CN85101444B - Method of chormatogram analysis and an apparatus therefor - Google Patents

Method of chormatogram analysis and an apparatus therefor Download PDF

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Publication number
CN85101444B
CN85101444B CN85101444A CN85101444A CN85101444B CN 85101444 B CN85101444 B CN 85101444B CN 85101444 A CN85101444 A CN 85101444A CN 85101444 A CN85101444 A CN 85101444A CN 85101444 B CN85101444 B CN 85101444B
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chromatogram
composition
filling agent
diagram
relevant
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CN85101444A (en
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内野兴一
浜野吉政
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Hitachi Ltd
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Hitachi Ltd
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Abstract

The present invention relates to a chromatogram analysis method in methods for analyzing samples by measuring the holding time of sample components. In the present invention, the method displays graphic chromatograms relative to object components to be analyzed and filling agents through the half width and the holding time of the components of the stored various objects to be analyzed relative to the various filling agents; the filling agents are sent to a separation column. The present invention also relates to a chromatogram analysis device comprising a device used for storing the holding time and the half width of the components of the objects to be analyzed relative to the filling agents and to be sent to the separation column, and a device used for preparing graphic chromatograms relative to special filling agents; the display of the graphic chromatograms can be used for fast and effectively sorting out the filling agents suitable for saccharide analysis. The analysis device can be singly used and can also be used as a subassembly of chromatographic instrument data processors.

