CN204855470U - Novel plane chromatogram sample application appearance - Google Patents
Novel plane chromatogram sample application appearance Download PDFInfo
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- CN204855470U CN204855470U CN201520556188.8U CN201520556188U CN204855470U CN 204855470 U CN204855470 U CN 204855470U CN 201520556188 U CN201520556188 U CN 201520556188U CN 204855470 U CN204855470 U CN 204855470U
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Abstract
The utility model discloses a novel plane chromatogram sample application appearance, this sample application appearance include motion control system, control temperature sample application platform, air current control system, motion control system includes horizontal moving system and perpendicular moving system. Its theory of operation does: the gas of miniature air pump or the output of external air supply is adjusted through gas flowmeter and is got into micro - nozzle, even release of solution in with micro - sample application needle of the preforming of vertical motion the time, the micro - nozzle of level motion is carrying micro - sample application needle and is being uniform motion among the motion control system, and perpendicular motion with the horizontal direction mutually supports, and the gas that goes out from micro - jet is carrying the sample solution and is spraying to the stationary phase surperficially, forms even sample strip. Thin layer plate line segment sample application not only can be realized to this sample application appearance, can also satisfy chromatographic paper sample application and punctiform sample application's requirement.
Description
Technical field
The present invention is a kind of novel planar chromatogram point sample instrument, belongs to the planar chromatograph field of analytic instrument in analytical instrument.What this instrument can be widely used in using in the industries such as chemistry, chemical industry, medicine, food, environmental protection, agricultural, forestry planar chromatograph technology to carry out qualitative and quantitative analysis and minority specioz is separated the aspects such as preparation.
Background technology
Plate chromatography is a kind of operation format of chromatographic technique, comprises thin-layered chromatography and paper chromatography, and wherein the most frequently used is thin-layered chromatography.Thin-layered chromatography Stationary liquid (as silica gel, polyamide, aluminium oxide etc.) is coated a kind of planar chromatograph technology that the carrier (as glass, aluminium foil, terylene plate etc.) of plane is separated sample, is mainly used in the Qualitive test of compound, quantitative measurement and is separated preparation.The experimentation of thin-layered chromatography mainly comprises the steps such as plate-making, point sample, saturated, expansion, colour developing, and wherein point sample is one of committed step affecting separating effect.
The point sample step of planar chromatograph has been come by craft or instrument, and the shape of initial point can be divided into spot application and ribbon point sample per sample, the manual spot application of many employings in real work.But manual shortcoming is the bad control of point sample dynamics, the bad control of sample point sample round spot size, destructible Stationary liquid surface, causes that separating effect is poor, separation capacity is less.If research shows that the sample solution of same volume adopts ribbon point sample, the separating power that greatly can improve planar chromatograph be separated capacity, improve separating effect.Such as, more in the discriminating of Chinese crude drug in thin-layer chromatography application, sample spot is ribbon by " the colored atlas of Chinese crude drug thin-layer chromatography " (2008) suggestion that Chinese Pharmacopoeia Commission publishes.But make the homogeneity of band wayward because sample solution flows out speed difference when carrying out band point sample by hand, and contact point sample also destructible Stationary liquid surface, be difficult to the band of acquisition even concentration, cause point sample repeatability poor.If use the point sample instrument of robotization, adopt noncontact spraying point sample mode, the process of point sample can be controlled by the parameter that programming is suitable, thus reduce the interference of human factor, edge clear, the uniform ribbon point sample of lines can be realized.
At present, the point sample instrument on home market is primarily of the production import of Ji Jia foreign company, and the advantage of its product is that design concept is advanced, reliable for effect.Use the external point sample instrument produced, higher to the requirement of sample solution, the sample solution for point sample requires to anticipate, otherwise special spotting needle is easily blocked, once blocking can only change spotting needle, the spotting needle that the external point sample instrument produced uses also is that its company produces specially.Due to the restriction of various factors, use the unit of import point sample instrument not extensive.Domestic also have some entity and individual to carry out the effort of various aspects to point sample instrument technology, also all delivered respective patented technology and opinion.And we feel from instrument research process the gordian technique of point sample instrument be how to be familiar with nozzle effect, be the point sample band boundaries understanding of rule and the corresponding solution taked clearly.
