CN103623611A - Ultrasonic-assisted anti-blocking solid-phase extraction device - Google Patents
Ultrasonic-assisted anti-blocking solid-phase extraction device Download PDFInfo
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Abstract
The invention discloses an ultrasonic-assisted anti-blocking solid-phase extraction device. The ultrasonic-assisted anti-blocking solid-phase extraction device comprises a collection device and an ultrasonic-assisted system vertically arranged above the collection device, wherein the ultrasonic-assisted system comprises a water tank, solid-phase extraction column troughs and an ultrasonic oscillating plate capable of ultrasonically oscillating along the vertical direction of the solid-phase extraction column troughs, the solid-phase extraction column troughs and the ultrasonic oscillating plate are vertically arranged in the water tank, openings are formed in both the upper and lower ends of each solid-phase extraction column trough, and the ultrasonic oscillating plate is arranged on one sides of the solid-phase extraction column troughs and is parallel with the side faces of the solid-phase extraction column troughs; the collection device is communicated with the openings in the lower ends of the solid-phase extraction column troughs through flow guide tubes, and valves are arranged on the flow guide tubes between the collection device and the solid-phase extraction column troughs. According to the ultrasonic-assisted anti-blocking solid-phase extraction device, air films cannot be formed on the surfaces of liquid-phase and solid adsorbing materials, the blockage of solid-phase extraction columns is avoided, and samples can pass through the solid-phase extraction columns at a steady speed. Besides, the invention further discloses a method for carrying out the solid-phase extraction by the device.
Description
Technical field
The present invention relates to a kind of chemical analysis extraction equipment, especially a kind of solid-phase extraction device.
Background technology
Water environment safety is to be related to a happy and peace major issue.To water environment, comprise in the different water bodys such as surface water, underground water, seawater that pollutant monitoring and drinking water safety problem are the important process contents of a plurality of mechanisms such as Environmental Protection Department, the Ministry of Public Health, quality inspection portion.Because the contents level of thing to be detected in water sample is extremely low, instrument direct-detection cannot meet country and industry standard demand.Therefore the pretreatment process link that is absolutely necessary, and pretreatment process has decisive role to the accuracy of sample result.Water sample pretreatment process mainly comprises liquid-liquid extraction method and solid phase extraction comparatively widely at present.Wherein to have solvent-oil ratio few for solid phase extraction, and method accuracy and precision are high, and can effectively remove a plurality of advantages such as chaff interference in water body, become one of pre-treatment means important in important analyzing and testing industry.In existing standard, the multiclass organic pollutions such as the Microcystin in water body, polycyclic aromatic hydrocarbon, nonyl phenol, nitrophenol are all set up based on solid phase extraction techniques.
In prior art, the flow process that adopts solid phase extraction to carry out pre-treatment to water sample is as shown in the table:
As seen from the above table, by sample, by solid-phase extraction column, the time that example enrichment link needs in pretreatment process is the longest.The object of this step is that object is adsorbed on solid phase column filler completely, is the most key link of SPE.Yet in actual sample analytic process, often there is clogging during by solid-phase extraction column in water sample, increased analysis time, cannot, by sample all by solid-phase extraction column, cause the inaccurate phenomenon of interpretation of result even.
At present ，Duo company all developmental research gone out solid-phase extraction device, existing solid-phase extraction device mainly comprises seal cover (above having solid-phase extraction column mounting interface, conduit, sealing-plug), vavuum pump connector, Pressure gauge, rack for test tube, pressure-reducing valve etc.Its accessory comprises large volume sampling pipe, post converting interface etc.During sample analysis, solid-phase extraction device is connected to vavuum pump, solid-phase extraction column and sample successively.Under condition of negative pressure, sample is introduced solid phase extraction column by conduit by sample; Or under condition of negative pressure, sample passes through extraction column by the 60ml syringe being connected on solid-phase extraction column.
