CN103623611B - Ultrasonic assistant anti-clogging solid-phase extraction device - Google Patents
Ultrasonic assistant anti-clogging solid-phase extraction device Download PDFInfo
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Abstract
The present invention discloses a kind of ultrasonic assistant anti-clogging solid-phase extraction device, and it comprises gathering-device and is vertical at the ultrasonic assistant system above described gathering-device; Described ultrasonic assistant system comprise water tank, solid-phase extraction column groove with can along the sonic oscillation plate of the direction sonic oscillation vertical with described solid-phase extraction column groove, solid-phase extraction column groove and sonic oscillation plate are all vertical in described water tank, the two ends up and down of solid-phase extraction column groove are equipped with opening, and sonic oscillation plate is located at the side of solid-phase extraction column groove and is parallel to the side of solid-phase extraction column groove; Gathering-device is by the open communication of mozzle and solid-phase extraction column groove lower end, and the mozzle between gathering-device and solid-phase extraction column groove is provided with valve.Solid-phase extraction device of the present invention, can prevent liquid phase and solid adsorption material surface from forming air film, avoid solid-phase extraction column to block, the stable speed of guarantee sample passes through solid-phase extraction column.In addition, the invention also discloses the method adopting described device to carry out SPE.
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 related to a happy and peace major issue.To water environment, comprising pollutant monitoring and drinking water safety problem in the different water body such as surface water, underground water, seawater is the important process content of multiple 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 professional standard demand.Therefore pretreatment process is absolutely necessary link, and the accuracy of pretreatment process to sample result has decisive role.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, method accuracy and precision high, and effectively can remove multiple advantage such as chaff interference in water body, become one of pre-treatment means important in important analysis detection 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 adopting 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, namely time of needing in pretreatment process of example enrichment link 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.But in actual sample analytic process, water sample often occurs clogging by during solid-phase extraction column, makes increase analysis time, by sample all by solid-phase extraction column, the inaccurate phenomenon of interpretation of result cannot be caused even.
At present, all developmental research of many companies has gone out solid-phase extraction device, and 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 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 be connected on solid-phase extraction column.
In example enrichment process, water sample flow velocity is set to 5-10mL, and namely the theory analysis time of 0.5L water sample is 50-100 minute.But in sample analysis process, can form air film, result in blockage between solid phase extraction column stuffing and aqueous phase surface, make sample cannot smoothly by pillar, flow velocity can be reduced to < 1ml/min, blocks even completely.Now, bubble can be discharged by knocking pillar, making flow restoration.But solid phase extraction column stuffing and aqueous phase contact 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, solid phase extraction procedure, analysis time extends, staff must keep by solid-phase extracting instrument for a long time simultaneously, causes 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 sample all by the phenomenon of solid-phase extraction column.Before it is pointed out that example enrichment, filter and particle in sample is removed, the blocking of water sample can't be caused due to particle.This problem is that the air film formed at aqueous phase and solid phase (solid phase column filler) blocks the process of sample by solid phase extraction column, also weakens the adsorption process of sorbing material to object because the gas in the aqueous solution overflows when enrichment.
At present, also there is the on-line solid phase extraction device carrying out Curve guide impeller for above-mentioned existing solid-phase extraction device, described on-line solid phase extraction device can realize enrichment to sample by software design patterns, solid phase column purification, drip washing, wash-out liquid nitrogen 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; Meanwhile, apply pressure in post front end, make the aqueous solution quickly through solid phase pillar.On-line solid phase extraction technology also fails to avoid in example enrichment process between sample and solid phase filler, and namely form air film between aqueous phase and solid phase, therefore, this technology can not improve the pretreatment process of sample.On the contrary, owing to existing in solid phase column front-end and back-end uniform pressure, in order to prevent, pressure is excessive causes leakage, very high to the requirement of sample, only has the extremely low water sample of impurity content 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.
