CN111595843A - Preparation method and application of viscous sampling detection paper for arrayed colorimetric analysis - Google Patents
Preparation method and application of viscous sampling detection paper for arrayed colorimetric analysis Download PDFInfo
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Abstract
The invention relates to a preparation method and application of viscosity sampling detection paper for arrayed colorimetric analysis. The method has the advantages of simple processing, easily obtained manufacturing tools, and mass production and preparation. The viscous sampling detection paper for arrayed colorimetric analysis, which is obtained by the method, provides a colorimetric unit environment with multiple regions, independent preservation, reaction and display in the aspects of powder sample collection, mixed sample analysis, sample type identification and the like, so that the aim of one-paper multi-mode detection is fulfilled, the complex operation problems of repeated sample collection by using multiple pieces of filter paper and repeated reagent dropping detection in the prior art are solved, one piece of detection paper is used, and a complete detection environment is provided. The back of the detection paper contains a waterproof layer, so that the detection reagent is prevented from permeating the detection paper to cause pollution.
Description
Technical Field
The invention relates to a paper-based microfluidic chip processing technology, in particular to a method for realizing the graphic partition array of a paper-based microfluidic chip by impregnating and curing polydimethylsiloxane with hydrophobic property on a paper base.
Background
Microfluidic Chips (Microfluidic Analysis Chips) refer to the control of micro-flow of fluids (10) in channels of a few microns to a few hundred microns-9-10-18L) or a detection reagent. At the end of the 70's of the 20 th century, Terry et al realized the construction of a miniaturized gas chromatograph on a silicon wafer and successfully performed the effect of component analysis of mixed gas. However, the preparation of the microfluidic chip using silicon material, quartz and glass material, and high molecular polymer as substrate material is not only complicated in operation and high in cost, but also difficult to popularize. Since 2007, Martinez et al proposed that paper-based microfluidic chips were used to detect glucose and protein, and the paper-based microfluidic technology was rapidly developed. Because the paper material is cheap and easy to obtain, the manufacturing technology can use means such as cutting, masking, printing, manual writing/stamping, printing and dyeing and the like, and the pattern can be drawn by self definition. The basic working principle of the paper-based microfluidic chip is to manufacture a self-defined hydrophobic boundary on a hydrophilic paper base, and the common means mainly comprise: physical barrier methods, physical deposition methods, and chemical modification methods. The physical barrier method is to impregnate hydrophobic substances such as polydimethylsiloxane and the like into paper fibers, and to block and fill gaps in the paper fibers so as to achieve the purpose of hydrophobicity; the physical deposition method is to deposit hydrophobic substances such as wax, polystyrene and the like on the fiber surface of paper, and to enable liquid to permeate into a hydrophilic area by reducing the surface energy of the paper so as to achieve the hydrophobic effect; the chemical modification method is to introduce hydrophobic groups into cellulose molecular chains by using reagents capable of reacting with-OH hydrophilic groups such as alkyl ketene dimer and the like, so that paper forms hydrophobic boundary to achieve hydrophobicityThe purpose is.
Polydimethylsiloxane (PDMS), also known as dimethicone, is a hydrophobic class of silicone materials. Dimethyl silicone oil in a chemical state of polydimethylsiloxane is colorless or light yellow liquid, is tasteless and high in transparency, has the characteristics of heat resistance, cold resistance, small viscosity change along with temperature, waterproofness, small surface tension, thermal conductivity, light transmittance of 100% and the like, and has good mechanical property, optical property, chemical stability and biocompatibility due to the characteristics, and is simple to process and low in price. In conclusion, the polydimethylsiloxane becomes a microfluidic chip material widely applied, but the polydimethylsiloxane is easy to deform, is difficult to maintain a stable structure, and is difficult to load other reagents. But the paper base and the polydimethylsiloxane are combined for use, so that good advantage complementation is achieved, the fibers in the paper base have the capillary action and can drive liquid to flow, and the paper base also has a large specific surface area and a strong adsorption effect. The polydimethylsiloxane and the paper base are combined by a hydrophobic means, so that the paper chip has a detection device with the functions of penetration depth, flow direction, partition planning and integrated sample preparation, sample treatment and sample analysis of a sample detection box. However, the existing paper base design mainly faces the sampling detection of trace liquid, the sampling detection of powder on the complex surface is still limited, and the design of the paper base for simultaneously detecting multiple components by aiming at multiple component samples and single test paper is still solved.