In example enrichment process, water sample flow velocity is set to 5-10mL, and the theory analysis time of 0.5L water sample is 50-100 minute.But, in sample analysis process, between solid phase extraction column stuffing and water surface, can form air film, result in blockage, make sample to pass through smoothly pillar, flow velocity can be reduced to < 1ml/min, stops up even completely.Now, by knocking pillar, bubble can be discharged, make flow restoration.Yet solid phase extraction column stuffing and water contact-making surface place can form air film very soon again, stop that sample passes through.Due to above reason, in actual sample analytic process, 0.5L water sample often needs 3-4 hour, even longer analysis time, SPE process, extend analysis time, staff must keep by solid-phase extracting instrument for a long time simultaneously, has caused waste of human resource.If the extract of soil, deposit or biological tissue samples, enrichment time will be longer, and have and cannot realize whole samples all by the phenomenon of solid-phase extraction column.Before it is pointed out that example enrichment, filter particle in sample is removed, can't cause due to particle the obstruction of water sample.This problem is because the gas in the aqueous solution overflows when the enrichment, and the air film forming in water and solid phase (solid phase column filler) has stopped that sample, by the process of solid phase extraction column, has also weakened the adsorption process of sorbing material to object.
At present, also have the on-line solid phase extraction device that improves design for above-mentioned existing solid-phase extraction device, enrichment, solid phase column purification, drip washing, wash-out liquid nitrogen that described on-line solid phase extraction device can be realized sample by software setting blow the functions such as concentrated.In enrichment process, on-line solid phase extraction device not only, in the tail end negative pressure of post, forms tractive force to sample; , at post front end, exert pressure meanwhile, make the aqueous solution fast by solid phase pillar.On-line solid phase extraction technology also fails to avoid in example enrichment process, between sample and solid phase filler, between water and solid phase, to form air film, and therefore, this technology can not be improved the pretreatment process of sample.On the contrary, owing to existing in solid phase column front-end and back-end uniform pressure, for preventing that pressure is excessive, cause leakage, very high to the requirement of sample, only have the water sample that impurity content is extremely low can be applicable to this technological means; In addition, high pressure also may cause sample penetration solid phase column, and the object in the aqueous solution is not adsorbed by solid phase column, reduces extraction efficiency, makes measurement result incorrect.
Through experiment, confirm, while adopting existing above-mentioned solid phase extraction equipment to carry out SPE, with allow water sample take 5mL/min flow velocity during by solid phase pillar as example, the gas that after 10min～20min, fluid sample is separated out forms air film at solid phase pillar filling surface, makes sample be reduced to rapidly <1mL/min by the speed of pillar; If with 5mL/min flow velocity during by solid phase pillar, 5min left and right sample is reduced to <1mL/min by the flow velocity of solid phase extraction column containing the sample extraction solution of 10% methyl alcohol.Now, can the air film forming between liquid phase and solid adsorption material is broken by knocking vibration, sample flow rate is increased to 3-5mL/min; But after 3-5min, between liquid phase and solid adsorption material, again form, flow velocity reduces again; In a word in example enrichment process, " vibration---flow velocity quickening---flow velocity slows down---vibration " becomes cyclic process.Therefore, no matter adopt solid-phase extraction device described above, or on-line solid phase extraction device, being all faced with uncontrollable problem analysis time, staff needs long-time stay-at-home by solid-phase extraction device, is unfavorable for saving human cost.
Summary of the invention
The object of the invention is to provide for above-mentioned the deficiencies in the prior art part a kind of can prevent liquid phase and solid adsorption material surface form air film, avoid solid phase column stop up, guarantee sample with stable speed by the solid-phase extraction device of solid phase extraction column.In addition, another object of the present invention is to provide a kind of method that adopts described solid-phase extraction device to carry out SPE.
For achieving the above object, the technical scheme that the present invention takes is: a kind of ultrasonic wave is assisted anti-clogging solid-phase extraction device, comprises gathering-device and the ultrasonic wave accessory system that is vertical at described gathering-device top;
Described ultrasonic wave accessory system comprise water tank, solid-phase extraction column groove with can be along the sonic oscillation plate of the direction sonic oscillation vertical with described solid-phase extraction column groove, described solid-phase extraction column groove and sonic oscillation plate are all vertical in described water tank, the two ends up and down of described solid-phase extraction column groove are equipped with opening, and described sonic oscillation plate is located at a side of described solid-phase extraction column groove and is parallel to the side of described solid-phase extraction column groove;
Described gathering-device is by the open communication of mozzle and described solid-phase extraction column groove lower end, and the mozzle between described gathering-device and described solid-phase extraction column groove is provided with valve.
