CN203164043U - Sample preparation instrument - Google Patents
Sample preparation instrument Download PDFInfo
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- CN203164043U CN203164043U CN 201320072541 CN201320072541U CN203164043U CN 203164043 U CN203164043 U CN 203164043U CN 201320072541 CN201320072541 CN 201320072541 CN 201320072541 U CN201320072541 U CN 201320072541U CN 203164043 U CN203164043 U CN 203164043U
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Abstract
The utility model discloses a sample preparation instrument. The sample preparation instrument comprises an outer housing, wherein the inner top of the outer housing is provided with a nitrogen blowing groove, and a nitrogen blowing plate device is arranged at the lower part of the nitrogen blowing groove; slideways are respectively arranged on both sides and at the middle positions of the nitrogen blowing plate device, a nitrogen blowing plate sliding along the slideway is arranged on the nitrogen blowing plate device, the slideway is provided with a clamping groove, and the nitrogen blowing plate is fixed by the clamping groove; the inner bottom of the outer housing is provided with a first fixed groove for placing a sample liquid receiving plate, the first fixed groove is provided with a middle seal ring and a second fixed groove in sequence, and the second fixed groove is provided with a sample preparation plate and an SPE (Solid Phase Extraction) bracket; the lower part of the first fixed groove is provided with a lever, an oscillator and a negative pressure pump; the measuring side surface of the first fixed groove is provided with two small holes connected with two fans and a gas heating device positioned at the back of the first fixed groove; and a waste liquid flowing outlet, a nitrogen outer joint, a negative pressure joint, a power supply joint and a nitrogen heating device are arranged at the back surface of the outer housing.
Description
Technical field
The utility model relates to chemical analysis and Pharmaceutical Analysis field, relates in particular to a kind of specimen preparation instrument.
Background technology
In analytical chemistry and Pharmaceutical Analysis process, sample pre-treatments is the key link of analyzing and testing result precision height, is to concentrate determined trace components, improves detection sensitivity and removes the important means that analytic system is had interfering material.The step of sample pretreatment has very big influence to credibility, analysis cost and the experimenter's of the high flux of sample detection, data satisfaction.Fast development along with the sample detection technology, for example: LC-MS(Liquid Chromatography-Mass Spectrum, liquid chromatography and mass spectrometry) technology, GC-MS(Gas Chromatography-Mass Spectrum, gas chromatography and mass spectrometry) technology and CE-MS(Capillary Electrophoresis-Mass Spectrum, Capillary Electrophoresis and mass spectrometry) technology, also strengthened day by day for the demand of the fast high-flux of sample pre-treatments technology.Therefore, for detection method of exploitation of success, select and optimize a suitable sample-pretreating method to be very important.The trend of sample pre-treatments technical development at present be quick, required sample size little, in batches big, automaticity is high, cost is low, labour intensity is low, reagent consumption less, environmental pollution is little and the method pseudo-selectivity is high.Therefore, explore sample-pretreating method quick, efficient, easy and easy robotization and become one of important research direction of current analytical chemistry.
SPE(Solid Phase Extraction, Solid-Phase Extraction) be a kind of novel sample pretreatment technology, by the development that combines of liquid-solid extraction and column liquid chromatographic technology, the history of existing two more than ten years.SPE compares with traditional liquid-liquid extraction has multinomial graceful function, for example: extraction column is disposable throw-away-type, the problem of no cross pollution, no emulsification phenomenon, sample extraction recovery height, discarded object is easily removed from the laboratory, do not need to use ultrapure solvent, the consumption of organic solvent is few, environmental pollution is little, little to the human injury, required volume of sample is few, processing speed is fast, operate under the room temperature, being particularly suited for handling volatility reaches the thermally labile medicine, there is not the operation that is separated, easy collection analysis thing component, simple to operate, save time, laborsaving and be easy to advantage such as robotization, the annual growth with 10% enlarges its application always since SPE occurs.
SLE(Supported Liquid-liquid Extraction, the medium liquid-liquid extraction) based on traditional liquid-liquid extraction principle, in conjunction with the form of solid-phase extraction column, utilize a kind of adsorbability height, inertia, porous aggregate that specific surface area is big to be medium, carry out sample pre-treatments.Detachment process is: (different with Solid-Phase Extraction is to pillar with sample on the water-soluble sample solution, all sample solutions all are retained, n.s. liquid flows out), water-soluble sample liquid is coated on inertia porous aggregate surface rapidly and forms the sample thin film layer, using with the immiscible organic solvent of water then is eluent, target compound is extracted, collect extract and obtain target compound solution.This method has effectively solved difficult problems such as the complex operation that exists in traditional liquid-liquid extraction process, time-consuming and easy emulsification, reduced the loss of sample simultaneously, effectively improve the recovery of extraction of sample, and can be combined with 96 orifice plates or 384 orifice plates, realized the high flux sample pre-treatments.
PPT(Protein Precipitation Technology, fast protein precipitation) technology is a kind of principle based on organic solvent deposit protein, combines the form of modern solid-phase extraction column and membrane technology development commonly used now.Wherein Solid-Phase Extraction is a support of whole technique, and core is film.Employed film is a kind of special film in the experiment, this film does not allow organic solvent or water to pass through at normal temperatures and pressures, under the situation of negative pressure or malleation existence, liquid can pass film and flow out, and oarse-grained material as the denatured protein aggregation, can be retained in the film upside, thereby realize the protein of post precipitation and separating of supernatant, reach biological sample except the purpose of deproteinize.In addition, this technology can be combined with 96 orifice plates or 384 orifice plates, is applied on the robotization solid-phase extracting instrument, thereby realizes high flux and robotization.