Because planar chromatograph technical operation is simple, applied widely, especially there is in Control of drug quality considerable status.Be necessary optimize or improve existing planar chromatograph sample application instrument structure.
Summary of the invention
The novel planar chromatogram point sample instrument of the present invention's design, organically combines the application of temperature control sample application platform, jet system, kinetic control system, micro-nozzle, this point sample instrument manufacture and design reproducible, reliability is high, simple to operate.
Another object of the present invention is to provide a kind of Step-and-repeat spotting methods, the cumulative volume of point sample is put on same band by the method several times uniformly, utilize the design of apparatus structure system to accelerate solvent volatilization simultaneously, make Stationary liquid fully absorb active principle in sample, thus ensure that sample strip edge clear, highly consistent.
Concrete technical scheme of the present invention is as follows:
Novel planar chromatogram point sample instrument, comprises kinetic control system, temperature control sample application platform, jet system, and described kinetic control system comprises tangential movement system and vertical movement system:
Described temperature control sample application platform comprises sample application platform and heating plate, heating plate is inlaid in sample application platform, heat insulation gap is left between heating plate surrounding and sample application platform, heating plate and sample application platform are arranged in parallel, heater element that is bar-shaped, banded or sheet is provided with in heating plate, can accelerate the volatilization of solvent, described sample application platform is also provided with pressure plates on L shape, on this, pressure plates to be located at outside spotted area and to be equipped with scale on both sides.
Further design of the present invention is:
Sample application platform and heating plate are also equipped with glass plate, and described upper pressure plates is located at this glass plate top.
In use procedure, the sample application platform temperature beyond heating plate, lower than 50 degree, can ensure that user is not burned.
Jet system comprises micro air pump, source of the gas switch, flowmeter, micro-nozzle and the micro-sampling pin be arranged in micro-nozzle is connected, micro-sampling cushion flow nozzle in a subtle way during point sample.
Step-and-repeat spotting methods, comprises the following steps:
The first, setting point sample platform temperature, opens heater switch, preheating sample application platform; Draw the sample solution of V volume with spotting needle, insert micro-nozzle, open micro air pump switch, or access external gas source, regulate the pressure versus flow of air-flow, complete point sample and prepare;
Second, start point sample switch, tangential movement system drives micro-nozzle by starting point along horizontal positive-displacement X, and in same time, vertical movement system drives spotting needle compressing tablet vertical depression Y displacement, and the sample solution in spotting needle is evenly released forms band on Stationary liquid;
3rd, tangential movement system drives nozzle to get back to starting point along horizontal upstream shift X, spotting needle compressing tablet stationary pause point sample in same time;
4th, tangential movement secondary system drive nozzle along level by starting point along horizontal positive-displacement X, in same time, vertical movement system drives spotting needle compressing tablet to continue vertical depression Y displacement, and sample solution is evenly released on Stationary liquid band again;
5th, tangential movement secondary system drives nozzle to get back to starting point along horizontal upstream shift X, spotting needle compressing tablet stationary pause point sample in same time;
6th, nozzle moves N time and so forth and gets back to starting point, till spotting needle completes release V volume sample solution;
7th, tangential movement system drives for the N+1 time nozzle along horizontal positive-displacement X+d, and the system of vertical movement simultaneously drive spotting needle compressing tablet vertically upward Yt=Y*N returns starting point, and wait for second time point sample, wherein d is the interval between two bands.
In above-mentioned deposition process, jet system continues to carry out gas flow purging to the band pointed out through micro-nozzle, accelerates the volatilization of solvent.
Before point sample, regulate micro-spray nozzle front end to the Distance geometry micro-sampling pin needle point of point sample plane to the distance of point sample plane with focusing straightedge.
Above-mentioned deposition process is applicable to thin-layer chromatography point sample and paper chromatography point sample.
The present invention has following beneficial effect compared to existing technology:
The present invention devises a kind of novel planar chromatogram point sample instrument, adopt monolithic processor controlled electromechanical integration technology, temperature control sample application platform, jet system, kinetic control system are organically combined, has made the novel planar chromatogram point sample instrument that point sample is reproducible, reliability is high, simple to operate.When the advantage of this instrument is point sample, required sample size is little, and sample solution is without the need to special processing, and science, specification more compared with manual point sample, the point sample used time is few, efficiency is high.