Ultrasonic wave of the present invention is assisted anti-clogging solid-phase extraction device, and in described ultrasonic wave accessory system, solid-phase extraction column groove is used for placing solid-phase extraction column, and described sonic oscillation plate is vertical in described water tank, and is positioned at a side of described solid-phase extraction column groove.During use, solid-phase extraction column is placed in to described solid-phase extraction column groove, sample is incorporated in described solid-phase extraction column, can use vavuum pump to connect gathering-device negative pressure is provided, traction sample passes through solid-phase extraction column, open described sonic oscillation plate hight low amplitude oscillation frequently simultaneously, thereby for the solid-phase extraction column in described solid-phase extraction column groove provides lasting high frequency low amplitude oscillation, lasting vibration makes the air film of liquid phase and solid adsorption material contact-making surface in solid-phase extraction column broken, effectively prevented the obstruction causing due to air film in example enrichment process, guarantee that sample passes through solid-phase extraction column with stable speed.And, the object in sample with solid adsorption material by fully contacting, thereby guaranteed that object can be caught by the high efficiency absorption of solid adsorption material, improve the accuracy of measurement result.The sample described solid-phase extraction column of flowing through, then by the mozzle being connected with described solid-phase extraction column groove lower ending opening, flow in gathering-device, the valve arranging on mozzle between described gathering-device and described solid-phase extraction column groove, in order to control the flowing of liquid of the mozzle of flowing through.
As the preferred embodiment of the auxiliary anti-clogging solid-phase extraction device of ultrasonic wave of the present invention, described water tank is located at the top of described gathering-device by support vertical.Can a plurality of supports be set in corner or the optional position of described water tank, support the top that described ultrasonic wave accessory system is vertical at described gathering-device.
As the preferred embodiment of the auxiliary anti-clogging solid-phase extraction device of ultrasonic wave of the present invention, the parallel two row's solid-phase extraction column grooves that are provided with in described water tank, described sonic oscillation plate is located at the centre of described two row's solid-phase extraction column grooves.Usually, two row's solid-phase extraction column grooves be arranged in parallel in described water tank, every row arranges a plurality of solid-phase extraction column grooves, described sonic oscillation plate is located to the centre of two row's solid-phase extraction column grooves, and what can guarantee the equilibrium of described sonic oscillation plate is the lasting high frequency low amplitude oscillation of solid-phase extraction column.
Preferred embodiment as the auxiliary anti-clogging solid-phase extraction device of ultrasonic wave of the present invention, described solid-phase extraction column groove is the hollow cylindrical that two ends are provided with opening, and the upper and lower two ends of described solid-phase extraction column groove are opened on respectively upper surface and the lower surface of described water tank.Preferably, the two ends of described solid-phase extraction column groove are opened on respectively upper surface and the lower surface of described water tank, and described solid-phase extraction column groove penetrates into lower surface from the upper surface extension of described water tank, facilitates like this placement and the taking-up of solid-phase extraction column.
As the preferred embodiment of the auxiliary anti-clogging solid-phase extraction device of ultrasonic wave of the present invention, the lower ending opening of described solid-phase extraction column groove is connected with described mozzle by adapter.Usually, the lower ending opening diameter of described solid-phase extraction column groove is larger, upper end from the lower ending opening of described solid-phase extraction column groove to described mozzle need to dwindle gradually, be the narrow cone shape in wide lower end, upper end, therefore, the lower ending opening of solid-phase extraction column groove need to be connected with described mozzle by adapter, so that solution can be stable, by mozzle, flow into gathering-device.
As the preferred embodiment of the auxiliary anti-clogging solid-phase extraction device of ultrasonic wave of the present invention, described water tank is cuboid hermetically-sealed construction, and the front and back sides of described water tank is transparency glass plate.The front and back sides of described water tank is set to transparency glass plate, is convenient to staff and sees through the state that transparency glass plate is observed sample.
As the preferred embodiment of the auxiliary anti-clogging solid-phase extraction device of ultrasonic wave of the present invention, described sonic oscillation plate connects the power supply that promising its vibration provides power.
As the preferred embodiment of the auxiliary anti-clogging solid-phase extraction device of ultrasonic wave of the present invention, the bottom of described gathering-device is provided with sample flow export.The sample flow export that described gathering-device bottom arranges, the liquid that conveniently enters into gathering-device flows out.