Filtering technique (Filtration) is a kind of a kind of new quick filtering technique that grows up based on the single filter filtering technique of tradition fast.Fast filtering technique adopts the form of 96 orifice plates or 384 orifice plates, has realized the high flux pre-treatment of sample, simultaneously, has kept the form of single solid-phase extraction column again, make the selectivity of experimenter in process of the test more, have more dirigibility.Compare with traditional single filter filter type, fast filtering technique had both kept the advantage of single filter, had overcome some defectives in the single filter filtering technique again, for example: complex operation, consuming time, can't realize robotization and high flux etc.So the application of novel quick filtering technique in sample pretreatment process also more and more widely.
DPE(Dynamic Packing Extraction, dynamically Solid-Phase Extraction) technology is based on solid phase extraction techniques, prepares the new technology that theory grows up in conjunction with quick sample.Dynamically the core of solid phase extraction techniques is, filler is in bulk in the Tip head or in the little solid-phase extraction column, fix with baffle plate up and down, and a space is arranged between baffle plate and the filler, this space makes filler in bulk in solid-phase extraction column or in the Tip head, and filler can be movable within the specific limits.Sample pretreatment process is, the Tip head is connected on the pipettor or the solid phase post that comes together is connected with piston, by drawing repeatedly and getting sample liquid, make testing sample or target compound by filling adsorption, if the compound that is adsorbed on the filler is impurity, then need not next step processing, if target compound is adsorbed on the impurity, then need to utilize a kind of suitable eluant, eluent, target compound is eluted, thereby reach the purpose of removing impurity or obtaining target compound.Because filler can move within the specific limits, so in extraction process, the time that sample liquid contacts with filler is compared with common Solid-Phase Extraction process with number of times have been increased a lot, therefore, the efficient that the common Solid-Phase Extraction of speed ratio that dynamic Solid-Phase Extraction reaches extraction equilibrium reaches extraction equilibrium is high a lot, so this method has shortened time for sample pretreatment greatly.Generally speaking, DPE has namely inherited the advantage of traditional Solid-Phase Extraction, has shortened the time of sample pre-treatments simultaneously again, has improved the efficient of sample pre-treatments, has realized new breakthrough on the basis of traditional Solid-Phase Extraction, is with a wide range of applications.
The method of SPE, SLE, PPT, Filtration and five kinds of sample pretreatments of DPE is that method the most frequently used in the sample pretreatment also is state-of-the art sample pretreating method.
Utility model people finds to exist at least in the prior art following shortcoming and defect in realizing process of the present utility model:
At present, in most of assay laboratory, these five kinds of sample pretreatment technology have application, and major part all is the medical grade polypropylene injection tube form of single tube, need manual operation.And for manual operation, have the following disadvantages: personnel interfere the too many poor repeatability of easily introducing error, sample, can't realize that employed organic reagent is also bigger to the injury of human body in robotization and high flux and the specimen preparation process.At present, 96 orifice plates or 384 orifice plate sample pretreatment technology, frequency of utilization is also fewer in the assay laboratory of China or scientific research institution, and main cause is not have supporting high flux specimen preparation instrument mutually; Even high-throughout specimen preparation instrument is arranged, a plurality of instruments such as needed Nitrogen evaporator and shaker in the subsequent step so, not only expensive but also shared spatial volume is bigger, is unfavorable for actual application.
The utility model content
The utility model provides a kind of specimen preparation instrument, the utility model realized semi-automatic so that automatically high flux carry out the experiment of various sample pre-treatments, avoided the introducing of error, improved the recovery of sample, guaranteed the repeatability of sample preparation, simultaneously, also kept and implemented traditional single tube Solid-Phase Extraction and liquid-liquid extraction isotype, seen for details hereinafter and describe:
A kind of specimen preparation instrument comprises: shell, and described shell inner top is provided with nitrogen and blows groove, is provided with nitrogen in the bottom that described nitrogen blows groove and blows panel assembly; Both sides and centre position that described nitrogen blows panel assembly also are respectively arranged with slideway, blow panel assembly at described nitrogen and the nitrogen that slides along described slideway is set blows plate, and described slideway is provided with draw-in groove, and the fixing described nitrogen of described draw-in groove blows plate; Described shell inner bottom part is provided with for first pickup groove of placing the sample liquid dash receiver, is disposed with intermediate seal circle and second pickup groove on described first pickup groove, and described second pickup groove is provided with specimen preparation plate and Solid-Phase Extraction column holder; Be provided with waste liquid flow export, nitrogen external tapping, negative pressure interface, power interface and nitrogen heating arrangement at the described shell back side, there is two electric fans of device and the gas-heating apparatus that recyclegas is provided at the described first pickup groove back; Described two electric fans provide hydronic gas by two electric fan holes and the side vent port that is positioned on the first pickup groove sidewall for first pickup groove; Be provided with oscillator, lever and negative pressure pump in described first pickup groove bottom.
Described nitrogen blows groove and comprises: variable valve, described nitrogen blow panel assembly and are arranged on described nitrogen by described variable valve and blow on the groove.
The model that described nitrogen blows plate is specially: 96 holes, 24 holes, 12 holes or 9 holes; Described nitrogen blows the model of plate and the model of described Solid-Phase Extraction column holder is complementary.
Described nitrogen heating arrangement is made up of the heating cylinder body of two series connection.