Confirm through experiment, when adopting existing above-mentioned solid phase extraction equipment to carry out SPE, with allow water sample for 5mL/min flow velocity by solid phase pillar time, 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 <1mL/min rapidly by the speed of pillar; If when the sample extraction solution containing 10% methyl alcohol passes through solid phase pillar with 5mL/min flow velocity, about 5min sample is reduced to <1mL/min by the flow velocity of solid phase extraction column.Now, can be broken by the air film formed between liquid phase and solid adsorption material by knocking vibration, sample flow rate is increased to 3-5mL/min; But after 3-5min, again formed between liquid phase and solid adsorption material, flow velocity reduces again; In a word in example enrichment process, " vibration---flow velocity quickening---flows decrease---vibration " become cyclic process.Therefore, no matter adopt solid-phase extraction device described above, or on-line solid phase extraction device, be all faced with uncontrollable problem analysis time, staff needs stay-at-home by solid-phase extraction device for a long time, 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 and can prevent liquid phase and solid adsorption material surface from forming air film, avoid solid phase column to block, ensure that sample is with the solid-phase extraction device of stable speed by solid phase extraction column.In addition, another object of the present invention is to provide a kind of method adopting 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 assistant anti-clogging solid-phase extraction device, comprises gathering-device and is vertical at the ultrasonic assistant system above described gathering-device;
Described ultrasonic assistant system comprise water tank, solid-phase extraction column groove with can 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 the 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 assistant anti-clogging solid-phase extraction device of the present invention, in described ultrasonic assistant system, solid-phase extraction column groove is for placing solid-phase extraction column, and described sonic oscillation plate is vertical in described water tank, and is positioned at the side of described solid-phase extraction column groove.During use, solid-phase extraction column is placed in described solid-phase extraction column groove, sample is incorporated in described solid-phase extraction column, vavuum pump can be used 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, thus provide the vibration of lasting frequency low-amplitude for the solid-phase extraction column in described solid-phase extraction column groove, the vibration continued makes the air film of liquid phase and solid adsorption material contact surface in solid-phase extraction column broken, effectively prevent in example enrichment process due to blocking that air film causes, ensure that sample passes through solid-phase extraction column with stable speed.And the object in sample and solid adsorption material by fully contacting, thus ensure that object can be caught by the high efficiency absorption of solid adsorption material, improve the accuracy of measurement result.Sample flows through described solid-phase extraction column, then the mozzle by being connected with described solid-phase extraction column groove lower ending opening flow in gathering-device, the valve that mozzle between described gathering-device and described solid-phase extraction column groove is arranged, in order to the flowing of control flow check through the liquid of mozzle.
As the preferred embodiment of ultrasonic assistant anti-clogging solid-phase extraction device of the present invention, described water tank is located at the top of described gathering-device by support vertical.Multiple support can be set in the corner of described water tank or optional position, support the top that described ultrasonic assistant systematic vertical is located at described gathering-device.
As the preferred embodiment of ultrasonic assistant anti-clogging solid-phase extraction device of the present invention, parallelly in described water tank be provided with two row's solid-phase extraction column grooves, the centre of described two row's solid-phase extraction column grooves is located at by described sonic oscillation plate.Usually, be arranged in parallel in described water tank two row's solid-phase extraction column grooves, often row arranges multiple solid-phase extraction column groove, described sonic oscillation plate is located at the centre of two row's solid-phase extraction column grooves, can ensure the frequency low-amplitude vibration lasting for solid-phase extraction column of described sonic oscillation plate equilibrium.
As the preferred embodiment of ultrasonic assistant anti-clogging solid-phase extraction device of the present invention, described solid-phase extraction column groove is the hollow cylindrical that two ends are provided with opening, and the described upper and lower two ends of solid-phase extraction column groove are opened on upper surface and the lower surface of described water tank respectively.Preferably, the two ends of described solid-phase extraction column groove are opened on upper surface and the lower surface of described water tank respectively, and namely described solid-phase extraction column groove penetrates into lower surface from the upper surface extension of described water tank, facilitates placement and the taking-up of solid-phase extraction column like this.