The cost of use of source of the gas has been saved in the design of micro air pump.This point sample instrument coordinates the use of focusing straightedge, and can be used for the thin layer plate of various thickness and the point sample of filter paper for chromatography, this instrument not only meets the point sample of thin layer plate, can also meet the point sample of paper chromatography; Not only can make straight-line segment point sample, round point shape point sample can also be made; Not only may be used for the planar chromatograph analysis of sample solution, the separation preparation of sample solution can also be used for.
1, less demanding to sample solution during novel planar chromatogram point sample instrument point sample of the present invention, without the need to doing special process to sample solution, facilitating operator and using.
2, the invention of this instrument is conducive to planar chromatograph sample application technology standardization, reduces the interference of human factor, makes the repeatability that ribbon point sample effect is more reliable, improve point sample.All accessories of this instrument are domestic simultaneously, reduce use cost.
3, have certain gap between heating plate surrounding and sample application platform, when heating plate is heated by heater element, this gap has thermal resistance effect, prevents heat to transmit to whole sample application platform.Simultaneously heating plate volume is little, rises to uniform temperature required time short, easy constant temperature, and heat transmits slowly towards periphery, lack, thus saves energy.
4, owing to there being certain gap between heating plate and sample application platform, whole print table surface temperature can not be made to change excessive, thus avoid defect user being caused to scald.
5, the present invention design L shape on pressure plates, by regulating the fixed screw in upper pressure plates, move in parallel the distance on its position and adjustable sample strip and thin layer plate base, adjust, operator is without the need to doing any mark on Stationary liquid surface again, and on sample application platform, the design of upper pressure plates makes user very easy to use.
6, in point sample instrument of the present invention, can mutually change between miniature air air pump and external gas cylinder, during point sample can per sample in solution the character of component adopt different gas.
7, Step-and-repeat point sample method of the present invention can the volatilization of accelerated solvent to obtain narrow as far as possible sample strip, the cumulative volume of this Step-and-repeat point sample point sample is put on same band several times uniformly, again by several householder method accelerated solvent volatilization, make Stationary liquid fully absorb component in sample, thus ensure that sample strip edge clear, highly consistent.
Accompanying drawing explanation
Accompanying drawing 1 novel planar chromatogram point sample instrument schematic appearance.
In Fig. 1, the title of each several part is respectively: 1 gas meter, 2 compressing tablets, the position of 3 micro-sampling pins, 4 micro-nozzles, 5 heating plates, 6 sample application platforms, 7 program self-test switch, 8 manual/auto control switches, 9 start buttons, 10 heater switch, 11 air pump switches, 12 horizontal direction Zheng Xiang the reverse switch of ╱, 13 temperature controllers, 14 tangential movement controllers, 15 vertical movement controllers, pressure plates on 16,17 complete machine power switches (being positioned on the right side of instrument), 18 source of the gas switches (being positioned on instrument rear panel).
Accompanying drawing 2 sample application platform temperature control system compositional block diagram.
The structural representation of accompanying drawing 3 temperature control sample application platform.
In Fig. 3, the title of each several part is respectively: 19 back up pads move horizontally hole, the heat insulation gap between 20 heating plates and sample application platform, 21 heating rods, 5 heating plates, 6 sample application platforms, pressure plates on 16.
On accompanying drawing 4, pressure plates and temperature measuring point are at the relative position relation figure of sample application platform.
In Fig. 4, the title of each several part is respectively: pressure plates on 16,5 heating plates, the gap between 20 heating plates and sample application platform, 22a-i) nine temperature measuring points.
The temperature test curve of accompanying drawing 5 sample application platform diverse location.
Pressure plates design drawing on accompanying drawing 6.In figure, the title of each several part is respectively: 23 adjustable screws, 24 graduated scales.
Accompanying drawing 7 jet system compositional block diagram.
The cushion of accompanying drawing 8 micro-sampling in a subtle way flow nozzle guiding choke tube diagrammatic cross-section.