Also be provided with the nitrogen flow table in the described shell, linked to each other with extraneous source nitrogen by described nitrogen external tapping by nitrogen conduit; Also be provided with negative pressure dynamics indicator gauge on the described shell, show vacuum magnitude;
The back side of described shell also is provided with fan.
The bottom of described first pickup groove also is provided with aperture, realizes the bottom negative pressure by described aperture and negative pressure pump; The side of described first pickup groove also is provided with three apertures, wherein electric fan hole and electric fan directly communicate, side vent port, electric fan hole, electric fan and solid-phase extraction device be common to form an airtight box, thereby dries up the heated air that process provides circulation for Solid-Phase Extraction.
Also be provided with oscillation device below described first pickup groove and described second pickup groove, described oscillation device comprises: lever and oscillator,
Described first pickup groove is connected described oscillator with described second pickup groove by described lever.
Described specimen preparation instrument also comprises: display control panel,
By the regulation and control of described display control panel realization to liquid feeding, positive negative pressure conversion, time-delay, nitrogen blowing temp.
Described nitrogen blows the rifle head assembly that plate is specially 96 holes.
The model of described Solid-Phase Extraction column holder is specially: 1mL, 3mL, 6mL or 10mL;
When the model of described Solid-Phase Extraction column holder was 1mL, 1mL Solid-Phase Extraction column jecket was arranged by 3 * 8 and is placed; When the model of described Solid-Phase Extraction column holder was 3mL, 3mL Solid-Phase Extraction column jecket was arranged by 4 * 6 and is placed; When the model of described Solid-Phase Extraction column holder was 6mL, 6mL Solid-Phase Extraction column jecket was arranged by 3 * 4 and is placed; When the model of described Solid-Phase Extraction column holder was 10mL, 10mL Solid-Phase Extraction column jecket was arranged by 3 * 3 and is placed.
The beneficial effect of the technical scheme that the utility model provides is: the utility model can be simultaneously with high flux nitrogen blowing apparatus, rocking equipment with move subsidiary function in the specimen preparations such as liquid and the core technology of specimen preparation has organically been joined together, be integrated on same the instrument; In addition, this instrument can also be easily with two yuan of above sample pretreatment technology or polynary combining, thereby realize the pre-service to complex sample; The exchange function of single tube and 96-orifice plate makes the specimen preparation instrument have adaptability widely; The design of its Subminature multifunctional is easy to carry and movement, has saved valuable lab space simultaneously; Avoid the introducing error, improved the repeatability of sample; Adding the specimen preparation instrument can also directly link to each other with computing machine, makes it more convenient to use effectively, so this multifunctional all high flux specimen preparation instrument is the brand-new multi-functional specimen preparation new instrument of a cover, is with a wide range of applications.
Description of drawings
The Facad structure synoptic diagram of a kind of specimen preparation instrument that Fig. 1 provides for the utility model;
The structure synoptic diagram of a kind of specimen preparation instrument that Fig. 2 provides for the utility model;
The side structure synoptic diagram of a kind of specimen preparation instrument that Fig. 3 provides for the utility model;
A kind of specimen preparation instrument bottom solid-phase extraction device part right section structural representation that Fig. 4 provides for the utility model;
Vertical view on the 1mL Solid-Phase Extraction column holder that Fig. 5 provides for the utility model;
Vertical view on the 1mL solid-phase extraction column frame bottom hole that Fig. 6 provides for the utility model;
Vertical view on the 3mL Solid-Phase Extraction column holder that Fig. 7 provides for the utility model;
Vertical view on the 3mL solid-phase extraction column frame bottom hole that Fig. 8 provides for the utility model;
Vertical view on the 6mL Solid-Phase Extraction column holder that Fig. 9 provides for the utility model;
Vertical view on the 6mL solid-phase extraction column frame bottom hole that Figure 10 provides for the utility model;
Vertical view on the 10mL Solid-Phase Extraction column holder that Figure 11 provides for the utility model;
Vertical view on the 10mL solid-phase extraction column frame bottom hole that Figure 12 provides for the utility model.
In the accompanying drawing, the list of parts of each label representative is as follows:
1: shell; 2: variable valve;
3: nitrogen blows groove; 4: nitrogen blows panel assembly;
5: nitrogen blows plate; 6: the second pickup grooves;
7: the first pickup grooves; 8: the intermediate seal circle;
9: specimen preparation plate and Solid-Phase Extraction column holder; 10: display control panel;
11: slideway; 12: draw-in groove;
13: the nitrogen flow table; 14: negative pressure dynamics indicator gauge;
15: the nitrogen heating arrangement; 16: fan;
17: the waste liquid flow export; 18: the nitrogen external tapping;
19: the negative pressure interface; 20: power interface;
21: oscillator; 22: lever;
23: negative pressure pump; 24: electric fan;
25: gas-heating apparatus; 26: the side vent port;
27: the electric fan hole;
A:1 mL column jecket hole; Bottom, B:1 mL column jecket hole;
C:3 mL column jecket hole; Bottom, D:3 mL column jecket hole;
E:6 mL column jecket hole; Bottom, F:6 mL column jecket hole;
F:10 mL column jecket hole; Bottom, G:10 mL column jecket hole.
Embodiment
For making the purpose of this utility model, technical scheme and advantage clearer, below in conjunction with accompanying drawing the utility model embodiment is described in further detail.
Therefore, at the problem that exists in the present sample pretreatment, the problem of succeeding in developing that has solved for the specimen preparation field of high flux and automatic multifunctional specimen preparation instrument.The utility model embodiment just at these problems that exist in the sample pretreatment process, has developed a kind of multifunctional all high flux specimen preparation instrument.
