device core and the cutting ferrule.
Further, the end of the device core inner is provided with sieve plate, and the sieve plate connects with the cavity, and the sieve plate
Quantity is 1~100.
The invention also discloses a kind of efficient liquid phase chromatographic analysis device, it is characterised in that has described in the above
Prolong suppressor before peak shape.
Further, in addition to high performance liquid chromatograph and the chromatographic column that is connected with the high performance liquid chromatograph and enter
Sample device, prolong suppressor before the peak shape and be connected between the chromatographic column and injector, prolong the outlet of suppressor before the peak shape
It is connected with the chromatographic column, entrance is connected with the injector.
Further：Prolong before the peak shape suppressor cutting ferrule and device core with stainless steel, polyether-ether-ketone or polytetrafluoroethylene (PTFE)
Deng for material.
The invention also discloses a kind of HPLC analytical method, it is characterised in that comprises the following steps：Mobile phase
It is temporarily stored within a cavity；The cavity is flowed through with the sample solvent of sample；The sample solvent is dilute by the mobile phase
Release.
Efficient liquid phase chromatographic analysis and first it need to be balanced each other chromatographic system, in the process, mobile phase stream with flowing when preparing
Through prolonging suppressor before peak shape and being full of the cavity of suppressor core.After sample introduction, sample solvent is mixed before sample flows through peak shape together
Prolong the cavity of suppressor, now sample solvent is diluted by the mobile phase remained in cavity immediately, and sample solvent is by mobile phase
Still sample is mixed after dilution, therefore " raw sample solvent " constitutes that " fresh sample is molten with " newly be mixed into come mobile phase "
Agent ", the chemical analysis and mobile phase of " fresh sample solvent " are closer, equivalent to substituting original in a manner of on-line dilution in principle
The first mode before sample introduction " with flowing phase dilution raw sample solution ", effectively eliminates and alleviates between mobile phase and sample solvent and wash
The larger difference of de- ability, improve peak shape so as to realize, improve post effect and improve the effect of separating degree.
The device have the advantages that：
1. prolonging before peak shape, suppressor can effectively " sample solvent and mobile phase be or not suppression on the basis of existence conditions is not changed
Prolong phenomenon before peak shape caused by matching ", some is had to spend a lot of time because the use of " sample solvent " and is improved or even
The method abandoned and smoothly applied, solve because what " sample solvent " was brought bothers, improve peak shape, add post effect,
Improve separating degree.The interference that sample solvent is brought when analysis, preparation and method are developed is greatly reduced, is greatly saved people
Power, material resources.And prolong suppressor before the peak shape and be not limited to liquid-phase chromatographic analysis field, in addition to prepared by liquid chromatogram, half prepares
Etc. application field, such as the purification of Chinese medicine the inside effective ingredient.
2. there is sieve plate at suppressor core both ends, pot strainer is may replace, effectively prevents solid particulate matter from reaching chromatographic column,
Avoid the post pressure rise because caused by blocking solid particulate matter.
3. prolonging before peak shape and direction indicating structure being equipped with suppressor and cutting ferrule, laser printing can be used on direction indicating structure
Deng direction setting direction arrow, entrance or outlet mark are indicated, allows user to prolong suppressor before frequently removing and loading onto peak shape
It is not easy to mistake use direction during use, protection chromatographic column more more effective than pot strainer, extends making for chromatographic column
Use the life-span.
Brief description of the drawings
Fig. 1 is structural representation of the present invention with the high performance liquid chromatograph for prolonging suppressor before peak shape；
Fig. 2 is to prolong the structural representation of suppressor before peak shape of the present invention；
Fig. 3 is the structural representation for prolonging suppressor device core in Fig. 2 before peak shape；
Fig. 4 is the structural representation of cutting ferrule in Fig. 1；
Fig. 5 is the structural representation that sample solvent enters before cavity；
Fig. 6 is the structural representation that sample solvent enters after cavity.
Embodiment
With reference to embodiment, the invention will be further described, but protection scope of the present invention is not limited solely to implement
Example.