In Fig. 8, each ingredient is respectively: 25 micro-sampling pin needle tubings, 26 micro-sampling pin needle tubing entrances, 27 housings, 28 draft tube, 29 air collecting chambers, 30 guiding choke tubes, 31 guiding choke chambeies, 32 line chambeies.
Accompanying drawing 9 kinetic control system compositional block diagram.
Accompanying drawing 10 is focused straightedge schematic diagram.
Specific embodiment
Embodiment one:
The novel planar chromatogram point sample instrument of the present invention's design uses monolithic processor controlled electromechanical integration technology, the application of temperature control sample application platform, jet system, kinetic control system, micro-nozzle and focusing straightedge is organically combined, manufacture and design the novel planar chromatogram point sample instrument reproducible, reliability is high, simple to operate, the appearance design of complete machine as shown in Figure 1.The principle of work of this instrument is: control to keep spotted area constant temperature on sample application platform by temperature, uses the gas of micro air pump or the external gas source output carried, regulates, enter micro-nozzle through gas meter.While sample solution in micro-sampling pin is released by the compressing tablet of vertical movement in kinetic control system uniformly, the micro-nozzle of tangential movement carries micro-sampling pin and does constant level's motion, and vertical movement and tangential movement also exist temporal cooperation, the gas that now micro-nozzle ejects carry sample solution be injected into need point sample Stationary liquid on the surface, form uniform sample strip.
Novel planar chromatogram point sample instrument adopts the principle of " Step-and-repeat point sample " to complete ribbon point sample, is about to need the cumulative volume of the sample solution of point sample to repeat several times.The theoretical foundation of design " Step-and-repeat point sample " method is: the suggestion of publishing " the colored atlas of Chinese crude drug thin-layer chromatography " (2008) by Chinese Pharmacopoeia Commission, when using silica gel plate to carry out thin-layer chromatographic analysis, according to ribbon point sample, wide for 8-10mm (common plate) or 5-8mm (efficient plate), be highly no more than 1mm and be advisable.The ordinary silicon offset plate point sample being 0.2mm for Stationary liquid thickness, when bar bandwidth 10mm, high 1mm, volume shared by Stationary liquid is 10 × 1 × 0.2=2mm
3=2 μ l, if point sample volume is 10 μ l, even if ignore stationary phase volume, the volume of sample solution is also 5 times of volume shared by Stationary liquid.If disposable by the sample solution point of 10 μ l in 2mm
3stationary liquid on and absorbed in the short time, solvent has little time the diffusion that volatilization can cause sample solution, makes the height of sample strip be greater than 1mm.Even if the volume 4 μ l of a point sample, its volume ratio is still 2 times, and sample solution also can be made to spread, and we also demonstrate this conclusion on novel planar chromatogram point sample instrument.For solving the problem of sample strip diffusion, the principle that we clearly propose " Step-and-repeat point sample ", the cumulative volume of point sample is put on same band several times uniformly, again by several householder method accelerated solvent volatilization, make Stationary liquid fully absorb component in sample, thus ensure that sample strip edge clear, highly consistent.
Novel planar chromatogram point sample instrument is on the basis of " Step-and-repeat point sample " principle, one by one solve the factor relevant with the effect of band point sample, as speed, the evaporation rate etc. of solvent on thin layer plate of the flow of gas, micro-nozzle level movement, jointly realized the object of accelerated solvent volatilization by the function playing instrument various piece.
By the point sample instrument function that each several part realizes in deposition process, instrument is mainly divided into three ingredients: 1 temperature control sample application platform; 2 jet systems; 3 kinetic control systems, kinetic control system is arranged on the cabinet of point sample instrument by sample application platform, comprises tangential movement system and vertical movement system.
Sample application platform is fixedly connected with cabinet, and tangential movement system is connected to below sample application platform by fixed support plate, and vertical movement system is connected by transmission shaft with tangential movement system.The micro-nozzle of jet system is arranged in vertical movement system, and the compressing tablet of micro-sampling pin is connected with vertical movement system, is released by the sample solution in spotting needle by vertical movement system.