For realize semi-automatic so that automatically high flux carry out various specimen preparations experiment, avoid introducing error, improve the repeatability of sample, the utility model embodiment provides a kind of specimen preparation instrument, referring to Fig. 1 to Fig. 4, sees for details hereinafter and describes:
A kind of specimen preparation instrument comprises: shell 1, shell 1 inner top are provided with nitrogen and blow groove 3, are provided with nitrogen in the bottom that nitrogen blows groove 3 and blow panel assembly 4; Both sides and centre position that nitrogen blows panel assembly 4 also are respectively arranged with slideway 11, blow panel assembly 4 at nitrogen and the nitrogen that slides along slideway 11 is set blows plate 5, and slideway 11 is provided with draw-in groove 12, and draw-in groove 12 fixed nitrogens blow plate 5; Shell 1 inner bottom part is provided with for being disposed with intermediate seal circle 8 on first pickup groove, 7, the first pickup grooves 7 of placing the sample liquid dash receiver and second pickup groove, 6, the second pickup grooves 6 are provided with specimen preparation plate and SPE(solid-phase extraction column) support 9; First pickup groove has electric fan hole 27 and side vent port 26 on 7 sides; There is electric fan 24 27 back, electric fan hole; Gas-heating apparatus 25 is arranged at electric fan 24 bottoms; First pickup groove 7, second pickup groove 6, intermediate seal circle 8, specimen preparation plate and SPE support 9 and electric fan 24, gas-heating apparatus 25 and concussion are adorned 21 and are put airtight cavity of common composition; Lever 22 and rocking equipment 21 are arranged at first pickup groove, 7 bottoms; Be provided with waste liquid flow export 17, nitrogen external tapping 18, negative pressure interface 19, power interface 20 and nitrogen gas heating arrangement 15 at housing 1 back side.
Wherein, during specific implementation, the nitrogen that blows groove 3 by nitrogen external tapping 18 realization nitrogen blows; Realize the derivation of waste liquid by waste liquid flow export 17; Realize the energising of specimen preparation instrument by power interface 20.Waste liquid flow export 17 and negative pressure interface 19 are connected to form circuit system by surge flask; In experimentation, the waste liquid that produces flows out by the aperture that is positioned at first pickup groove, 7 bottoms.
Wherein, during specific implementation, can also regulate the height that nitrogen blows plate 5 by slideway 11 and draw-in groove 12.
Wherein, nitrogen blows groove 3 and comprises: variable valve 2, nitrogen blow panel assembly 4 and are arranged on nitrogen by variable valve 2 and blow on the groove 3.Variable valve 2 can be stationary installations such as bolt during specific implementation.
Further, in order to satisfy the multiple needs in the practical application, the model that nitrogen blows plate 5 is specially: 96 holes, 24 holes, 12 holes or 9 holes.Should guarantee in the practical application that nitrogen blows the model of plate 5 and the model of Solid-Phase Extraction column holder is complementary.
When the model of blowing plate 5 when nitrogen is 96 holes, be 8 * 12; When the model of blowing plate 5 when nitrogen is 24 holes, be 3 * 8 or 4 * 6; When the model of blowing plate 5 when nitrogen is 12 holes, be 3 * 4; When the model of blowing plate 5 when nitrogen is 9 holes, be 3 * 3.The nitrogen that is used for the above-mentioned different model of placement on second pickup groove 6 blows plate 5.
Wherein, top nitrogen air blowing body heating arrangement 15 is made up of the heating cylinder body 15 of two series connection.
Further, for the nitrogen flow that nitrogen external tapping 18 is poured is counted, in shell 1, also be provided with nitrogen flow table 13, linked to each other with extraneous source nitrogen by nitrogen external tapping 18 by nitrogen conduit, show concrete airshed size by the nitrogen flow table 13 that is positioned on the shell 1.
Further, for the pressure of show sample preparing instrument inside, on shell 1, also be provided with negative pressure dynamics indicator gauge 14, show vacuum magnitude.
Form negative pressure by the negative pressure pump 23 that places instrument internal, be used for showing that the vacuum meter of vacuum magnitude is by placing negative pressure dynamics indicator gauge 14 realizations on the instrument front panel.
Further, for the airshed that makes specimen preparation instrument inside is disperseed more even, sample can dry up as soon as possible, also be provided with electric fan hole 27 in the side of first pickup groove 7 and link to each other with back electric fan 24, utilize side vent port 26, electric fan 24 bottom heating arrangements 25, first pickup groove 7, second pickup groove 6, intermediate seal circle 8 and specimen preparation plate and airtight cavity of SPE support 9 common formation that the function of circulation heated air is provided.
Further, for the heat radiation of supplementary instrument, also be provided with fan 16 at the back side of shell 1.
Further, for the recovery that improves sample and the reappearance of method, also be provided with oscillation device below first pickup groove 7 and second pickup groove 6, oscillation device comprises: lever 22 and oscillator 21, the first pickup grooves 7 and second pickup groove 6 are connected with oscillator 21 by lever.During specific implementation, the frequency by vibration and time are realized the control to oscillator 21.
Wherein, the mode of operation of this specimen preparation instrument: manually operation and programmed control move two kinds of patterns.Manual mode of operation, in the whole process of sample pretreatment, can be by the button at PC interface, at any time change the temperature of heating, the time-delay of operation, the amount of 96 hole rifle head imbititions, stream of nitrogen gas amount, vacuum tightness size, vacuum time-delay, temperature and the time-delay of auxiliary heat air.Program control mode, more than action in each step controlled by PC, instrument can move according to the step of having set voluntarily, until finishing whole procedure.