The publication number is: CN 104437689 a discloses a method for manufacturing paper-based microfluidic chip based on photosensitive stamp printing, which is a method for manufacturing paper-based microfluidic chip by using photosensitive stamp printing, and uses the current mature photosensitive stamp as the core template of the paper-based microfluidic chip.
The publication number is: CN 103394384 a discloses a paper-based microfluidic chip and a preparation method thereof, which is a paper-based microfluidic chip comprising a paper-based chip and a paper-based negative, wherein the paper-based negative is bonded at the bottom of the paper-based chip, and then is subjected to cross-linking curing treatment by heating and/or ultraviolet irradiation. The invention also discloses a three-dimensional paper-based microfluidic chip which is formed by stretching or folding the paper-based microfluidic chip.
The publication number is: CN 106040324A discloses a method for preparing a fluorine material paper-based microfluidic chip based on a screen printing method, which is a paper-based microfluidic chip prepared by using a fluorine material as a hydrophobic and oleophobic material and having a hydrophilic channel and a hydrophobic cofferdam on a paper substrate.
The publication number is: CN 104677896A discloses 'preparation and application of a paper-based microfluidic chip for colorimetric analysis', which is to attach a hydrophilic channel on a hydrophobic substrate, wherein the hydrophilic channel is obtained by printing a channel pattern on filter paper and then shearing the filter paper; the hydrophobic substrate is obtained by treating filter paper with n-hexane solution of methyltrichlorosilane and octadecyltrichlorosilane.
The method modifies the paper base by a physical barrier method, a physical deposition method and a chemical modification method aiming at the hydrophilicity of the paper, so that the paper base has both hydrophilicity and hydrophobicity, however, the method is mainly used for shaping or constructing a microfluidic linear, spiral or three-dimensional structure channel. Because the polydimethylsiloxane has stable performance and simple crosslinking curing mode, the industrial rapid filter paper has larger aperture and stronger capillary action. The handheld convenience of actual user is considered, the paper base design protection layer is convenient to hold, pollution is avoided, and independent design of handheld equipment is not needed. The invention has the advantages of cheap processing materials, simple process, easy equipment acquisition and the like by considering the aspects of cost, batch, operation process complexity and the like. The paper base prepared by the method can be used for detection of various water-soluble and organic reagents and the like.
Disclosure of Invention
The invention aims to provide a preparation method and application of viscosity sampling detection paper for arrayed colorimetric analysis, wherein the detection paper is composed of release paper, a paper base, water-based pressure-sensitive adhesive, a hydrophilic unit, a hydrophobic unit and a waterproof layer. The method has the advantages of simple processing, easily obtained manufacturing tools, and mass production and preparation. The viscous sampling detection paper for arrayed colorimetric analysis, which is obtained by the method, provides a colorimetric unit environment with multiple regions, independent preservation, reaction and display in the aspects of powder sample collection, mixed sample analysis, sample type identification and the like, and achieves the aim of one-paper multi-mode detection. The paper base can be applied to products such as explosives and the like which are collected by mixed samples and use a chemical colorimetric detection technology. The problem of use many filter papers among the prior art to gather the sample repeatedly, the loaded down with trivial details operation that the dropwise add reagent detected many times is overcome, accomplishes to use a detection paper, provides complete testing environment. The back of the detection paper contains a waterproof layer, so that the reagent is retained on the detection paper, and the detection reagent is prevented from permeating the detection paper to cause pollution.
The invention relates to a preparation method of sticky sampling detection paper for arrayed colorimetric analysis, which comprises the following steps of:
a. designing a hydrophilic and hydrophobic pattern of the microfluidic chip of the paper base (2), and preparing a first screen printing plate; designing a pattern for printing the water-based pressure-sensitive adhesive (3), and preparing a second screen printing plate;
b. coating the back of the paper base (2) by using a film coating machine to form a waterproof layer (6), wherein the paper base (2) is industrial fast filter paper, medium-speed filter paper, slow-speed filter paper or copy paper, the average thickness is 0.18mm, and the average pore diameter is 100 mu m; the film is made of matte PVC material, the thickness is 0.09mm, and release paper (1) is attached to the surface of the paper base (2);
c. preparing a mixture of a prepolymer of polydimethylsiloxane and a curing agent according to a mass ratio of 10:1 at room temperature;
d. c, printing the polydimethylsiloxane mixture prepared in the step c on the surface of the paper base (2) by using the first screen printing plate manufactured in the step a by using a screen printing machine, wherein hydrophobic units (6) are formed on the surface of the paper base (2) through the polydimethylsiloxane mixture of the screen printing plate, and hydrophilic units (4) are formed on the polydimethylsiloxane mixture which does not penetrate through the screen printing plate;
e. d, placing the paper base (2) printed in the step d into an oven, and curing at the temperature of 100 ℃ and 150 ℃ for 40 min;
f. c, printing the water-based pressure-sensitive adhesive (3) on the surface of the paper base (2) by using the second screen printing plate manufactured in the step a through the screen printing machine on the paper base (2) cured in the step e, and drying for 30 minutes at the temperature of 40-60 ℃ through an oven;
g. and f, covering the release paper (1) on the surface of the paper base (2) dried in the step f, and cutting by using a paper cutter to obtain the viscous sampling detection paper for the arrayed colorimetric analysis.