Temperature control sample application platform comprises sample application platform and heating plate, heating plate upper surface is concordant with sample application platform, heating plate is inlaid in sample application platform, heat insulation gap is left between heating plate surrounding and sample application platform, heating plate is concordant with sample application platform upper surface, heater element that is bar-shaped, banded or sheet is provided with in heating plate, heater element spotting needle movement locus arranged beneath, heater element is arranged in below spotting needle movement locus, described sample application platform is also provided with pressure plates on L shape, and on this, pressure plates to be located at outside spotted area and to be provided with scale on both sides.
The principle of work of each several part is described below:
1, temperature control sample application platform:
The object controlling point sample platform temperature is that the volatilization of accelerated solvent is to obtain sample strip narrow as far as possible.
As shown in Figure 3, micro-nozzle level movement locus is parallel to immediately below heater element, micro-nozzle inner at heating plate in temperature control sample application platform.Have certain gap between heating plate surrounding and sample application platform, its relative position is shown in Fig. 4.When heating plate is heated by heater element, this gap has thermal resistance effect, prevents heat to transmit to whole sample application platform.Its advantage is: heating plate volume is little, rises to uniform temperature required time short, easy constant temperature, and heat transmits slowly towards periphery, few, thus save energy.Gap design between heating plate and sample application platform is one of invention of novel planar chromatogram point sample instrument.
Owing to there being certain gap between heating plate and sample application platform, whole print table surface temperature can not being made to change excessive, thus avoid defect user being caused to scald.We have chosen a-i nine temperature measuring points on sample application platform, and as shown in Figure 5, the temperature of display heating plate is significantly higher than other parts of sample application platform to the temperature test curve of each position.
In addition, on heating plate and sample application platform, spread the thick glass of one piece of 2mm, namely beautified the outward appearance of instrument, also can prevent in use having tiny object to fall in heat insulation gap (Fig. 4).Above the glass that 2mm is thick, installed the upper pressure plates of one piece of L shape, see Fig. 6, be used on the one hand pushing down glass and move to prevent glass sliding, on L shape, pressure plates both sides all indicate size scale on the other hand, handled easily person can determine the position of thin layer plate.Scale convenient operation person pressure plates is parallel to L shape on micro-nozzle level movement locus one side observes the width of band, and scale is in addition for determining the distance on band and thin layer plate base.The suggestion of " the colored atlas of Chinese crude drug thin-layer chromatography " (2008) of publishing by Chinese Pharmacopoeia Commission, when using silica gel plate to carry out thin-layer chromatographic analysis, requires sample baseline distance base 10-15mm.Experimentally requirement, by regulating the fixed screw on L shape in pressure plates, move in parallel the distance on its position and adjustable sample strip and thin layer plate base, moving range is 0-5mm, and namely band is minimum apart from base is 10mm, be 15mm to the maximum.Once adjust, operator is without the need to doing any mark on Stationary liquid surface again.On sample application platform, the design of upper pressure plates makes user very easy to use.
2, jet system
Jet system comprises miniature air air pump, switch, gas meter and micro-nozzle between micro air pump and external gas source, and the design of jet system as shown in Figure 7.
The gas exported by micro air pump or external gas source, by the laggard flow nozzle in a subtle way of gas meter adjust flux, sprays through micro-spray nozzle front end.Novel planar chromatogram point sample instrument devises the function carrying and can mutually change between miniature air air pump and external gas cylinder.When carrying out point sample can per sample in solution the character of component adopt different gas, as the sample solution containing oxidizable component can adopt external nitrogen, the sample not containing oxidizable component can adopt air.When gas is by gas circuit, adopt gas meter adjust flux, can observe easily with the size of adjusting gas flow and air-flow the impact of point sample effect.Micro air pump and gas meter regulate the function of air-flow to be one of innovative point of novel planar chromatogram point sample instrument.