When the mode of operation of specimen preparation instrument was the programmed control operation, this specimen preparation instrument also comprised: display control panel 10, and by the regulation and control of display control panel 10 realizations to liquid feeding, positive negative pressure conversion, time-delay, nitrogen blowing temp.The process that realizes is that by the instrument internal whole procedure is carried out software programming, integrated on a chip, external presentation is a LCDs, by the control of display screen realization to all programs of whole device.
The specimen preparation instrument that the utility model embodiment provides, can regulate airshed by external source of the gas, and the airshed size used of can be the at any time online demonstration experiment of the nitrogen flow table 13 that has by instrument itself, thereby can regulate and control as soon as possible; The nitrogen that has by instrument blows panel assembly 4, can realize that different size nitrogen blows the replacing of plate 5, nitrogen blows the O-ring seal on the panel assembly 4, the nitrogen that can guarantee different holes blows plate 5, for example: 96 holes (8 * 12), 24 holes (3 * 8), 24 holes (4 * 6), 12 holes (3 * 4), 9 holes (3 * 3) etc. different size, fit like a glove with the specimen preparation instrument.By the nitrogen gas heating arrangement 15 that specimen preparation instrument inside carries, can realize needed nitrogen temperature in the experiment is controlled; By slideway 11 and draw-in groove 12, realize that nitrogen blows the fixing of plate 5, and the height and position that nitrogen blows plate 5 is adjusted.
Referring to Fig. 5 to Figure 12, the utility model embodiment also designs the SPE support in specimen preparation plate and the SPE support 9, and the model of Solid-Phase Extraction column holder is specially: the Solid-Phase Extraction column holder of 1mL, 3mL, 6mL or 10mL.
When the model of Solid-Phase Extraction column holder was 1mL, 1mL Solid-Phase Extraction column jecket was arranged by 3 * 8 and is placed; When the model of Solid-Phase Extraction column holder was 3mL, 3mL Solid-Phase Extraction column jecket was arranged by 4 * 6 and is placed; When the model of Solid-Phase Extraction column holder was 6mL, 6mL Solid-Phase Extraction column jecket was arranged by 3 * 4 and is placed; When the model of Solid-Phase Extraction column holder was 10mL, 10mL Solid-Phase Extraction column jecket was arranged by 3 * 3 and is placed.
The Solid-Phase Extraction column holder in 96 holes adopts general support in this area, and the utility model embodiment does not do at this and gives unnecessary details.
Wherein, during specific implementation, the O-ring seal on the O-ring seal around first pickup groove 7, first pickup groove 7, second pickup groove 6, second pickup groove 6, and intermediate seal circle 8 has been formed solid-phase extraction device.By changing sample pretreatment Solid-Phase Extraction plate of different nature and realizing different The pretreatment with the dash receiver that the specimen preparation plate is complementary, for example the design of the SPE support of 96 holes (8 * 12), 24 holes (3 * 8), 24 holes (4 * 6), 12 holes (3 * 4), 9 holes (3 * 3) has realized the conversion of the solid-phase extraction column placing plate of specification, thereby has adapted to the demand of different specimen preparations.The existence of intermediate seal circle 8 has realized the sealing of first pickup groove 7 and second pickup groove 6 on the solid-phase extraction device, has guaranteed the sealing in the experimentation, has solved the problem of vacuum magnitude.By the aperture in the middle of first pickup groove, 7 bottoms, the waste liquid that produces in the sample pretreatment process can be derived by inner conduit and the waste liquid flow export that is connected with external waste collection bottle 17 that is positioned at the back side, and with waste collection, reduce the pollution to environment and people.By the circuit system between aperture, inner conduit, waste liquid flow export 17, negative pressure pump 23 and the negative pressure interface 19 on first pickup groove, 7 sides, realize the required negative pressure of sample pretreatment process, show the size of negative pressure by negative pressure dynamics indicator gauge 14 simultaneously, thereby can regulate accordingly.
The principle of work of this specimen preparation instrument is specially: diversified nitrogen blows the design of plate 5, sample after pre-service can being finished directly dries up, and does not need to shift, and has reduced the chance of sample contamination, saved the space simultaneously, and by the dual regulation to airshed and temperature, realize that at different material the nitrogen of different dynamics blows, enlarged the range of application of instrument, in addition, can adopt two kinds of patterns of programmed control and manual operation to carry out nitrogen and blow control, reduce the man power and material.
During specific implementation, nitrogen blows plate 5 can be the rifle head assembly in 96 holes, adds internal components to the control of rifle head assembly accuracy, has realized the effect that the 96 passage volley of rifle fires move liquid and application of sample, has saved time and labour greatly.By regulating different gears, the inhalant liquid scale of construction is controlled.Automatically eject assembly by the rifle head in the design of the lower end of rifle head assembly, reduced automatic application of sample and the time of removing in the rifle head process in the sample pretreatment process, improved sample pretreatment speed, increased efficient.