As the preferred embodiment of the auxiliary anti-clogging solid-phase extraction device of ultrasonic wave of the present invention, the bottom of described water tank is provided with water out.The water out that described water tank bottom arranges facilitates the outflow of water.
In addition, the present invention also provides a kind of flow speed stability, SPE method that analysis efficiency is higher, and described method adopts the as above auxiliary anti-clogging solid-phase extraction device of arbitrary described ultrasonic wave to complete, and said method comprising the steps of:
(1) solid-phase extraction column is placed in to described solid-phase extraction column groove, activates described solid-phase extraction column;
(2) sample is introduced in solid-phase extraction column, and connected the power supply of sonic oscillation plate simultaneously, make sonic oscillation plate hight low amplitude oscillation frequently;
(3) at sample, by the filler in solid-phase extraction column, all flow in the process of gathering-device, waste liquid is discharged by gathering-device;
(4) use suitable solvent to wash away the impurity on filler in solid-phase extraction column, the solution after washing away flows into gathering-device and then discharges;
(5) with suitable solvent by the object wash-out in filler in solid-phase extraction column, collect eluent, analyze.
In SPE method of the present invention, first according to the characteristic of the sample of required analysis, the solid-phase extraction column that selection contains suitable solid adsorption material, the solid-phase extraction column of selection is placed in to described solid-phase extraction column groove, adopt existing conventional method activation solid-phase extraction column, then sample is incorporated in solid-phase extraction column, generally under the condition of negative pressure, by conduit, sample is incorporated in solid-phase extraction column, connect the power supply of sonic oscillation plate simultaneously, sonic oscillation plate starts high frequency low amplitude oscillation, thereby for described solid-phase extraction column provides lasting high frequency low amplitude oscillation, vibration makes the air film fragmentation of liquid phase and solid adsorption material contact-making surface in solid-phase extraction column, effectively prevented the obstruction causing due to air film in example enrichment process, make sample pass through described solid-phase extraction column with stable speed.Sample by solid-phase extraction column flow in gathering-device, then from gathering-device, discharges.Object in sample and impurity are attracted in the solid adsorption material of solid-phase extraction column, select suitable solvent to wash away the impurity on solid adsorption material in solid-phase extraction column, and the solution that contains impurity after washing away is discharged from gathering-device, and then select suitable solvent in solid-phase extraction column, to be adsorbed on the object wash-out of solid adsorption material, collect eluent, and eluent is concentrated, then adopt suitable means to carry out monitoring analysis.
Ultrasonic wave of the present invention is assisted anti-clogging solid-phase extraction device, side at solid-phase extraction column groove arranges sonic oscillation plate, during use, described sonic oscillation plate can provide high frequency low amplitude oscillation, thereby provide the vibration by a narrow margin of lasting high frequency for being placed in the solid-phase extraction column of described solid-phase extraction column groove, prevent that liquid phase and solid adsorption material surface from forming air film, avoided solid-phase extraction column to stop up, guarantee that sample can pass through solid-phase extraction column with a stable speed; Staff can amount per sample correctly estimate the SPE time, without long-time stay-at-home on solid-phase extraction device side, has effectively saved human cost.And, due to the object in sample with the solid adsorption material in solid-phase extraction column by fully contacting, thereby can guarantee that object can be caught by the high efficiency absorption of solid adsorption material, improve the accuracy of measurement result.SPE method of the present invention, owing to adopting the auxiliary anti-clogging solid-phase extraction device of ultrasonic wave of the present invention, in the process of extraction, because sonic oscillation plate provides lasting high frequency low amplitude oscillation for solid-phase extraction column, effectively prevented that liquid phase and solid adsorption material surface from forming air film, avoided solid-phase extraction column to stop up, can make sample pass through solid-phase extraction column with stable speed, and can guarantee that object can be caught by the high efficiency absorption of solid adsorption material, improve the accuracy of measurement result.
Accompanying drawing explanation
Fig. 1 is the structural representation of the auxiliary a kind of embodiment of anti-clogging solid-phase extraction device of ultrasonic wave of the present invention.
Fig. 2 is the use status architecture schematic diagram of the auxiliary a kind of embodiment of anti-clogging solid-phase extraction device of ultrasonic wave shown in Fig. 1.。
Fig. 3 is the structural representation of a kind of embodiment of supersonic oscillations accessory system in the auxiliary anti-clogging solid-phase extraction device of ultrasonic wave shown in Fig. 1.