Trace nozzle is the core component of novel planar chromatogram point sample instrument, its effect be by sample solution in a non-contact manner evenly, continuous print is sprayed on Stationary liquid surface.Trace nozzle design and produce and use the particular/special requirement needing to meet novel planar chromatogram point sample instrument, as micro-nozzle and Stationary liquid surface distance can regulate, micro-nozzle can change, and the clearance fit between micro-nozzle and micro-sampling pin needle tubing can make micro-sampling pin can insert and extract micro-nozzle easily.Gas-circulating should be ensured in deposition process around micro-sampling pin needle tubing from nozzle ejection, ensure again to be less than at the quantity of gas leakage of micro-sampling pin inflow point the flow that gas sprays at spray nozzle front end out and away.Therefore the micro-nozzle meeting above-mentioned requirements is a special applications of micro-nozzle for novel planar chromatogram point sample instrument, it designs and produces and fully can ensure that novel planar chromatogram point sample instrument accurately, reliably can carry out point sample, obtain the uniform sample strip meeting pharmacopoeial requirements, Fig. 8 is shown in by the micro-nozzle schematic diagram being inserted with micro-sampling pin.Patent of invention has been applied in the design of trace nozzle, and number of patent application or the patent No. are 201410131382.1, has entered now announcement and Substantive Examination Stage.
3, kinetic control system
Kinetic control system is made up of tangential movement system and vertical movement system, sees Fig. 9.Under Single Chip Microcomputer (SCM) program controls, tangential movement system can realize stepper motor drive micro-nozzle carry out forward, reverse, stop three kinds of motion states, vertical movement system can realize that stepper motor drives compressing tablet to carry out pressing down, suspends, rising returns initial initial point three kinds of motion states.The stepper motor of vertical movement in kinetic control system during point sample drives compressing tablet, sample solution in micro-sampling pin is released uniformly, the stepper motor of tangential movement drives micro-nozzle to do horizontal direction uniform motion together with micro-sampling pin, and vertical direction and horizontal motion also exist temporal cooperation, meanwhile, namely the gas sprayed from micro-nozzle carry sample solution and be injected into Stationary liquid on the surface, forms uniform sample strip.
Usually in planar chromatograph sample application, require that the height of sample strip is not more than 1mm, and when using instrument point sample, the height of band is relevant with factors such as the evaporation rate of solvent in sample solution, each point sample amounts.If solvent has little time volatilization during point sample, too much solvent can spread on Stationary liquid, makes point sample band thicker, affects point sample effect.If point sample amount is excessive, as 5 μ l sample solutions point sample completes, band also can be made thicker.Therefore novel planar chromatogram point sample instrument is for the problems referred to above, and take the volatilization of following method accelerated solvent when designing and producing: 1, adopt temperature control sample application platform, the temperature improving platform makes the solvent a little on Stationary liquid in sample solution volatilize as soon as possible; When 2, utilizing nozzle point sample to terminate return to origin, the purging of air-flow accelerates solvent volatilization; 3 optimum configurations utilizing Single Chip Microcomputer (SCM) program, adopt " Step-and-repeat point sample " principle, the point repeated several times by a certain amount of sample solution is on same band, and this mode of operation is one of invention of this instrument.
The optimum configurations of Single Chip Microcomputer (SCM) program is utilized to complete the design concept of " Step-and-repeat point sample " as follows: arranged positive-displacement amount Xmm, the upstream shift amount Xmm of tangential movement by tangential movement programming controller (accompanying drawing 9), come and gone the positive-displacement amount X+dmm of times N, last motion, wherein d is the distance (i.e. band interval) of point sample strap end to next band starting point.Tangential movement displacement X and micro-nozzle carry the distance of micro-sampling pin movement in the horizontal direction, i.e. the width of band.As selected the displacement of X=8mm, then the width of band is 8mm.If select the displacement of X=0mm, then the width of band is 0mm, is now spot application.
If by the sample solution of V μ l, repeat a little on same sample band by N point sample, then each vertical depression micro-sampling pin can release the sample solution of V/N μ l equably, N time repeatedly, just the sample solution of V μ l all can be sprayed on Stationary liquid.Now the volume of V μ l can be converted to the distance Y of micro-sampling pin pushrod movement
tmm, then each compressing tablet promotes push rod descending displacement amount is Y
tmm/N=Ymm, namely the descending moving displacement amount Ymm once of compressing tablet i.e. micro-sampling pin once discharge the sample solution of V/N μ l.Namely each descending displacement amount Ymm of compressing tablet in vertical direction, moving pause time t are set by vertical movement programming controller (accompanying drawing 9) according to above data, press down times N, the displacement Y of suspending count N-1, the up correcting action of compressing tablet
t=Y × Nmm.