In the step a, the first screen printing plate is 300 meshes and has the diameter of about 50 mu m; the second screen printing plate is 150 meshes and has the diameter of about 100 mu m;
the water-based pressure-sensitive adhesive in the step f is 3M SP-7533 silk screen printing adhesive, and the water adding proportion is 5% by mass.
The release paper in the step g is 65g of glassine release paper.
The application of the sticky sampling detection paper for arrayed colorimetric analysis obtained by the method in collecting solid explosives or drugs.
Compared with the prior art, the preparation method of the viscous sampling detection paper for arrayed colorimetric analysis has the following specific effects:
by combining the paper base and the polydimethylsiloxane, the hydrophilic-hydrophobic water separation and reagent loading capacity are achieved by utilizing the characteristics of flexibility and adsorbability of the paper, the capillary action of an internal porous fiber structure, the hydrophobicity, the heat resistance, the chemical stability and the like of the polydimethylsiloxane. The paper base can customize a graphical interface, a multi-area independent detection partition which exists simultaneously is provided, and a colorimetric analysis environment is provided for the loaded reagent in an independent background. The method can realize batch detection of paper base production by using simple screen printing tools and constant temperature equipment, and has the advantages of low raw material cost, low equipment cost, low learning cost, good stability, batch applicability and the like.
Drawings
FIG. 1 is a schematic structural diagram of the present invention, wherein 1, release paper, 2, paper base, 3, aqueous pressure sensitive adhesive, 4, hydrophilic unit, 5, hydrophobic unit and 6, and waterproof layer;
FIG. 2 is a diagram of an embodiment of the present invention, wherein in A, 1 is a release paper, 6 is a waterproof layer; b, 3, a water-based pressure-sensitive adhesive, 4, a hydrophilic unit, 5 and a hydrophobic unit;
FIG. 3 is a diagram of the paper-based surface printing screen printing glue and effect of the present invention, wherein A is a schematic diagram of the design of the screen printing glue pattern; b is a purple powder effect picture collected after paper-based printing screen printing glue; c, after a paper-based finished product collects a sample and reacts with a reagent for detection, the brownish red reaction characteristic of the position of the printing adhesive tape is obvious.
Detailed Description
The invention is explained in more detail below with reference to the figures and examples.
Example 1
Using industrial quick filter paper as paper base:
a. designing a hydrophilic and hydrophobic pattern of the paper base 2 industrial rapid filter paper microfluidic chip, and preparing a first screen printing plate with a mesh size of 300 and a diameter of about 50 mu m; designing a pattern for printing the water-based pressure-sensitive adhesive 3, and preparing a second screen printing plate with 150 meshes and the diameter of about 100 mu m;
b. using a film laminating machine to carry out film laminating treatment on the back of industrial rapid filter paper with the average thickness of 0.18mm and the average pore diameter of 100 mu m to form a waterproof layer 5, wherein the film is made of matte PVC material and has the thickness of 0.09mm, and attaching release paper (1) to the surface of the paper base (2);
c. preparing a mixture of a prepolymer of polydimethylsiloxane and a curing agent according to a mass ratio of 10:1 at room temperature;
d. b, printing the polydimethylsiloxane mixture prepared in the step c on the surface of the industrial quick filter paper of the paper base 2 by using the first screen printing screen plate manufactured in the step a by using a screen printing machine, wherein the hydrophobic unit 6 is formed on the surface of the industrial quick filter paper of the paper base 2 through the polydimethylsiloxane mixture of the screen printing screen plate, and the hydrophilic unit 4 is formed on the surface of the polydimethylsiloxane mixture which does not pass through the screen printing screen plate;
e. d, putting the printed industrial quick filter paper of the paper base 2 in the step d into an oven, and curing at 100 ℃ for 40 min;
f. c, printing the water-based pressure-sensitive adhesive 3 on the surface of the paper base 2 industrial quick filter paper by using the cured paper base 2 industrial quick filter paper prepared in the step e through a second screen printing plate manufactured in the step a by using a screen printing machine, and drying for 30 minutes at the temperature of 40 ℃ of an oven, wherein the water-based pressure-sensitive adhesive is 3M SP-7533 screen printing adhesive and is mixed with water in a proportion of 5% by mass;
g. and f, covering 65g of glassine release paper (1) on the surface of the industrial quick filter paper of the paper base 2 dried in the step f, and cutting by using a paper cutter to obtain the viscous sampling detection paper for the arrayed colorimetric analysis.