The robotization solid-phase extraction device has been realized all processes of sample semi-automation and even robotization sample pretreatment.Comprise steps such as the pre-service of extraction column, last sample, drip washing and wash-out.In addition, the design of the Solid-Phase Extraction of semi-automation and even robotization part, the technology of switching repeatedly of employing negative pressure and malleation can be carried out pre-service or drip washing to extraction column at any time, has increased the Modulatory character in the process; The introducing of nitrogen heating arrangement 15 has realized nitrogen air blowing body temperature controlling has been shortened sample greatly and dried up the employed time, can be combined with the malleation of dash receiver part simultaneously, and both direction carries out drying up of liquid, has improved The pretreatment speed.Simultaneously, this specimen preparation instrument has also kept implements traditional single tube Solid-Phase Extraction, support liquid-liquid extraction isotype, can also realize the semi-automatic or full-automatic process of single tube Solid-Phase Extraction.The exchange function of this single tube and 96-orifice plate makes this specimen preparation instrument have adaptability widely.
The concussion function, concussion depends on solid-phase extraction device and realizes that concussion can guarantee the homogeneity that sample mixes in preprocessing process, improves the recovery of sample and the reappearance of method.
Embodiment 1:SPE operating process
C18 bonded silica gel filler, specification are the operating process of 96-well plate of the 2mL in 100mg filler/hole:
The placement of specimen preparation 96 hole C18 filler plates: the 96 hole C18 filler plates of 2mL are fixed on second pickup groove 6 that the last pre-processed board of solid-phase extraction device is placed, make it and fit like a glove on every side.Receiving trap below noting is not put for the time being, guarantees 96 orifice plates and fits like a glove all around, to guarantee the sealing of Solid-Phase Extraction entire portion.
Activation: every hole adds 2mL methyl alcohol, add 1mL for the first time after, after the balance 1min, vacuumize it flowed out, the methyl alcohol that adds 1mL again activates, and vacuumizes after the balance 1min and makes its outflow.Every hole adds the water of 2mL then, and the step that adds according to methyl alcohol activates.After activation is finished, vacuumize activating solution is flowed out fully, finish the reactivation process of pillar.
Last sample: the benzoic acid aqueous solution 1mL that pipettes concentration and be 500 μ g/mL goes up in the hole of sample to 96 orifice plate, and sample solution following of nature under the gravity effect if a following speed is very slow, can adopt sample process in the acceleration of assisted vacuum, and the vacuum dynamics is controlled to be-0.5bar.The principle of last sample is, the speed that sample liquid is following is can not ether fast, guarantee that the absorption of sample on pillar can reach balance, and is also can not ether slow, otherwise can prolong analysis time, and general 1mL sample liquid needs 1-3min.
Drip washing: draw the specimen preparation plate that the water of 1mL joins in specimen preparation plate and the SPE support 9 with 96 row's liquid-transfering gun heads of upper part and carry out drip washing; repeat 2 times; if the following speed of leacheate is very slow; then start the carrying out of the auxiliary lessivation of negative pressure function; leacheate is flowed out, and the vacuum dynamics is controlled to be-0.5bar.
With taking off of specimen preparation plate and SPE support 9, dash receiver is placed the trough of solid-phase extraction device first pickup groove 7, specimen preparation plate and SPE support 9 are restored, place original position.Attention: guarantee sealing.
Wash-out: the methyl alcohol that pipettes 1mL with 96 rifle heads joins in the specimen preparation plate in specimen preparation plate and the SPE support 9, make following naturally of leacheate, if a following speed is very slow, then vacuumize auxiliary drip washing, leacheate is flowed in the dash receiver, repeat this process several times repeatedly, finally need the methyl alcohol of 3mL that the complete drip washing of sample is got off.
Dry up: specimen preparation plate and SPE support 9 are removed, following dash receiver is taken out, place the position of specimen preparation plate and SPE support 9, nitrogen dries up.Simultaneously, the bottom can adopt heated air to assist to dry up.The stream of nitrogen gas amount is 0.6mL/min.The temperature of following heating is controlled to be 30 ℃.
Redissolve: the distilled water or the damping fluid that pipette 1mL join in the sample well ultrasonic redissolution.
Embodiment 2: medium liquid-liquid extraction (SLE) operating process
The operating process of medium liquid-liquid extraction, the specification of used 96 hole SLE plates is: amount of filler is the SLE96 orifice plate of the 2mL in 200mg/ hole.
Place dash receiver: place solid-phase extraction device to place the trough of first pickup groove 7 of dash receiver dash receiver.
The placement of specimen preparation plate 96 hole SLE plates: the 96 hole SLE plates of 2mL are fixed on second pickup groove 6 that the last pre-processed board of solid-phase extraction device is placed, make it and fit like a glove on every side.
Last sample: the concentration that pipettes 200 μ L is the propylparaben aqueous solution of 200 μ g/mL, and last sample is noted in SLE post hole: maximum applied sample amount should guarantee that sample can not flow out balance 5min.
Extraction: the methylene chloride that pipettes 1mL with 96 rifle heads joins in specimen preparation plate and the SPE support 9, makes following naturally of leacheate, and leacheate flows in the dash receiver, repeats this process several times repeatedly, finally needs the methylene chloride of 3-5mL that the complete drip washing of sample is got off.If a following speed is very slow, then vacuumize auxiliary drip washing, the vacuum dynamics is controlled to be-0.5bar, continues 10-15s.
Dry up: (being determined on a case-by-case basis) removes 96-well plate specimen preparation plate and SPE support 9, and following dash receiver is placed on second pickup groove 6 of placing specimen preparation plate and SPE support 9, and nitrogen dries up, and adds down that hot-air is auxiliary to be dried up.Nitrogen air blowing flow is 0.6mL/min, and the temperature of following heating is controlled to be 30 ℃.
Redissolve: if sample need dry up processing, distilled water or the damping fluid that then need pipette 1mL join in the sample well ultrasonic redissolution.