As the preferred embodiment of ultrasonic assistant anti-clogging solid-phase extraction device 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 needs to reduce gradually, the cone shape that wide lower end is narrow in upper end, therefore, the lower ending opening of solid-phase extraction column groove needs to be connected with described mozzle by adapter, flow into gathering-device with what make that solution can be stable by mozzle.
As the preferred embodiment of ultrasonic assistant anti-clogging solid-phase extraction device 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 observes sample state through transparency glass plate.
As the preferred embodiment of ultrasonic assistant anti-clogging solid-phase extraction device of the present invention, described sonic oscillation plate connects the power supply that its vibration promising provides power.
As the preferred embodiment of ultrasonic assistant anti-clogging solid-phase extraction device 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 is arranged, the liquid conveniently entering into gathering-device flows out.
As the preferred embodiment of ultrasonic assistant anti-clogging solid-phase extraction device of the present invention, the bottom of described water tank is provided with water out.The water out that described water tank bottom is arranged facilitates the outflow of water.
In addition, the present invention also provides the solid phase extraction method that a kind of flow speed stability, analysis efficiency are higher, and described method adopts as above arbitrary described ultrasonic assistant anti-clogging solid-phase extraction device to complete, and said method comprising the steps of:
(1) solid-phase extraction column is placed in described solid-phase extraction column groove, activates described solid-phase extraction column;
(2) sample is introduced in solid-phase extraction column, and connect the power supply of sonic oscillation plate simultaneously, make sonic oscillation plate hight low amplitude oscillation frequently;
(3) all flow in the process of gathering-device by the filler in solid-phase extraction column at sample, waste liquid is discharged by gathering-device;
(4) use suitable solvent to wash away impurity in solid-phase extraction column on filler, 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 solid phase extraction method of the present invention, first according to the characteristic of the sample of required analysis, select the solid-phase extraction column containing appropriate solid sorbing material, the solid-phase extraction column of selection is placed in described solid-phase extraction column groove, adopt existing conventional method activated solid 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 frequency low-amplitude vibration, thus provide the vibration of lasting frequency low-amplitude for described solid-phase extraction column, vibration makes the air film of liquid phase and solid adsorption material contact surface in solid-phase extraction column broken, effectively prevent the blocking caused due to air film in example enrichment process, make sample with stable speed by described solid-phase extraction column.Flow in gathering-device by the sample of solid-phase extraction column, then discharge from gathering-device.Object in sample and impurity are attracted in the solid adsorption material of solid-phase extraction column, suitable solvent is selected to wash away impurity in solid-phase extraction column on solid adsorption material, and discharge washing away the rear solution containing impurity from gathering-device, and then select suitable solvent will be adsorbed on the object wash-out of solid adsorption material in solid-phase extraction column, collect eluent, and eluent is concentrated, then adopt suitable means to carry out monitoring analysis.
Ultrasonic assistant anti-clogging solid-phase extraction device of the present invention, at the side of solid-phase extraction column groove, sonic oscillation plate is set, during use, described sonic oscillation plate can provide frequency low-amplitude to vibrate, thus provide the vibration of lasting frequency low-amplitude for the solid-phase extraction column being placed in described solid-phase extraction column groove, prevent liquid phase and solid adsorption material surface from forming air film, avoid solid-phase extraction column and block, guarantee sample can pass through solid-phase extraction column with a stable speed; Staff amount per sample can correctly estimate the SPE time, without the need to stay-at-home on solid-phase extraction device side for a long time, effectively saves human cost.And, because the object in sample and the solid adsorption material in solid-phase extraction column are by fully contacting, thus can guarantee that object can be caught by the high efficiency absorption of solid adsorption material, improving the accuracy of measurement result.Solid phase extraction method of the present invention, owing to adopting ultrasonic assistant anti-clogging solid-phase extraction device of the present invention, in the process of extraction, due to sonic oscillation plate for solid-phase extraction column provides lasting frequency low-amplitude vibration, effectively prevent liquid phase and solid adsorption material surface formation air film, avoid solid-phase extraction column to block, sample can be made to pass through solid-phase extraction column with stable speed, and can ensure 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 a kind of embodiment of ultrasonic assistant anti-clogging solid-phase extraction device of the present invention.