Fig. 4 is the polycrystalline substance schematic diagram of supersonic oscillations accessory system shown in Fig. 3.
In figure, 10 is that gathering-device, 12 is that mozzle, 14 is that valve, 16 is that sample flow export, 20 is that ultrasonic wave accessory system, 22 is that water tank, 23 is that water out, 24 is that solid-phase extraction column groove, 240 is solid-phase extraction column, and 25 is that adapter, 26 is that support, 27 is that power supply, 30 is that shuttle, 32 is conduit.
The specific embodiment
For the object, technical solutions and advantages of the present invention are better described, below in conjunction with the drawings and specific embodiments, the invention will be further described.
A kind of embodiment of the auxiliary anti-clogging solid-phase extraction device of ultrasonic wave of the present invention, as shown in accompanying drawing 1 and 3, comprises gathering-device 10 and the ultrasonic wave accessory system 20 that is vertical at described gathering-device 10 tops; Described ultrasonic wave accessory system 20 comprise water tank 22, solid-phase extraction column groove 24 with can be along the sonic oscillation plate 26 of the direction sonic oscillation vertical with described solid-phase extraction column groove 24, described solid-phase extraction column groove 24 and sonic oscillation plate 26 are all vertical in described water tank 22, the two ends up and down of described solid-phase extraction column groove 24 are equipped with opening, and described sonic oscillation plate 26 is located at a side of described solid-phase extraction column groove 24 and is parallel to the side of described solid-phase extraction column groove 24; Described gathering-device 10 is the open communication with described solid-phase extraction column groove 24 lower ends by mozzle 12, and the mozzle 12 between described gathering-device 10 and described solid-phase extraction column groove 24 is provided with valve 14.
Ultrasonic wave described above is assisted anti-clogging solid-phase extraction device, in described ultrasonic wave accessory system 20, solid-phase extraction column groove 24 is for placing solid-phase extraction column 240, and described sonic oscillation plate 26 is vertical in described water tank 22, and is positioned at a side of described solid-phase extraction column groove 24.During use, as shown in attached Fig. 1 and 2, solid-phase extraction column 240 is placed in to described solid-phase extraction column groove 24, sample is incorporated in described solid-phase extraction column 240 by conduit 32 from shuttle 30, open described sonic oscillation plate 26 high frequency low amplitude oscillation simultaneously, thereby for the solid-phase extraction column 240 in described solid-phase extraction column groove 24 provides lasting high frequency low amplitude oscillation, lasting vibration makes the air film of liquid phase and solid adsorption material contact-making surface in solid-phase extraction column 240 broken, effectively prevented the obstruction causing due to air film in example enrichment process, guarantee that sample passes through solid-phase extraction column with stable speed.And, the object in sample with solid adsorption material by fully contacting, thereby guaranteed that object can be caught by the high efficiency absorption of solid adsorption material, improve the accuracy of measurement result.The sample described solid-phase extraction column 240 of flowing through, then by the mozzle 12 being connected with described solid-phase extraction column groove 24 lower ending openings, flow in gathering-device 10, the valve 14 arranging on mozzle 12 between described gathering-device 10 and described solid-phase extraction column groove 24, in order to control the flowing of liquid of the mozzle 12 of flowing through.
Preferably, as shown in Figure 2, described water tank 22 is vertical at the top of described gathering-device 10 by support 28.Can a plurality of supports 28 be set in corner or the optional position of described water tank 22, support the top that described ultrasonic wave accessory system 20 is vertical at described gathering-device 10.
Preferably, as shown in Figure 2, the parallel two row's solid-phase extraction column grooves 24 that are provided with in described water tank 22, described sonic oscillation plate 26 is located at the centre of described two row's solid-phase extraction column grooves 24.Usually, two row's solid-phase extraction column grooves 24 be arranged in parallel in described water tank 22, every row arranges a plurality of solid-phase extraction column grooves 24, described sonic oscillation plate 26 is located to the centre of two row's solid-phase extraction column grooves 24, what can guarantee described sonic oscillation plate 26 equilibriums is the lasting high frequency low amplitude oscillation of solid-phase extraction column.
