CN211274688U - Capillary liquid drop micro-fluidic device - Google Patents
Capillary liquid drop micro-fluidic device Download PDFInfo
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- CN211274688U CN211274688U CN201921473724.2U CN201921473724U CN211274688U CN 211274688 U CN211274688 U CN 211274688U CN 201921473724 U CN201921473724 U CN 201921473724U CN 211274688 U CN211274688 U CN 211274688U
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Abstract
A capillary liquid drop micro-fluidic device relates to the field of chromatographic column preparation. Comprises a dispersed phase input capillary, a continuous phase input capillary, a liquid drop output capillary, a connecting capillary and a tee joint; the dispersion phase input capillary penetrates through a first input end and an output end of the tee joint, one end of the dispersion phase input capillary is conical, and the conical end is positioned on one side of the output end; one end of the liquid drop output capillary is sleeved with the conical end of the disperse phase input capillary, and a gap is formed at the joint of the liquid drop output capillary and the disperse phase input capillary; a connecting capillary tube is sleeved outside the joint, and one end of the connecting capillary tube is inserted into the output end of the tee joint and is communicated with the interior of the tee joint; one end of the continuous phase input capillary tube is inserted into the second input end of the tee joint and is communicated with the interior of the tee joint. The capillary liquid drop microfluidic device is simple in structure and convenient to operate, and the prepared microspheres have high monodispersity and are suitable for being used as silicon dioxide microsphere materials of capillary plungers of various specifications.
Description
Technical Field
The utility model relates to a chromatographic column preparation field especially relates to a capillary liquid drop micro-fluidic device.
Background
From 1988, it is first proposed to date that nanoflow liquid chromatography is gradually developed into an important supplement of traditional high performance liquid chromatography, and especially plays an important role in the fields of proteomics and pharmaceutical analysis, and capillary chromatographic columns applied to nanoflow liquid chromatography have become key separation tools in the analysis of biomolecules. The capillary chromatographic column mainly comprises an open-tube capillary column, an integral column and a particle packed column. Due to the high sample capacity, high sensitivity and reproducibility, particle-packed capillary columns are currently the most commonly used capillary columns in micro-scale bioseparation and analysis applications.
One of the core problems of the particle-packed capillary column technology is the plunger technology. The function of the plunger is to retain the stationary phase within the capillary while allowing the mobile phase to freely permeate; the use of the plunger is accompanied with the problems of peak broadening, bubble generation and the like, and the regulation and control of parameters such as the material, the permeability, the mechanical strength, the length and the like of the plunger are key links for preparing the high-quality particle-filled capillary column. The current plunger preparation processes which are commonly used mainly comprise: monolithic plunger technology, sintering technology, tail cone technology, and single particle plunger technology. The single particle plunger technology fixes a single microsphere as a plunger at one end of a capillary based on the kerbstone effect, and the preparation process is very simple and convenient: a porous silicon ball slightly larger than the inner diameter of the hollow capillary tube is clamped at one end of the hollow capillary tube, and then the silicon ball is pressed into the tube on a horizontal table top. The column bed occupied by the plug made by this process is only one microsphere in size, and if the microspheres used can be controlled to be highly monodisperse and uniform, the reproducibility between packed capillary columns will be greatly improved when the plug is made based on single particle plug technology. Meanwhile, if the particle size of the microspheres can be controlled, the column preparation process of capillary liquid chromatographic columns with various specifications can be greatly simplified, and the standardization of capillary column quality control is further promoted.
The silicon spheres generally have high mechanical strength, and the monodisperse silicon dioxide microspheres with the cross-linked and through hole structures can meet various requirements of single-particle plungers, and are very suitable single-particle plunger materials. However, no preparation method for preparing silicon ball materials with different particle sizes, high monodispersity, high permeability and high mechanical strength is reported in the existing literature. Therefore, the development of a simple preparation technology capable of preparing single-particle plunger microsphere materials with high throughput and controlling the particle size of the microspheres is a key problem in the technical field.
Disclosure of Invention
An object of the utility model is to solve the above-mentioned problem among the prior art, provide a capillary liquid drop micro-fluidic device, capillary liquid drop micro-fluidic device simple structure, convenient operation adopts the microballon of the device preparation to have high monodispersity, is applicable to the silica microsphere material as various specification capillary plungers.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
a capillary droplet microfluidic device comprises a dispersed phase input capillary, a continuous phase input capillary, a droplet output capillary, a connecting capillary and a tee joint; the tee joint is provided with a first input end, a second input end and an output end; the dispersion phase input capillary penetrates through a first input end and an output end of the tee joint, one end of the dispersion phase input capillary is conical, and the conical end is positioned on one side of the output end; one end of the liquid drop output capillary is sleeved with the conical end of the disperse phase input capillary, and a gap is formed at the joint of the liquid drop output capillary and the disperse phase input capillary; a connecting capillary tube is sleeved outside the joint, one end of the connecting capillary tube is inserted into the output end of the tee joint and communicated with the interior of the tee joint, and the other end of the connecting capillary tube is hermetically connected with the outer wall of the liquid drop output capillary tube; one end of the continuous phase input capillary tube is inserted into the second input end of the tee joint and is communicated with the interior of the tee joint.