Description

Chromatogram analysis method and device therefor thereof
The invention relates to a kind of chromatogram analysis method.More clearly say, the invention relates to this method of a kind of like this chromatogram analysis method-use, the sample that resembles sucrose and derivant thereof or the like saccharide can launch in an adding has the separating column of filling agent, thereby obtains the chromatogram of the contained various compositions of sample; Then, chromatogram is handled by analysis again.
This method that is used for red, orange, green, blue, yellow (ROGBY) of the present invention can be used separately, or uses with a liquid chromatograph or a gas chromatograph, or as one of them a inner assembly.
In normally used liquid chromatograph, sample is to be launched by eluent in being added with the separating column of filling agent, and is separated into heterogeneity.When each composition of sample passes through separating column, owing to have the caused different speed of separating out of different dissolubilities in the filling agent of various compositions in separating column, thus having caused the separation of each composition of sample, isolated composition is then sent into analyzer.In analyzer, determine the one-tenth dosis refracta that in the unit interval, arrives, and be recorded on the recording chart, thereby obtained to have a series of peak values and corresponding to the chromatogram (Jap.P. publication NO.1994/1979.) of each composition.
Be filled with a kind of fine powder in the separating column, it is by a kind of plastics that have the functional group of being replaced by metallic element, or a kind of sponge plastics constitutes.The wash-out duration of the retention time of each composition (retention time) and half-breadth or composition, change according to the variation of metallic element or pore size.
Can distinguish out composition in the sample according to the retention time of each composition, the intensity by measuring each composition chromatogram and the output quantity of analyzer can be determined the concentration of each composition in the sample.
When using this analytical approach, at first will be according to a kind of filling agent of one-tenth component selections to be separated, this selection is based on different compositions should present different retention times and half-breadth.In many cases, also to study analysis case in the past, select the filling agent that may be fit to again, and try out in new analysis.For example,, just need remove to study retention time analytical table relevant and half-breadth analytical table, and when selecting multiple filling agent or separating column, consider that the chromatogram that makes these five kinds of compositions can be not overlapping with these compositions as five kinds of compositions to be analyzed.
Yet this is a kind of analytic approach of fallibility.Its data that place one's entire reliance upon, and need complicated special technology.When can not find suitable analysis case, then must grope and wrong basis on analyze for a long time, this has just greatly reduced work efficiency.
The objective of the invention is to provide a kind of chromatogram analysis method, and this method can be selected filling agent efficiently.
Another object of the present invention is that a kind of chromatogram analysis method will be provided, and this method can be selected filling agent reliably.
Another purpose of the present invention is that a kind of chromatogram analysis method will be provided, and this method can be selected the data relevant with filling agent, and can show the diagram chromatogram.
When coming analytic sample by the different retention times of measuring the contained various compositions of sample, the present invention's chromatographic analytical approach of a kind of use of having touched upon.Retention time and half-breadth that this method is relevant with the various filling agents of being deposited according to various object under test compositions demonstrate the diagram chromatogram relevant with special filling agent with particular matter composition to be analyzed, and selected filling agent will be admitted to a separating column.
The constituent concentration time to time change that wash-out goes out.
Time when sample is fed to a kind of constituent concentration that is gone out by wash-out and reaches maximal value Hmax is called retention time (Tr) (seeing Fig. 4).
Usually, the constituent concentration that is gone out by wash-out is to move along normal distribution curve or a secondary normal distribution curve over time.When this is lighted from constituent concentration peaked 50%, through Cmax, the required time W of 50% another point that arrives Cmax again is called the half-breadth (see figure 4).The wash-out duration is generally represented by half-breadth W.
Diagram chromatogram is the chromatogram that shows on a chromatogram analysis equipment, or one with register that this analytical equipment is connected on the chromatogram that shows.Diagram chromatogram be equal to or the cathode-ray tube (CRT) that is similar to very much a data processor according to from the shown chromatogram of the analysis result of chromatographic determination device.
Diagram chromatogram can show or synthetic according to following method.That is, to the intensity of each chromatogram constantly sue for peace (Fig. 5); Intensity to each chromatogram do not sue for peace (Fig. 6); Chromatographic function is got and is made linear equation in the function program, thereby obtains a triangle chromatogram (Fig. 7).
This equipment that is used for stratographic analysis can use separately, also can be as an inner assembly of chromatographic data processor.
Among the present invention, earlier retention time and the half-breadth that object composition to be analyzed is relevant with various filling agents all stored, and selects relevant data after still to illustrate with chromatogram.Therefore, the filling agent of Shi Heing can be selected very soon.
According to content displayed, the operator can select suitable filling agent soon.The separating column that adds the filling agent that is fit to stratographic analysis has been arranged, and analysis can be carried out efficiently.
Fig. 1 is in one embodiment of the present of invention, is used for the basic comprising of the equipment of liquid-phase chromatographic analysis.
Fig. 2 is the structure of a primary clustering of the present invention.
Fig. 3 (a), 3(b), 3(c), 3(d) and 3(e) be that set of diagrams in one embodiment of the present of invention is separated chromatogram.
Fig. 4 is a chromatogram synoptic diagram having represented retention time and half-breadth.
Fig. 5,6 and 7 shows diagram chromatogram and example.
Among Fig. 1, pump 2 is sent into a separating column 3 with an eluent container 1 interior a kind of eluent that certain speed will be stored in liquid chromatograph.Sampler 4 adds a kind of testing liquid (sample) with scheduled volume.Sampler 4 is contained between pump 2 and the separating column 3, and sample and eluent are admitted to separating column 3 together, and is launched into various compositions there, enters analyzer 5 then and measures, and the data that record are handled by data processor 17.
Narration is to the analysis of the various compositions of sucrose and sucrose alcohol below.At first, the various compositions retention time relevant with various filling agents of research sucrose equally, studied the wash-out duration of each composition, in table 1 and table 2, provided the example of retention time Tr and half-breadth W.
The various separating columns of filling agent are housed, and GL-C600, CL-C613, GK-C614 and CL-C615 are the water type posts that is used to analyze, and are produced by Hitachi chemical company limited (Hifachi Chemical Co.Ltd).
Five kinds of compositions (a1), (a2), (a4) and (a5) be as representing the composition example to provide, and are described embodiment by the processing to them.In the time will analyzing five kinds of compositions of from (a1) to (a5), select filling agent or the method for the separating column of filling agent is housed, be to make the chromatogram of five kinds of compositions can be not overlapping.
Therefore among the present invention, the system that shows diagram chromatogram by computing machine is arranged, Fig. 2 has provided the example of this system.After the kind of material composition to be analyzed and filling agent was imported by keyboard 6, the half-breadth storer 7 by the half-breadth of storing filling agent and material composition to be analyzed produced the constant corresponding to half-breadth.These constants are changed the function of imaging normal distribution curves or secondary normal distribution curve again through function program 8.For example, curve 9 correspondences of generation the chromatogram of composition (a1).
Data input by keyboard 6 enters the retention time storer 10 that has each filling agent and composition retention time, so the data of the retention time of relevant material composition to be analyzed have just produced.For example, the curve 11 of generation has been indicated the position of the diagram chromatogram of the composition that will show (a1).
Chromatogram 9 and curve 11 are admitted to chromatogram storer 12, synthesize there and store.Similarly, composition (a2) to (a5) and diagram chromatogram all will deposit this storer in, for example, one group of chromatogram 13 be arranged, and after the material composition to be analyzed by the keyboard input is recorded, they will be synthetic by totalizer 14, show on cathode-ray tube (CRT) 15 then.
Like this, just can directly determine intuitively on the cathode-ray tube (CRT) 15 whether to have between the diagram chromatogram overlapped.Diagram chromatogram can also be further by register 16 records.
Totalizer 14(multiplexer) computing function is arranged, it can be with each diagram chromatogram in each moment and intensity addition.For example, when the diagram chromatogram of the diagram chromatogram of composition (a1) and composition (a3) overlaps as shown in Figure 5, then just show by the diagram chromatogram that the continuous addition of intensity is obtained.
Fig. 3 (a) is to 3(e) expression situation be that five kinds of compositions (a1) to (a5) will be analyzed with other various compositions.At Fig. 3 (a) to 3(e) in, used filling agent (A), (B), (C), (D) and (E) respectively.When having used filling agent (A), shown in Fig. 3 (a), composition (a2) and diagram chromatogram (a4) do not separate fully, and when having used filling agent (B), shown in Fig. 3 (b), composition (a1) and diagram chromatogram (a5) are overlapping.When having used filling agent (E), composition (a2) and diagram chromatogram (a3) do not separate fully.
Therefore, selected the filling agent (C) that is fit to and (D).But till being come out by wash-out to a last composition, filling agent D required time is shorter,, uses filling agent (D) than using filling agent (C) required analysis time short (3(C with the aid of pictures) and 3(d) that is).Then filling agent (D) is a kind of of the best.So best filling agent just can quickly and reliably be selected.
In addition, can also be in the chromatography data processor in the analyzer load map 1 17, and select filling agent by means of the cathode-ray tube (CRT) of data processor 17.