Preferably, as shown in Figure 2, described solid-phase extraction column groove 24 is provided with the hollow cylindrical of opening for two ends, and described solid-phase extraction column groove is opened on respectively upper surface and the lower surface of described water tank 22 in two ends Shang Xia 24.Preferably, the two ends of described solid-phase extraction column groove 24 are opened on respectively upper surface and the lower surface of described water tank 22, and described solid-phase extraction column groove 24 penetrates into lower surface from the upper surface extension of described water tank 22, facilitates like this placement and the taking-up of solid-phase extraction column.
Preferably, as shown in Figure 3, the lower ending opening of described solid-phase extraction column groove 24 is connected with described mozzle 12 by adapter 25.Usually, the lower ending opening diameter of described solid-phase extraction column groove 24 is larger, upper end from the lower ending opening of described solid-phase extraction column groove 24 to described mozzle 12 need to dwindle gradually, be the narrow cone shape in wide lower end, upper end, therefore, the lower ending opening of solid-phase extraction column groove 24 need to be connected with described mozzle 12 by adapter 25, so that the mozzle 12 that passes through that solution can be stable flow into gathering-device 10.Described adapter 25 is fixed by screw thread with water tank 22 back plate connections, and placement is leaked.
Preferably, as shown in Figure 2, described water tank 22 is cuboid hermetically-sealed construction, and the front and back sides of described water tank 22 is transparency glass plate.The front and back sides of described water tank 22 is set to transparency glass plate, is convenient to staff and sees through the state that transparency glass plate is observed sample.
Preferably, as shown in Figure 1, described sonic oscillation plate 26 connects the power supply 27 that promising its vibration provides power.
Preferably, as shown in Figure 1, the bottom of described gathering-device 10 is provided with sample flow export 16.The sample flow export 16 that described gathering-device 10 bottoms arrange, the liquid that conveniently enters into gathering-device 10 flows out.Described sample flow export can connect surge flask (not shown in FIG.) and vavuum pump (not shown in FIG.) successively, convenient in use for gathering-device provides negative pressure, and traction sample passes through solid-phase extraction column.More preferably, as shown in Figure 1, the bottom of described water tank 22 is provided with water out 23, facilitates the outflow of water.
The method that adopts the auxiliary anti-clogging solid-phase extraction device of ultrasonic wave described above to carry out SPE, comprises the following steps:
(1) solid-phase extraction column is placed in to described solid-phase extraction column groove 24, activates described solid-phase extraction column;
(2) sample is introduced in solid-phase extraction column by conduit 32 from shuttle 30, and connected the power supply 27 of sonic oscillation plate 26 simultaneously, make sonic oscillation plate 26 high frequency low amplitude oscillation;
(3) at sample, by the filler in solid-phase extraction column, all flow in the process of gathering-device 10, the discarded sample of collecting in gathering-device 10 is discharged;
(4) use suitable solvent to wash away the impurity on filler in solid-phase extraction column, the solution after washing away flows into gathering-device 10 and then discharges;
(5) with suitable solvent by the object wash-out in filler in solid-phase extraction column, collect eluent, analyze.
In SPE method described above, first according to the characteristic of the sample of required analysis, the solid-phase extraction column that selection contains suitable solid adsorption material, the solid-phase extraction column of selection is placed in to described solid-phase extraction column groove 24, adopt existing conventional method activation solid-phase extraction column, then sample is incorporated in solid-phase extraction column, generally under the condition of negative pressure, by conduit, sample is incorporated in solid-phase extraction column, connect the power supply 27 of sonic oscillation plate 26 simultaneously, sonic oscillation plate 26 starts high frequency low amplitude oscillation, thereby for described solid-phase extraction column provides lasting high frequency low amplitude oscillation, vibration makes the air film fragmentation of liquid phase and solid adsorption material contact-making surface in solid-phase extraction column, effectively prevented the obstruction causing due to air film in example enrichment process, make sample pass through described solid-phase extraction column with stable speed.Sample by solid-phase extraction column flow in gathering-device 10, then from gathering-device 10, discharges.Object in sample and impurity are attracted in the solid adsorption material of solid-phase extraction column, select suitable solvent to wash away the impurity on solid adsorption material in solid-phase extraction column, and the solution that contains impurity after washing away is discharged from gathering-device 10, and then select suitable solvent in solid-phase extraction column, to be adsorbed on the object wash-out of solid adsorption material, collect eluent, and eluent is concentrated, then adopt suitable means to carry out monitoring analysis.