The disperse phase input capillary, the connecting capillary and the continuous phase input capillary are respectively connected with the first input end, the second input end and the output end of the tee joint in a sealing way.
The tee joint is in a T-shaped structure, and a first input end, a second input end and an output end of the tee joint are respectively provided with a connector for inserting a dispersed phase input capillary tube, a continuous phase input capillary tube and a connecting capillary tube.
The tee joint and the joint are made of PEEK materials.
The other end of the connecting capillary tube and the outer wall of the liquid drop output capillary tube are sealed through thermoplastic glue.
A single-particle plunger preparation method based on a capillary droplet microfluidic device comprises the following steps: respectively introducing the dispersed phase and the continuous phase into a capillary droplet microfluidic device by adopting a liquid propelling pump, controlling the flow rate of the dispersed phase and the continuous phase, collecting the generated droplets into a container through a droplet output capillary, performing polycondensation reaction on the collected droplets to solidify the droplets into microspheres, and cleaning, drying and calcining the microspheres.
The dispersed phase adopts a silica gel system; the continuous phase employs an organic solvent system immiscible with the dispersed phase, such as an alkane solvent such as n-hexane.
The preparation method of the silica gel system comprises the following steps: adding tetramethoxysiloxane into polyethylene glycol and acetic acid, hydrolyzing to obtain transparent solution, and dissolving in ammonia water to obtain dispersed phase.
The temperature of the polycondensation reaction is 60-90 ℃; the drying is vacuum drying, and the drying temperature is 30-60 ℃.
The calcination adopts programmed calcination, and the calcination conditions are as follows: firstly, heating to 80-100 ℃, preserving heat for 0.5-2 h, then heating to 170-250 ℃, preserving heat for 4-8 h, and finally naturally cooling.
Compared with the prior art, the utility model discloses technical scheme obtains beneficial effect is:
1. the utility model has simple structure, easy construction and operation and low manufacturing cost, the disperse phase input capillary and the continuous phase input capillary form a coaxial flow structure for generating liquid drops, the liquid drops with different sizes can be generated by adjusting the flow speed of the disperse phase and the continuous phase and the inner diameter of the liquid drop output capillary, and then the generated liquid drops are solidified into microspheres, thereby preparing the silicon dioxide microspheres with various particle diameters;
2. in the method for preparing the microspheres, the silica gel system is used as a disperse phase for generating liquid drops, the liquid drops are solidified into spheres based on sol-gel chemical reaction, the prepared silica microsphere material has micron-sized flowing holes, the hole structures are mutually crosslinked, and the microspheres have good permeability and high mechanical strength;
3. adopt the utility model discloses the silica microsphere material of preparation has high monodispersity, high mechanical strength and good permeability, can carry out the enrichment purification that the preparation of different internal diameter capillary chromatography packed columns is used for liquid chromatography and sample as single granule plunger, and preparation method is easy and simple to handle moreover, and stability is good.
Drawings
Fig. 1 is a schematic structural view of the present invention;
FIG. 2 is an electron micrograph of silica microspheres having an average particle size of 64.09 μm;
FIG. 3 is an electron micrograph of silica microspheres having an average particle size of 87.58 μm;
FIG. 4 is an electron micrograph of silica microspheres having an average particle size of 108.59 μm;
FIG. 5 is an electron micrograph of silica microspheres having an average particle size of 127.22 μm;
FIG. 6 is an electron micrograph of a single silica microsphere of FIG. 4;
FIG. 7 is an electron micrograph of the pore structure of silica microspheres;
FIG. 8 is a graph showing the results of chromatographic separation.
Reference numerals: the device comprises a dispersed phase input capillary 1, a continuous phase input capillary 2, a connecting capillary 3, a liquid drop output capillary 4, connectors 5, 6 and 7 and a tee joint 8.
Detailed Description
In order to make the technical problem, technical solution and beneficial effects to be solved by the present invention clearer and more obvious, the following description is made in detail with reference to the accompanying drawings and embodiments.