Embodiment 3: novel protein sedimentation operating process
Fast protein sedimentation operating process, the specification of used 96 orifice plates are the penetrating shape plate of 1mL.
Put into dash receiver: dash receiver is placed on first pickup groove 7 that solid-phase extraction device is placed dash receiver.
The placement of specimen preparation plate 96 hole PPT plates: the 96 hole PPT plates of 1mL are fixed on second pickup groove, 6 places that the last pre-processed board of solid-phase extraction device is placed, guarantee 96 orifice plates and fit like a glove all around, to guarantee the sealing of Solid-Phase Extraction entire portion.
Last sample: the acetonitrile that pipettes 1mL with 96 rifle heads joins in the 96 hole PPT specimen preparation plates, and the pending sample solution that pipettes 200 μ L again joins in the sample well that contains the 1mL acetonitrile, and concussion 2min precipitates protein fully.
Vacuumize: vacuumize liquid is flowed out fully.The vacuum tightness size is controlled to be-0.8bar.Attention: the dynamics that vacuumizes can not be too big, otherwise film is leaked, and causes sample to become muddy.
Dry up (being determined on a case-by-case basis): remove the 96 hole PPT specimen preparation plates that are positioned at specimen preparation plate and SPE support 9 places, following dash receiver is placed the position of specimen preparation plate, nitrogen dries up, and adds down that hot-air is auxiliary to be dried up.Nitrogen air blowing flow is 0.6mL/min, and the temperature of following heating is controlled to be 30 ℃.
Redissolve: the distilled water or the damping fluid that pipette 1mL join in the sample well ultrasonic redissolution.
Embodiment 4: the operating process of dynamic Solid-Phase Extraction (DPE)
Dynamic solid phase collection operating process: the Tip specification: the SCX amount of filler is the rifle head of 50mg/1mL
Activation: the DPE post is connected on the liquid-transfering gun of 1mL, sucks 0.5mL methyl alcohol and an amount of air, make the abundant mixing of filler and solution, behind the mixing, methyl alcohol is got, suck the water of 0.5mL again, mixing, activation.
Last sample: below the DPE post, place the little reagent bottle of a 2mL, contain 0.6 sample solution in the reagent bottle, suck sample, and air is passed through, from but sample fully mix with filler, balance 25 seconds is got, go up sample again, 2 times repeatedly, all be sucked out up to sample.
Drip washing: suck each 1mL washing DPE pillar of methanol-water successively, at last aqueous solution is got.
Wash-out: the ammonification methanol solution 1mL of absorption 5% is in dash receiver, suck repeatedly and get 3 times, to guarantee that melamine is eluted fully, at last the eluent in the dash receiver is dried up, dash receiver is placed on second pickup groove 6, dry up, regulating the upper part nitrogen flow is 0.6mL/min, below temperature be controlled to be 30 ℃, bottom hot gas flow be instrument itself with airshed, need not regulate.
Redissolve: add the methanol aqueous solution of the 50:50 of 1mL, ultrasonic redissolution is filtered, and is to be detected.
In sum, the utility model embodiment provides a kind of specimen preparation instrument, the utility model embodiment can be simultaneously with high flux nitrogen blowing apparatus, rocking equipment with move subsidiary function in the specimen preparations such as liquid and the core technology of specimen preparation has organically been joined together, be integrated on same the instrument; In addition, this instrument can also be easily with two yuan of above sample pretreatment technology or polynary combining, thereby realize the pre-service to complex sample; The exchange function of single tube and 96-orifice plate makes the specimen preparation instrument have adaptability widely; The design of its Subminature multifunctional is easy to carry and movement, has saved valuable lab space simultaneously; Avoid the introducing error, improved the repeatability of sample; Adding the specimen preparation instrument can also directly link to each other with computing machine, makes it more convenient to use effectively, so this multifunctional all high flux specimen preparation instrument is the brand-new multi-functional specimen preparation new instrument of a cover, is with a wide range of applications.
It will be appreciated by those skilled in the art that accompanying drawing is the synoptic diagram of a preferred embodiment, above-mentioned the utility model embodiment sequence number does not represent the quality of embodiment just to description.
The above only is preferred embodiment of the present utility model, and is in order to limit the utility model, not all within spirit of the present utility model and principle, any modification of doing, is equal to replacement, improvement etc., all should be included within the protection domain of the present utility model.
Claims (10)
1. specimen preparation instrument comprises: shell (1), it is characterized in that described shell (1) inner top is provided with nitrogen and blows groove (3), and be provided with nitrogen in the bottom that described nitrogen blows groove (3) and blow panel assembly (4); Both sides and centre position that described nitrogen blows panel assembly (4) also are respectively arranged with slideway (11), blowing panel assembly (4) at described nitrogen arranges the nitrogen that slides along described slideway (11) and blows plate (5), described slideway (11) is provided with draw-in groove (12), and the fixing described nitrogen of described draw-in groove (12) blows plate (5); Described shell (1) inner bottom part is provided with for first pickup groove (7) of placing the sample liquid dash receiver, be disposed with intermediate seal circle (8) and second pickup groove (6) on described first pickup groove (7), described second pickup groove (6) is provided with specimen preparation plate and Solid-Phase Extraction column holder (9); Be provided with waste liquid flow export (17), nitrogen external tapping (18), negative pressure interface (19), power interface (20) and nitrogen heating arrangement (15) at described shell (1) back side, there is two electric fans of device (24) and the gas-heating apparatus (25) that recyclegas is provided at described first pickup groove (7) back; Described two electric fans (24) are that first pickup groove (7) provides hydronic gas by two electric fan holes (27) and the side vent port (26) that is positioned on first pickup groove (7) sidewall; Be provided with oscillator (21), lever (22) and negative pressure pump (23) in described first pickup groove (7) bottom.