Claims (10)

1, claim 1. chromatogram analysis method, it comprises following several steps:
Make sample by a separating column that a kind of filling agent is housed, the movement velocity difference when passing through filling agent owing to each composition of sample has caused component separating, and separated composition is sent to an analyzer, to measure the retention time of each composition;
Store each composition retention time relevant with this filling agent;
Store each composition half-breadth relevant with this filling agent;
The diagram chromatogram that shows composition;
The method is characterized in that:
The retention time and the half-breadth of the various material compositions relevant have been stored with various filling agents;
Retention time and half-breadth according to the various material compositions relevant with various filling agents of above-mentioned storage demonstrate the diagram chromatogram relevant with the particular matter composition with special filling agent.
From above-mentioned one group of diagram chromatogram that shows, select suitable diagram chromatogram;
Determine a kind of filling agent with the above-mentioned diagram chromatogram of selecting, and this filling agent is sent into separating column remove analytic sample.
CN85101444A 1985-04-01 1985-04-01 Method of chormatogram analysis and an apparatus therefor Expired CN85101444B (en)

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CN85101444A CN85101444B (en) 1985-04-01 1985-04-01 Method of chormatogram analysis and an apparatus therefor

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CN85101444A CN85101444B (en) 1985-04-01 1985-04-01 Method of chormatogram analysis and an apparatus therefor

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CN85101444B true CN85101444B (en) 1987-01-14
CN85101444A CN85101444A (en) 1987-01-17

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107110835A (en) * 2014-11-12 2017-08-29 通用电气健康护理生物科学股份公司 Method and system for determining influence of the experiment parameter to liquid chromatogram agreement

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101932525B (en) * 2008-02-01 2013-07-31 技迩科学有限公司 Method for silica monolith cladding and separation medium

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107110835A (en) * 2014-11-12 2017-08-29 通用电气健康护理生物科学股份公司 Method and system for determining influence of the experiment parameter to liquid chromatogram agreement
CN107110835B (en) * 2014-11-12 2019-07-26 通用电气健康护理生物科学股份公司 For determining the method and system of influence of the experiment parameter to liquid chromatogram agreement

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