Embodiment 1
Ultrasonic wave of the present invention is assisted anti-clogging solid-phase extraction device service test
Take and analyze in bark PFOS (PFOS) and demonstrate supersonic oscillations servicing unit operation principle for example:
First, accurately take the bark sample 1.5g after freeze drying, sample is contained in 50mL polypropylene vial (PP), and adds acetonitrile 10mL, sonic oscillation 30min, centrifugal rear supernatant is transferred in another 50mLPP bottle.Re-extract 3 times, combining extraction liquid 30mL, nitrogen blows and is concentrated into 10mL, adds high purity water 40mL, mixes, through 0.8 μ m membrane filtration.Then through solid-phase extraction column enrichment, purify.Solidify the method that extracting process carries out SPE with the auxiliary anti-clogging solid-phase extraction device of employing described above ultrasonic wave of the present invention, after SPE completes, eluent is concentrated into 1mL, use using high performance liquid chromatography tandem mass spectrum instrument monitoring analysis.
Table 1 has been listed 12 samples and has been used ultrasonic auxiliary anti-clogging solid-phase extraction device analytic process sample flow rate of the present invention and analysis result.
Table 2 has been listed 12 samples and has been adopted existing solid-phase extraction device analytic process sample flow rate and analysis result.
Table 1 is used sample flow rate and the result of ultrasonic auxiliary anti-clogging solid-phase extraction device of the present invention
Table 2 is used sample flow rate and the result of existing solid-phase extraction device
The data of contrast table 1 and table 2 can find out, while using existing solid-phase extraction device to sample analysis, sample may occur all by solid phase pillar, realizing the phenomenon of enrichment, thereby causes analysis result on the low side.On the other hand, also obviously find out and use ultrasonic auxiliary anti-clogging solid-phase extraction device of the present invention can improve sample analysis speed, and guarantee the stability of sample determination result simultaneously.
Last institute should be noted that; above embodiment is only in order to illustrate technical scheme of the present invention but not limiting the scope of the invention; although the present invention is explained in detail with reference to preferred embodiment; those of ordinary skill in the art is to be understood that; can modify or be equal to replacement technical scheme of the present invention, and not depart from essence and the scope of technical solution of the present invention.
Claims (10)
1. the auxiliary anti-clogging solid-phase extraction device of ultrasonic wave, is characterized in that, comprises gathering-device and the ultrasonic wave accessory system that is vertical at described gathering-device top;
Described ultrasonic wave accessory system comprise water tank, solid-phase extraction column groove with can be along the sonic oscillation plate of the direction sonic oscillation vertical with described solid-phase extraction column groove, described solid-phase extraction column groove and sonic oscillation plate are all vertical in described water tank, the two ends up and down of described solid-phase extraction column groove are equipped with opening, and described sonic oscillation plate is located at a side of described solid-phase extraction column groove and is parallel to the side of described solid-phase extraction column groove;
Described gathering-device is by the open communication of mozzle and described solid-phase extraction column groove lower end, and the mozzle between described gathering-device and described solid-phase extraction column groove is provided with valve.
2. the auxiliary anti-clogging solid-phase extraction device of ultrasonic wave as claimed in claim 1, is characterized in that, described water tank is located at the top of described gathering-device by support vertical.
3. the auxiliary anti-clogging solid-phase extraction device of ultrasonic wave as claimed in claim 1, is characterized in that, the parallel two row's solid-phase extraction column grooves that are provided with in described water tank, and described sonic oscillation plate is located at the centre of described two row's solid-phase extraction column grooves.
4. the ultrasonic wave as described in claim 1 or 3 is assisted anti-clogging solid-phase extraction device, it is characterized in that, described solid-phase extraction column groove is the hollow cylindrical that two ends are provided with opening, and the upper and lower two ends of described solid-phase extraction column groove are opened on respectively upper surface and the lower surface of described water tank.
5. the auxiliary anti-clogging solid-phase extraction device of ultrasonic wave as claimed in claim 4, is characterized in that, the lower ending opening of described solid-phase extraction column groove is connected with described mozzle by adapter.