Example 1
As shown in fig. 1, embodiment 1 of the present invention includes a dispersed phase input capillary 1, a continuous phase input capillary 2, a droplet output capillary 4, a connecting capillary 3, and a tee joint 8;
the tee joint 8 is provided with a first input end, a second input end and an output end; the dispersion phase input capillary 1 penetrates through a first input end and an output end of the tee joint 8, one end of the dispersion phase input capillary 1 is in a conical shape, and the conical end is positioned on one side of the output end; one end of the liquid drop output capillary 4 is sleeved with the conical end of the disperse phase input capillary 1, and a gap is formed at the joint of the liquid drop output capillary 4 and the disperse phase input capillary 1; a connecting capillary tube 3 is sleeved outside the joint, one end of the connecting capillary tube 3 is inserted into the output end of the tee joint 8 and communicated with the interior of the tee joint 8, and the other end of the connecting capillary tube 3 is hermetically connected with the outer wall of the liquid drop output capillary tube 4; one end of the continuous phase input capillary tube 2 is inserted into the second input end of the tee joint 8 and is communicated with the interior of the tee joint 8; three liquid channels of a first input end, a second input end and an output end of the tee joint 8 are communicated with one another, and the dispersed phase input capillary 1 and the continuous phase input capillary 2 form a coaxial flow structure for generating liquid drops.
The disperse phase input capillary 1, the connecting capillary 3 and the continuous phase input capillary 2 are respectively connected with the first input end, the second input end and the output end of the tee joint 8 in a sealing way.
The tee joint 8 is in a T-shaped structure, and the first input end, the second input end and the output end of the tee joint 8 are respectively provided with connectors 5, 6 and 7 for inserting the disperse phase input capillary 1, the connecting capillary 3 and the continuous phase input capillary 2; and the tee joint 8 and the joints 5, 6 and 7 are made of PEEK materials.
In this embodiment 1, the other end of the connecting capillary 3 and the outer wall of the droplet output capillary 4 are sealed by thermoplastic.
The internal diameters of the dispersed phase input capillary 1, the continuous phase input capillary 2, and the droplet output capillary 4 may be selected according to the size of the target droplet and microsphere.
Example 2
Example 2 is a detailed description of the preparation of monodisperse silica microspheres having a particle size of 108 μm.
1. Preparation of the dispersed phase
And (3) putting 320 mu L of tetramethoxysiloxane into a round-bottom flask, adding 200mg of polyethylene glycol and 2mL of acetic acid, stirring and hydrolyzing until the solution is clear, then putting 1mL of hydrolysate into a centrifuge tube, adding 40mg of ammonia water, and performing ultrasonic treatment until the hydrolysate is completely dissolved to complete preparation of the dispersed phase.
2. Droplet preparation
Sucking the prepared dispersed phase into a 1mL disposable syringe, connecting a needle with a dispersed phase input capillary 1 through a PTFE sleeve, wherein the inner diameter of the dispersed phase input capillary 1 is 100 mu m, the outer diameter of the dispersed phase input capillary 1 is 365 mu m, and the inner diameter of the conical end of the dispersed phase input capillary 1 is 30 mu m; n-hexane is sucked in a 2mL disposable syringe, a needle is connected with a continuous phase input capillary 2 through a PTFE sleeve, the inner diameter of the continuous phase input capillary 2 is 100 mu m, and the outer diameter is 365 mu m; placing two disposable syringes on a Harvard injection pump, and introducing a dispersed phase and a continuous phase into a capillary droplet microfluidic device under the driving of the injection pump, wherein the flow rate of the dispersed phase is 0.15 muL/min, and the flow rate of the continuous phase is 90 muL/min; the generated droplets were collected in a 4mL centrifuge tube through a droplet output capillary 4.
3. Solidification, cleaning and drying of droplets
The 4mL centrifuge tube with the collected droplets was transferred to an oven and subjected to polycondensation reaction at 80 ℃ for 12 hours, and the centrifuge tube was put into the oven and vacuum-dried at 45 ℃ for 10 hours.
4. Programmed calcination of microspheres
Pouring the cleaned and dried silica microspheres into a crucible, and placing the crucible in an oven for programmed calcination, wherein the procedure is as follows: raising the temperature to 100 ℃, preserving the heat for 1h, raising the temperature to 200 ℃, preserving the heat for 6h, and finally naturally cooling.
The particle size and pore structure of the microspheres were characterized by scanning electron microscopy, as shown in fig. 4 and table 1, the average particle size of the silica microspheres was 108 μm, the coefficient of variation CV of the particle size was 3.62%, and the standard deviation was 0.01 μm; as shown in fig. 6 to 7, the silica microspheres have a cross-linked pore structure and have perfusion pores of micron order.