Fig. 2 is the using state structural representation of a kind of embodiment of the anti-clogging of ultrasonic assistant shown in Fig. 1 solid-phase extraction device.。
Fig. 3 is the structural representation of a kind of embodiment of supersonic oscillations accessory system in the anti-clogging of ultrasonic assistant shown in Fig. 1 solid-phase extraction device.
Fig. 4 is the polycrystalline substance schematic diagram of the accessory system of supersonic oscillations shown in Fig. 3.
In figure, 10 be gathering-device, 12 be mozzle, 14 be valve, 16 be sample flow export, 20 be ultrasonic assistant system, 22 be water tank, 23 be water out, 24 be solid-phase extraction column groove, 240 for solid-phase extraction column, 25 be adapter, 26 be support, 27 be power supply, 30 be shuttle, 32 be conduit.
Detailed description of the invention
For better the object, technical solutions and advantages of the present invention being described, below in conjunction with the drawings and specific embodiments, the invention will be further described.
A kind of embodiment of ultrasonic assistant anti-clogging solid-phase extraction device of the present invention, as shown in accompanying drawing 1 and 3, the ultrasonic assistant system 20 comprising gathering-device 10 and be vertical at above described gathering-device 10; Described ultrasonic assistant system 20 comprise water tank 22, solid-phase extraction column groove 24 with can 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 the 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 by the open communication of mozzle 12 with described solid-phase extraction column groove 24 lower end, and the mozzle 12 between described gathering-device 10 and described solid-phase extraction column groove 24 is provided with valve 14.
Ultrasonic assistant anti-clogging solid-phase extraction device described above, in described ultrasonic assistant 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 the side of described solid-phase extraction column groove 24.During use, as shown in figure 1 and 2, solid-phase extraction column 240 is placed in described solid-phase extraction column groove 24, sample is incorporated in described solid-phase extraction column 240 by conduit 32 from shuttle 30, open the vibration of described sonic oscillation plate 26 frequency low-amplitude simultaneously, thus provide the vibration of lasting frequency low-amplitude for the solid-phase extraction column 240 in described solid-phase extraction column groove 24, the vibration continued makes the air film of liquid phase and solid adsorption material contact surface in solid-phase extraction column 240 broken, effectively prevent in example enrichment process due to blocking that air film causes, ensure that sample passes through solid-phase extraction column with stable speed.And the object in sample and solid adsorption material by fully contacting, thus ensure that object can be caught by the high efficiency absorption of solid adsorption material, improve the accuracy of measurement result.Sample flows through described solid-phase extraction column 240, then the mozzle 12 by being connected with described solid-phase extraction column groove 24 lower ending opening flow in gathering-device 10, the valve 14 that mozzle 12 between described gathering-device 10 and described solid-phase extraction column groove 24 is arranged, in order to the flowing of control flow check through the liquid of mozzle 12.
Preferably, as shown in Figure 2, described water tank 22 is vertical at the top of described gathering-device 10 by support 28.Multiple support 28 can be set in the corner of described water tank 22 or optional position, support the top that described ultrasonic assistant system 20 is vertical at described gathering-device 10.