6. the auxiliary anti-clogging solid-phase extraction device of ultrasonic wave as claimed in claim 1, is characterized in that, described water tank is cuboid hermetically-sealed construction, and the front and back sides of described water tank is transparency glass plate.
7. the auxiliary anti-clogging solid-phase extraction device of ultrasonic wave as claimed in claim 1, is characterized in that, described sonic oscillation plate connects the power supply that promising its vibration provides power.
8. the auxiliary anti-clogging solid-phase extraction device of ultrasonic wave as claimed in claim 1, is characterized in that, the bottom of described gathering-device is provided with sample flow export.
9. the auxiliary anti-clogging solid-phase extraction device of ultrasonic wave as claimed in claim 1, is characterized in that, the bottom of described water tank is provided with water out.
Employing as arbitrary in claim 1-9 as described in the auxiliary anti-clogging solid-phase extraction device of a ultrasonic wave method of carrying out SPE, it is characterized in that, comprise the following steps:
(1) solid-phase extraction column is placed in to described solid-phase extraction column groove, activates described solid-phase extraction column;
(2) sample is introduced in solid-phase extraction column, and connected the power supply of sonic oscillation plate simultaneously, make sonic oscillation plate hight low amplitude oscillation frequently;
(3) at sample, by the filler in solid-phase extraction column, all flow in the process of gathering-device, waste liquid is discharged by gathering-device;
(4) use suitable solvent to wash away the impurity on filler in solid-phase extraction column, the solution after washing away flows into gathering-device and then discharges;
(5) with suitable solvent by the object wash-out in filler in solid-phase extraction column, collect eluent, analyze.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106198129A (en) * | 2016-07-11 | 2016-12-07 | 中国海洋大学 | A kind of example reaction generates gas collector |
| CN106237653A (en) * | 2016-08-16 | 2016-12-21 | 福州大学 | Hand-held is from ultrasound wave solid-phase microextraction rod and using method thereof |
| CN106908513A (en) * | 2017-03-09 | 2017-06-30 | 浙江大学 | It is a kind of for 96 hole high flux solid-phase extraction devices of mass spectral analysis and its application |
| CN106932516A (en) * | 2017-04-18 | 2017-07-07 | 蔡明红 | Original position ultrasound washing device and ultrasonic elution process based on SPE sampling column |
| CN110465113A (en) * | 2019-08-21 | 2019-11-19 | 广东联捷生物科技有限公司 | Integrated sample extraction box |
| CN112924266A (en) * | 2020-12-25 | 2021-06-08 | 湖北鼎泰高科有限公司 | Column socket of solid-phase extraction nitrogen blowing concentrator and nitrogen blowing assembly |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106198129A (en) * | 2016-07-11 | 2016-12-07 | 中国海洋大学 | A kind of example reaction generates gas collector |
| CN106237653A (en) * | 2016-08-16 | 2016-12-21 | 福州大学 | Hand-held is from ultrasound wave solid-phase microextraction rod and using method thereof |
| CN106237653B (en) * | 2016-08-16 | 2018-05-04 | 福州大学 | Hand-held is from ultrasonic wave solid phase microextraction rod and its application method |
| CN106908513A (en) * | 2017-03-09 | 2017-06-30 | 浙江大学 | It is a kind of for 96 hole high flux solid-phase extraction devices of mass spectral analysis and its application |
| CN106908513B (en) * | 2017-03-09 | 2019-08-06 | 杭州汇健科技有限公司 | It is a kind of for 96 hole high throughput solid-phase extraction devices of mass spectral analysis and its application |
| CN106932516A (en) * | 2017-04-18 | 2017-07-07 | 蔡明红 | Original position ultrasound washing device and ultrasonic elution process based on SPE sampling column |
| CN110465113A (en) * | 2019-08-21 | 2019-11-19 | 广东联捷生物科技有限公司 | Integrated sample extraction box |
| CN112924266A (en) * | 2020-12-25 | 2021-06-08 | 湖北鼎泰高科有限公司 | Column socket of solid-phase extraction nitrogen blowing concentrator and nitrogen blowing assembly |
| CN112924266B (en) * | 2020-12-25 | 2024-01-19 | 湖北鼎泰高科有限公司 | Column insert and nitrogen blowing assembly of solid phase extraction nitrogen blowing concentrator |
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