It is a kind of with the efficient liquid phase chromatographic analysis device for prolonging suppressor before peak shape with reference to shown in Fig. 1, for efficient liquid phase
Chromatography, in application process, the order of connection of whole highly effective liquid phase chromatographic device is that high performance liquid chromatograph 3 pumps out
Prolong the detector of 1-chromatographic column of suppressor, 4-high performance liquid chromatograph 3 before 2-peak shape of mouth-injector.Prolong suppressor before peak shape
1 entrance for prolonging suppressor 1 between injector 2 and chromatographic column 4, before peak shape is connected with injector 2, outlet and the phase of chromatographic column 4
Even.Mobile phase flows through injector 2 under the effect of pressure that high performance liquid chromatograph provides, and mobile phase is by sample when flowing through injector 2
Product solution (mixed solution of sample solvent and sample) brings pipeline into and then prolongs suppressor 1 before entering peak shape, then by peak shape before
Chromatographic column 4 is reached after prolonging suppressor 1, then sample realizes separation in chromatographic column 4, enters back into the inspection of high performance liquid chromatograph 3
Survey device to be detected and show spectrogram on screen in the presence of software, complete whole analysis process.
Continuing with shown in Fig. 2 and Fig. 3, prolonging suppressor before a kind of peak shape, including cutting ferrule 6 and inside cutting ferrule 6
Device core 11, device core 11 is hollow structure and inside is provided with cavity 12, and cavity 12 is any one in circular, ellipse, polygon
Kind is several, naturally it is also possible to is the structure of other shapes, the quantity of cavity 12 is 1~100.Preferably, cavity 12 is
Ellipse, quantity are 3~50, and when the quantity of cavity 12 is multiple, cavity 12 is sequentially communicated.The quantity of cavity 12 can root
Depending on actual conditions, the present embodiment is 3, and multiple cavitys 12 can be same shape, or different shape.
End inside device core 11 is provided with sieve plate 10, and sieve plate 10 connects with the cavity 12.Preferably, two in device core 11
The end on side is designed with sieve plate 10, and the quantity of sieve plate 10 is 1~100, preferably 2~50.Liquid is by first sieve
After plate 10, the cavity 12 is flowed successively through, then flow out from another sieve plate 10.Sieve plate 10 may replace traditional on-line filtration
Device, effectively prevent solid particulate matter from reaching chromatographic column 4, avoid the post pressure rise because caused by blocking solid particulate matter.
Continuing with shown in Fig. 4, cutting ferrule 6 includes intermediate member 8, left part part 7 and right members 9, is by three parts groups
Into three-body type structure, naturally it is also possible to be can fixator core 11 disome formula structure.Left part part 7 and right members 9 are located at respectively
The both sides of intermediate member 8, left part part 7 are connected with intermediate member 8 with thread forms, and right members 9 and intermediate member 8 are also with screw thread shape
Formula connects.It is hollow structure inside intermediate member 8, device core 11 is placed in intermediate member 8.During assembling, first device core 11 is put into
In intermediate member 8, then device core 11 is fixed in cutting ferrule 6 by left part part 7 and right members 9 by way of screw threads for fastening, assembling
Prolong suppressor 1 before into a complete peak shape.
Left part part 7 and right members 9 are provided with aperture, will prolong suppressor 1 and chromatographic column 4 and sample introduction before peak shape by the aperture
Device 2 connects.Wherein left part part 7 is connected with injector 2, and right members 9 are connected with chromatographic column 4, it is of course also possible to replace mutually
Change, because the structure of left part part 7 and right members 9 is identical.
The outside for prolonging suppressor 1 before peak shape is provided with cutting ferrule 6, and the effect of cutting ferrule 6 is to prolong suppressor 1 before protecting peak shape.Cutting ferrule 6
Can be quadrangle, pentagon, hexagon, octagon or cylindrical structural, naturally it is also possible to be other shapes.Preferably
It is that cutting ferrule 6 is the polygonized structure no more than hexagon so that when prolonging suppressor 1 before peak shape and being placed on desktop, there is bigger connect
Contacting surface is accumulated, it is not easy to is translated into, preferably hexagonal structure.
Direction indicating structure (not illustrating) is equipped with device core 11 and cutting ferrule 6, laser printing can be used on direction indicating structure
Deng direction setting direction arrow, entrance or outlet mark are indicated, allows user to prolong suppressor 1 before frequently removing and loading onto peak shape
It is not easy to mistake use direction during use, protection chromatographic column 4 more more effective than pot strainer, extends chromatographic column 4
Service life.