After completion system is arranged, draw the sample solution of V μ l with micro-sampling pin, insert micro-nozzle, start-up operation button, micro-nozzle carries micro-sampling pin and compressing tablet moves under the drive of two stepper motors simultaneously respectively.While the micro-sampling pin that carry insertion when micro-nozzle leaves initial point in the horizontal direction, compressing tablet also leaves initial point.When the micro-sampling pin that micro-nozzle carries insertion completes Xmm displacement in the horizontal direction, in same time, compressing tablet also completes displacement micro-sampling pin push rod being pressed down Ymm vertically downward.Complete this action respectively in same time after, the micro-sampling pin that trace nozzle carries insertion performs the reverse program returning initial initial point, the displacement returned is Xmm, meanwhile compressing tablet performs time out program, after waiting for that micro-sampling pin that micro-nozzle carries insertion returns initial point, more again move together.
Kinetic control system controls this two subsystem repeating motions like this, until the micro-sampling pin that micro-nozzle carries insertion completes the horizontal displacement of positive movement X+dmm, what second sample solution waited for by the micro-sampling pin that micro-nozzle carries insertion in the position of X+dmm restarts point sample.D represents that the starting point of second sample solution band and the end of first point sample band completed have the distance of dmm, is namely the interval of dmm between two bands.The micro-sampling pin that carry insertion at micro-nozzle completes in the process of the horizontal displacement of positive movement X+dmm, and compressing tablet performs Y
tthe up motion returning initial initial point of=Y × Nmm, gets back to the initial initial point of compressing tablet.Now namely complete the deposition process of a sample solution, take off micro-sampling pin, after cleaning, suck sample solution, carry out second time point sample.
The principle that said process is " Step-and-repeat point sample " and parameter selection method thereof, it should be noted that, compressing tablet performs the stand-by period t suspended each time, that is the micro-nozzle micro-sampling pin that carries insertion does reverse movement and starts to before the initial initial point of arrival, this t does not have sample solution to be injected in Stationary liquid plane in second, this time period is become by the design of novel planar chromatogram point sample instrument the stand-by period allowing solvent fully volatilize, and this is one of invention of novel planar chromatogram point sample instrument.Meanwhile, micro-nozzle is in the process of return to origin in the horizontal direction, utilizes the stand-by period not having sample solution to spray, lasting gas flow purging energy accelerated solvent volatilization.This is also one of invention of novel planar chromatogram point sample instrument design.Even if adopt the method spot application, also can be arranged by program parameter, allow the motion of compressing tablet in vertical direction divide a few step to complete, allowing the solvent be ejected on Stationary liquid fully volatilize by extending the stand-by period, making sample point enough little.
In sum, temperature control sample application platform, jet system, kinetic control system three part are organically merged, point sample work can be completed under Single-chip Controlling.This instrument can accelerate the volatilization of solvent in sample solution by the function playing above-mentioned three parts simultaneously, that is: 1 temperature improving heating plate on sample application platform; The time out of the compressing tablet of 2 prolongation vertical movements; The 3 purging functions making full use of jet-stream wind in time out.
But, find during actual point sample that the height of sample strip also depends on that micro-spray nozzle front end is to the Distance geometry micro-sampling pin needle point of point sample plane to the distance of point sample plane.Therefore, experimental data arranged by a large amount of experiments, sum up, specially for novel planar chromatogram point sample instrument invented one highly fixing for regulating the template with specification distance, be named as focusing straightedge, see accompanying drawing 10.As parts of novel planar chromatogram point sample instrument, focusing straightedge has applied for patent of invention, and this patent enters Substantive Examination Stage at present, and number of patent application is 201410257784.6.Use focusing straightedge can control micro-spray nozzle front end accurately to the Distance geometry micro-sampling pin needle point of point sample plane to the distance of point sample plane.Due to the application of straightedge of focusing, not only simplify the design of instrument, facilitate operator and use instrument, and the point sample making novel planar chromatogram point sample instrument can be used in the Stationary liquid plane of other any thickness, comprise the thin layer plate of different-thickness and the point sample of filter paper for chromatography.Which solves the repeated bad problem of point sample because Stationary liquid difference in thickness causes, therefore called after novel planar chromatogram point sample instrument of the present invention.