Preferably, as shown in Figure 2, parallelly in described water tank 22 be provided with two row's solid-phase extraction column grooves 24, the centre of described two row's solid-phase extraction column grooves 24 is located at by described sonic oscillation plate 26.Usually, be arranged in parallel in described water tank 22 two row's solid-phase extraction column grooves 24, often row arranges multiple solid-phase extraction column groove 24, described sonic oscillation plate 26 is located at the centre of two row's solid-phase extraction column grooves 24, the frequency low-amplitude vibration lasting for solid-phase extraction column of described sonic oscillation plate 26 equilibrium can be ensured.
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 about 24 two ends are opened on upper surface and the lower surface of described water tank 22 respectively.Preferably, the two ends of described solid-phase extraction column groove 24 are opened on upper surface and the lower surface of described water tank 22 respectively, and namely described solid-phase extraction column groove 24 penetrates into lower surface from the upper surface extension of described water tank 22, facilitates placement and the taking-up of solid-phase extraction column like this.
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 needs to reduce gradually, the cone shape that wide lower end is narrow in upper end, therefore, the lower ending opening of solid-phase extraction column groove 24 needs to be connected with described mozzle 12 by adapter 25, flow into gathering-device 10 with what make that solution can be stable by mozzle 12.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 observes sample state through transparency glass plate.
Preferably, as shown in Figure 1, described sonic oscillation plate 26 connects the power supply 27 that its vibration promising 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 bottom is arranged, the liquid conveniently entering 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.
Adopt ultrasonic assistant anti-clogging solid-phase extraction device described above to carry out the method for SPE, comprise the following steps:
(1) solid-phase extraction column is placed in 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 connect the power supply 27 of sonic oscillation plate 26 simultaneously, sonic oscillation plate 26 frequency low-amplitude is vibrated;
(3) all flow in the process of gathering-device 10 at sample by the filler in solid-phase extraction column, the waste sample collected in gathering-device 10 is discharged;
(4) use suitable solvent to wash away impurity in solid-phase extraction column on filler, 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 solid phase extraction method described above, first according to the characteristic of the sample of required analysis, select the solid-phase extraction column containing appropriate solid sorbing material, the solid-phase extraction column of selection is placed in described solid-phase extraction column groove 24, adopt existing conventional method activated solid 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 frequency low-amplitude vibration, thus provide the vibration of lasting frequency low-amplitude for described solid-phase extraction column, vibration makes the air film of liquid phase and solid adsorption material contact surface in solid-phase extraction column broken, effectively prevent the blocking caused due to air film in example enrichment process, make sample with stable speed by described solid-phase extraction column.Flow in gathering-device 10 by the sample of solid-phase extraction column, then discharge from gathering-device 10.Object in sample and impurity are attracted in the solid adsorption material of solid-phase extraction column, suitable solvent is selected to wash away impurity in solid-phase extraction column on solid adsorption material, and discharge washing away the rear solution containing impurity from gathering-device 10, and then select suitable solvent will be adsorbed on the object wash-out of solid adsorption material in solid-phase extraction column, collect eluent, and eluent is concentrated, then adopt suitable means to carry out monitoring analysis.
Embodiment 1
Ultrasonic assistant anti-clogging solid-phase extraction device service test of the present invention
To analyze PFOS (PFOS) demonstration supersonic oscillations servicing unit operation principle in bark:
First, accurately take the bark samples 1.5g after freeze drying, be contained in by sample in 50mL polypropylene vial (PP), and add acetonitrile 10mL, sonic oscillation 30min, centrifuged 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 μm of membrane filtration.Then purify through solid-phase extraction column enrichment.Solidification extracting process carries out the method for SPE with employing described above ultrasonic assistant anti-clogging of the present invention solid-phase extraction device, after SPE completes, eluent is concentrated into 1mL, uses using high performance liquid chromatography tandem mass spectrum instrument monitoring analysis.
Table 1 lists 12 samples and uses ultrasonic wave added anti-clogging solid-phase extraction device analytic process sample flow rate of the present invention and analysis result.
Table 2 lists 12 samples and adopts existing solid-phase extraction device analytic process sample flow rate and analysis result.