2. a kind of specimen preparation instrument according to claim 1 is characterized in that, described nitrogen blows groove (3) and comprising: variable valve (2), described nitrogen blow panel assembly (4) and are arranged on described nitrogen by described variable valve (2) and blow on the groove (3).
3. a kind of specimen preparation instrument according to claim 1 is characterized in that, the model that described nitrogen blows plate (5) is specially: 96 holes, 24 holes, 12 holes or 9 holes; Described nitrogen blows the model of plate (5) and the model of described Solid-Phase Extraction column holder is complementary.
4. a kind of specimen preparation instrument according to claim 1 is characterized in that, described nitrogen heating arrangement (15) is made up of the heating cylinder body of two series connection.
5. a kind of specimen preparation instrument according to claim 1 is characterized in that, also is provided with nitrogen flow table (13) in the described shell (1), is linked to each other with extraneous source nitrogen by described nitrogen external tapping (18) by nitrogen conduit; Also be provided with negative pressure dynamics indicator gauge (14) on the described shell (1), show vacuum magnitude; The back side of described shell (1) also is provided with fan (16).
6. a kind of specimen preparation instrument according to claim 1 is characterized in that, the bottom of described first pickup groove (7) also is provided with aperture, realizes the bottom negative pressure by described aperture and negative pressure pump (23); The side of described first pickup groove (7) also is provided with three apertures, wherein electric fan hole (27) and electric fan (24) directly communicate, side vent port (26), electric fan hole (27), electric fan (24) and solid-phase extraction device be common to form an airtight box, thereby dries up the heated air that process provides circulation for Solid-Phase Extraction.
7. a kind of specimen preparation instrument according to claim 1, it is characterized in that, below described first pickup groove (7) and described second pickup groove (6), also be provided with oscillation device, described oscillation device comprises: lever (22) and oscillator (21), described first pickup groove (7) is connected described oscillator (21) with described second pickup groove (6) by described lever (22).
8. a kind of specimen preparation instrument according to claim 1 is characterized in that, described specimen preparation instrument also comprises: display control panel (10),
By the regulation and control of described display control panel (10) realization to liquid feeding, positive negative pressure conversion, time-delay, nitrogen blowing temp.
9. according to claim 1 or 3 described a kind of specimen preparation instrument, it is characterized in that described nitrogen blows the rifle head assembly that plate (5) is specially 96 holes.
10. a kind of specimen preparation instrument according to claim 1 is characterized in that the model of described Solid-Phase Extraction column holder is specially: 1mL, 3mL, 6mL or 10mL;
When the model of described Solid-Phase Extraction column holder was 1mL, 1ml Solid-Phase Extraction column jecket was arranged by 3 * 8 and is placed; When the model of described Solid-Phase Extraction column holder was 3mL, 3mL Solid-Phase Extraction column jecket was arranged by 4 * 6 and is placed; When the model of described Solid-Phase Extraction column holder was 6mL, 6mL Solid-Phase Extraction column jecket was arranged by 3 * 4 and is placed; When the model of described Solid-Phase Extraction column holder was 10mL, 10mL Solid-Phase Extraction column jecket was arranged by 3 * 3 and is placed.
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CN 201320072541 CN203164043U (en) | 2013-02-07 | 2013-02-07 | Sample preparation instrument |
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CN 201320072541 CN203164043U (en) | 2013-02-07 | 2013-02-07 | Sample preparation instrument |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103175727A (en) * | 2013-02-07 | 2013-06-26 | 天津奥顺达科技有限公司 | Sample preparation instrument |
CN103884575A (en) * | 2014-03-28 | 2014-06-25 | 云南省农业科学院农业环境资源研究所 | Hot air nitrogen blowing instrument |
CN113030341A (en) * | 2021-04-14 | 2021-06-25 | 南芯芯仪(广州)制造有限公司 | System for preparing liquid phase tandem mass spectrum sample |
CN115219606A (en) * | 2021-04-20 | 2022-10-21 | 广州禾信仪器股份有限公司 | Automatic water sample pretreatment device, treatment method and automatic water sample detection system |
-
2013
- 2013-02-07 CN CN 201320072541 patent/CN203164043U/en not_active Withdrawn - After Issue
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103175727A (en) * | 2013-02-07 | 2013-06-26 | 天津奥顺达科技有限公司 | Sample preparation instrument |
CN103175727B (en) * | 2013-02-07 | 2015-10-14 | 天津奥顺达科技有限公司 | A kind of sample preparation instrument |
CN103884575A (en) * | 2014-03-28 | 2014-06-25 | 云南省农业科学院农业环境资源研究所 | Hot air nitrogen blowing instrument |
CN113030341A (en) * | 2021-04-14 | 2021-06-25 | 南芯芯仪(广州)制造有限公司 | System for preparing liquid phase tandem mass spectrum sample |
CN113030341B (en) * | 2021-04-14 | 2022-09-16 | 南芯芯仪(广州)制造有限公司 | System for preparing liquid phase tandem mass spectrum sample |
CN115219606A (en) * | 2021-04-20 | 2022-10-21 | 广州禾信仪器股份有限公司 | Automatic water sample pretreatment device, treatment method and automatic water sample detection system |
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