Application example:
By above design, temperature control sample application platform, jet system, kinetic control system are organically integrated together, namely become a complete novel planar chromatogram point sample instrument.The suggestion of " Chinese crude drug thin-layer chromatography colored atlas " (2008) of publishing by Chinese Pharmacopoeia Commission, when using silica gel prefabricated board to carry out thin-layer chromatographic analysis, sample baseline distance base 10-15mm, the distance between sample initial point is 5,8,10mm; If ribbon point sample, wide is 8-10mm, is highly no more than 1mm.The present embodiment, for thin-layer chromatography point sample 4 μ l, illustrates the using method of novel planar chromatogram point sample instrument.
This instrument utilizes the upper direct Quality control baseline distance base 10mm of pressure plates.Tangential movement optimum configurations is sample strip width X=8mm, band interval d=5mm.When point sample amount is 4 μ l, its push rod displacement of micro-sampling pin using 5 μ μ l is 40mm, then push rod often moves the solution that 10mm at the uniform velocity releases is 1 μ l, has therefore repeated the point sample work of a sample by four times.According to above data, tangential movement is become the pulse number of Driving Stepping Motor with the distance transform of vertical movement.Open point sample instrument power switch, horizontal and vertical motion controller arranges pulse number and the impulse speed of two stepper motors respectively, as long as it is equal apart from the required time to ensure to move horizontally 8mm Distance geometry vertical movement 10mm.Above-mentioned parameter is repeated on programming controller arrange 4 times.Move horizontally distance for the last time for 8mm+5mm=13mm, and starting point got back to by the compressing tablet of vertical movement.
Kinematic parameter is set by said process, can point sample according to the following steps:
1, set point sample platform temperature, open heater switch, preheating 30 minutes.
2, the height of micro-nozzle to thin layer plate is fixed with focusing straightedge, get the micro-sampling cushion flow nozzle in a subtle way of non-draw solution, the height of micro-sampling pin needle point to thin layer plate is fixed again, if undesirable replaceable micro-sampling pin or finely tune the position of micro-nozzle with focusing straightedge.
3, with selected micro-sampling pin pipette samples solution, after adjustment scale, micro-nozzle is inserted into, position (apart from base 10-15mm) suitable on adjustment nozzle to thin layer plate.
4, booster air pump, regulates suitable airshed (2-5L/min).
5, point sample is started by trigger button.
6, point sample takes off micro-sampling pin after terminating, and cleaning, prepares the point sample of next sample.
Carry out point sample by said process, can obtain width is 8mm, is spaced apart the sample strip of 5mm.
Claims (3)
1. novel planar chromatogram point sample instrument, comprises kinetic control system, temperature control sample application platform, jet system, and described kinetic control system comprises tangential movement system and vertical movement system, it is characterized in that:
Described temperature control sample application platform comprises sample application platform and heating plate, heating plate is inlaid in sample application platform, heat insulation gap is left between heating plate surrounding and sample application platform, heating plate and sample application platform are arranged in parallel, heater element that is bar-shaped, banded or sheet is provided with in heating plate, described sample application platform is also provided with pressure plates on L shape, and on this, pressure plates to be located at outside spotted area and to be equipped with scale on both sides.
2. planar chromatograph sample application instrument according to claim 1, it is characterized in that: sample application platform and heating plate are also equipped with glass plate, described upper pressure plates is located at this glass plate top.
3. planar chromatograph sample application instrument according to claim 1 or 2, it is characterized in that: the micro-sampling pin that jet system comprises micro air pump, source of the gas switch, flowmeter, micro-nozzle and is arranged in micro-nozzle, micro-sampling cushion flow nozzle in a subtle way during point sample.
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| CN201520556188.8U CN204855470U (en) | 2015-07-28 | 2015-07-28 | Novel plane chromatogram sample application appearance |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104965047A (en) * | 2014-10-13 | 2015-10-07 | 中国药科大学 | Novel planar chromatography sample application instrument and step repeated sample application method |
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2015
- 2015-07-28 CN CN201520556188.8U patent/CN204855470U/en not_active Withdrawn - After Issue
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104965047A (en) * | 2014-10-13 | 2015-10-07 | 中国药科大学 | Novel planar chromatography sample application instrument and step repeated sample application method |
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