Table 1 uses sample flow rate and the result of ultrasonic wave added anti-clogging solid-phase extraction device of the present invention
Table 2 uses sample flow rate and the result of existing solid-phase extraction device
The data of contrast table 1 and table 2 can be found out, when using existing solid-phase extraction device to sample analysis, the phenomenon that all cannot be realized enrichment by solid phase pillar may appear in sample, thus causes analysis result on the low side.On the other hand, also obviously find out and use ultrasonic wave added anti-clogging solid-phase extraction device of the present invention can improve sample analysis speed, and guarantee the stability of sample determination result simultaneously.
Finally to 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 be explained in detail the present invention with reference to preferred embodiment; those of ordinary skill in the art is to be understood that; can modify to technical scheme of the present invention or equivalent replacement, and not depart from essence and the scope of technical solution of the present invention.
Claims (10)
1. a ultrasonic assistant anti-clogging solid-phase extraction device, is characterized in that, comprises gathering-device and is vertical at the ultrasonic assistant system above described gathering-device;
Described ultrasonic assistant system comprise water tank, solid-phase extraction column groove with can 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 the 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. ultrasonic assistant anti-clogging solid-phase extraction device as claimed in claim 1, it is characterized in that, described water tank is located at the top of described gathering-device by support vertical.
3. ultrasonic assistant anti-clogging solid-phase extraction device as claimed in claim 1, is characterized in that, parallelly in described water tank is provided with two row's solid-phase extraction column grooves, and the centre of described two row's solid-phase extraction column grooves is located at by described sonic oscillation plate.
4. the ultrasonic assistant anti-clogging solid-phase extraction device as described in claim 1 or 3, it is characterized in that, described solid-phase extraction column groove is the hollow cylindrical that two ends are provided with opening, and the described upper and lower two ends of solid-phase extraction column groove are opened on upper surface and the lower surface of described water tank respectively.
5. ultrasonic assistant anti-clogging solid-phase extraction device as claimed in claim 4, it is characterized in that, the lower ending opening of described solid-phase extraction column groove is connected with described mozzle by adapter.
6. ultrasonic assistant anti-clogging solid-phase extraction device as claimed in claim 1, it 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. ultrasonic assistant anti-clogging solid-phase extraction device as claimed in claim 1, is characterized in that, described sonic oscillation plate connects the power supply that its vibration promising provides power.
8. ultrasonic assistant anti-clogging solid-phase extraction device as claimed in claim 1, it is characterized in that, the bottom of described gathering-device is provided with sample flow export.
9. ultrasonic assistant anti-clogging solid-phase extraction device as claimed in claim 1, it is characterized in that, the bottom of described water tank is provided with water out.
10. adopt as arbitrary in claim 1-9 as described in ultrasonic assistant anti-clogging solid-phase extraction device carry out the method for SPE, it is characterized in that, comprise the following steps:
(1) solid-phase extraction column is placed in described solid-phase extraction column groove, activates described solid-phase extraction column;
(2) sample is introduced in solid-phase extraction column, and connect the power supply of sonic oscillation plate simultaneously, make sonic oscillation plate hight low amplitude oscillation frequently;
(3) all flow in the process of gathering-device by the filler in solid-phase extraction column at sample, waste liquid is discharged by gathering-device;
(4) use suitable solvent to wash away impurity in solid-phase extraction column on filler, 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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| 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 |
| 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 |
| CN110465113B (en) * | 2019-08-21 | 2021-11-09 | 广东联捷生物科技有限公司 | Integrated sample extraction box |
| 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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| CN101797448A (en) * | 2010-04-12 | 2010-08-11 | 吉林大学 | High-flux dynamic microwave-assisted extraction device |
| CN102043028A (en) * | 2010-11-16 | 2011-05-04 | 中国水产科学研究院东海水产研究所 | Method for quickly detecting environmental endocrine disruptors in seawater |
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