5. Capillary column preparation
The prepared silicon dioxide microspheres are used as single-particle plungers, a homogenization filling method is adopted to fill particles with the inner diameter of 100 mu m, the outer diameter of 365 mu m and the length of 15cm into a capillary column, and the filler is 5 mu m C18 filler; and then carrying out chromatographic performance characterization on the prepared capillary column. Chromatographic conditions are as follows: the sample is a standard benzene series (a mixture of thiourea, toluene, ethylbenzene, propylbenzene and butylbenzene), the sample amount is 4nL, the mobile phase is a 60% acetonitrile solution, the flow rate is 200nL/min, and the ultraviolet detection wavelength is 214 nm; the chromatographic separation results are shown in fig. 8, which shows that the particle-packed capillary column prepared in this example has better chromatographic separation performance.
TABLE 1
| Reference numerals | Average particle diameter (μm) | Coefficient of variation CV of particle diameter | Standard deviation (mum) |
| 2 | 64.09 | 2.80％ | 1.76 |
| 3 | 87.58 | 2.02％ | 1.77 |
| 4 | 108.59 | 3.62％ | 0.01 |
| 5 | 127.22 | 4.86％ | 0.01 |
According to different requirements, the utility model can generate liquid drops with different sizes by adjusting the flow rates of the dispersion phase and the continuous phase and the inner diameter of the liquid drop output capillary, thereby preparing the high monodisperse silicon dioxide microspheres with various particle diameters; as shown in table 1, fig. 2, fig. 3 and fig. 5, the silica microspheres prepared by the present invention have average particle sizes of 64, 87 and 127 μm, respectively, and have high dispersibility and small standard deviation, and the prepared silica microspheres with different particle sizes can be filled into a required capillary column.
Claims (5)
1. A capillary droplet microfluidic device, characterized by: comprises a dispersed phase input capillary, a continuous phase input capillary, a liquid drop output capillary, a connecting capillary and a tee joint; the tee joint is provided with a first input end, a second input end and an output end; the dispersion phase input capillary penetrates through a first input end and an output end of the tee joint, one end of the dispersion phase input capillary is conical, and the conical end is positioned on one side of the output end; one end of the liquid drop output capillary is sleeved with the conical end of the disperse phase input capillary, and a gap is formed at the joint of the liquid drop output capillary and the disperse phase input capillary; a connecting capillary tube is sleeved outside the joint, one end of the connecting capillary tube is inserted into the output end of the tee joint and communicated with the interior of the tee joint, and the other end of the connecting capillary tube is hermetically connected with the outer wall of the liquid drop output capillary tube; one end of the continuous phase input capillary tube is inserted into the second input end of the tee joint and is communicated with the interior of the tee joint.
2. The capillary droplet microfluidic device of claim 1, wherein: the disperse phase input capillary, the connecting capillary and the continuous phase input capillary are respectively connected with the first input end, the second input end and the output end of the tee joint in a sealing way.
3. The capillary droplet microfluidic device of claim 1, wherein: the tee joint is in a T-shaped structure, and a first input end, a second input end and an output end of the tee joint are respectively provided with a connector for inserting a dispersed phase input capillary tube, a continuous phase input capillary tube and a connecting capillary tube.
4. A capillary droplet microfluidic device according to claim 3 wherein: the tee joint and the joint are made of PEEK materials.
5. The capillary droplet microfluidic device of claim 1, wherein: the other end of the connecting capillary tube and the outer wall of the liquid drop output capillary tube are sealed through thermoplastic glue.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110433882A (en) * | 2019-09-05 | 2019-11-12 | 厦门大学 | A kind of capillary drop micro fluidic device and individual particle plunger preparation method |
| CN113019348A (en) * | 2021-03-15 | 2021-06-25 | 厦门大学 | Method for preparing chromatographic packing based on capillary droplet microfluidics |
| CN113797986A (en) * | 2021-10-11 | 2021-12-17 | 北京永康乐业科技发展有限公司 | Micro-fluidic chip capable of finely adjusting coaxial arrangement of capillaries |
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2019
- 2019-09-05 CN CN201921473724.2U patent/CN211274688U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110433882A (en) * | 2019-09-05 | 2019-11-12 | 厦门大学 | A kind of capillary drop micro fluidic device and individual particle plunger preparation method |
| CN113019348A (en) * | 2021-03-15 | 2021-06-25 | 厦门大学 | Method for preparing chromatographic packing based on capillary droplet microfluidics |
| CN113019348B (en) * | 2021-03-15 | 2022-04-26 | 厦门大学 | Method for preparing chromatographic packing based on capillary droplet microfluidics |
| CN113797986A (en) * | 2021-10-11 | 2021-12-17 | 北京永康乐业科技发展有限公司 | Micro-fluidic chip capable of finely adjusting coaxial arrangement of capillaries |
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