Continuing with shown in Fig. 5 and Fig. 6, black triangle pattern represents mobile phase molecule, and empty quadrilateral pattern represents
Sample solvent molecule.Liquid phase analysis and first balanced each other with flowing during chromatographic system when preparing, before mobile phase flows through peak shape
Prolong suppressor 1 and the cavity 12 full of suppressor core.After sample introduction, sample solvent prolongs suppressor 1 before flowing through peak shape with sample, this
When sample solvent diluted to form " fresh sample solvent " by the mobile phase remained in cavity 12 immediately, the change of " fresh sample solvent "
Part is studied than the sample solvent before being diluted closer to mobile phase, it is original to substitute equivalent in a manner of on-line dilution in principle
Mode before sample introduction " with flowing phase dilution raw sample solution ", effectively eliminates and alleviates between mobile phase and sample solvent and elute
The larger difference of ability, improve peak shape so as to realize, improve post effect and improve the effect of separating degree.
Finally it should be noted that：Above example only not limits technology described in the invention to illustrate the present invention
Scheme, therefore, although this specification with reference to above-mentioned each embodiment to present invention has been detailed description, this
Field it is to be appreciated by one skilled in the art that still can be modified to the present invention or equivalent substitution, and all do not depart from this
The technical scheme of the spirit and scope of invention and its improvement, it all should cover in scope of the presently claimed invention.
Claims (6)
1. prolong suppressor before a kind of peak shape, it is characterised in that including cutting ferrule (6) and located at the internal device core of the cutting ferrule (6)
(11), the device core (11) is hollow structure and inside is provided with cavity (12),
The cutting ferrule (6) includes intermediate member (8) and the left part part (7) and right members located at the intermediate member (8) both sides
(9), the device core (11) is fixed on the cutting ferrule (6) by the left part part (7) and right members (9) by way of screw threads for fastening
It is interior,
The internal end of the device core (11) is provided with sieve plate (10), and the sieve plate (10) connects with the cavity (12), and described
The quantity of sieve plate (10) is 1~100.
2. prolong suppressor before peak shape according to claim 1, it is characterised in that：The cavity (12) is circular, ellipse,
Any one or a few in polygon, the quantity of the cavity (12) is 1~100.
3. prolong suppressor before peak shape according to claim 1, it is characterised in that：The cutting ferrule (6) is quadrangle, five sides
Shape, hexagon, octagon or cylindrical structural.
4. prolong suppressor before peak shape according to claim 1, it is characterised in that：The device core (11) and the cutting ferrule (6)
On be equipped with direction indicating structure.
5. a kind of efficient liquid phase chromatographic analysis device, it is characterised in that there is claim 1 to any one of claim 4 power
Profit prolongs suppressor before requiring described peak shape.
6. efficient liquid phase chromatographic analysis device according to claim 5, it is characterised in that：Also include high performance liquid chromatograph
(3) chromatographic column (4) and injector (2) and with the high performance liquid chromatograph (3) being connected, suppressor is prolonged before the peak shape
(1) it is connected between the chromatographic column (4) and injector (2), prolongs the outlet of suppressor (1) and the chromatographic column before the peak shape
(4) connect, entrance is connected with the injector (2).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510005647.8A CN104535699B (en) | 2015-01-05 | 2015-01-05 | Prolong suppressor, the efficient liquid phase chromatographic analysis device and method using it before peak shape |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510005647.8A CN104535699B (en) | 2015-01-05 | 2015-01-05 | Prolong suppressor, the efficient liquid phase chromatographic analysis device and method using it before peak shape |
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| CN104535699B true CN104535699B (en) | 2018-04-03 |
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| DE102004008755A1 (en) * | 2004-02-23 | 2005-09-08 | Hilti Ag | Static mixer and its use |
| CN101721933B (en) * | 2008-10-10 | 2012-12-19 | 华东理工大学 | Mixer using integral porous material as flow channel for liquid chromatogram and method for mixing by using same |
| CN102511647A (en) * | 2011-11-25 | 2012-06-27 | 河南天冠燃料乙醇有限公司 | Pipeline type fluid gluten crushing and homogenizing device |
| US9945820B2 (en) * | 2012-11-30 | 2018-04-17 | Agilent Technologies, Inc. | Mixer bypass sample injection for liquid chromatography |
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