Example 2
Using industrial medium speed filter paper as paper base:
a. designing hydrophilic and hydrophobic patterns of the paper base 2 industrial medium-speed filter paper microfluidic chip, and preparing a first screen printing plate with a mesh size of 300 and a diameter of about 50 mu m; designing a pattern for printing the water-based pressure-sensitive adhesive 3, and preparing a second screen printing plate with 150 meshes and the diameter of about 100 mu m;
b. coating the back of the industrial medium-speed filter paper with the average thickness of 0.18mm and the average pore diameter of 100 mu m by using a laminating machine to form a waterproof layer 5, wherein the laminating film is made of matte PVC material and has the thickness of 0.09mm, and attaching release paper (1) to the surface of the paper base (2);
c. preparing a mixture of a prepolymer of polydimethylsiloxane and a curing agent according to a mass ratio of 10:1 at room temperature;
d. b, printing the polydimethylsiloxane mixture prepared in the step c to the surface of the industrial medium-speed filter paper of the paper base 2 by using the first screen printing screen prepared in the step a by using a screen printing machine, wherein the hydrophobic unit 6 is formed on the surface of the industrial medium-speed filter paper of the paper base 2 by penetrating through the polydimethylsiloxane mixture of the screen printing screen, and the hydrophilic unit 4 is formed on the polydimethylsiloxane mixture which does not penetrate through the screen printing screen;
e. d, placing the paper base 2 printed in the step d as industrial medium-speed filter paper into an oven, and curing at 120 ℃ for 40 min;
f. c, printing the water-based pressure-sensitive adhesive 3 on the surface of the industrial medium-speed filter paper of the paper base 2 by using the cured paper base 2 in the step e and the second screen printing plate manufactured in the step a by using a screen printing machine, and drying for 30 minutes at the temperature of 50 ℃ of an oven, wherein the water-based pressure-sensitive adhesive is 3M SP-7533 screen printing adhesive and is mixed with water in a proportion of 5% by mass;
g. and f, covering 65g of glassine release paper 1 on the surface of the industrial medium-speed filter paper of the paper base 2 dried in the step f, and cutting by using a paper cutter to obtain the viscous sampling detection paper for array colorimetric analysis.
Example 3
Using copy paper as paper base:
a. designing a hydrophilic and hydrophobic pattern of a paper base 2 copy paper microfluidic chip, and preparing a first screen printing plate with a mesh size of 300 and a diameter of about 50 mu m; designing a pattern for printing the water-based pressure-sensitive adhesive 3, and preparing a second screen printing plate with 150 meshes and the diameter of about 100 mu m;
b. coating the back of copy paper with the average thickness of 0.18mm and the average pore diameter of 100 mu m on a paper base 2 by using a film coating machine to form a waterproof layer 5, wherein the film is made of matte PVC material and has the thickness of 0.09mm, and attaching release paper (1) on the surface of the paper base (2);
c. preparing a mixture of a prepolymer of polydimethylsiloxane and a curing agent according to a mass ratio of 10:1 at room temperature;
d. c, printing the polydimethylsiloxane mixture prepared in the step c on the surface of the copy paper of the paper base 2 by using the first screen printing screen plate manufactured in the step a by using a screen printing machine, wherein the hydrophobic units 6 are formed on the surface of the copy paper of the paper base 2 through the polydimethylsiloxane mixture of the screen printing screen plate, and the hydrophilic units 4 are formed on the surface of the polydimethylsiloxane mixture which does not penetrate through the screen printing screen plate;
e. d, placing the copy paper of the paper base 2 printed in the step d into an oven, and curing at 150 ℃ for 40 min;
f. c, printing the water-based pressure-sensitive adhesive 3 on the surface of the paper base 2 copy paper by using the second screen printing screen plate manufactured in the step a by using the screen printing machine on the paper base 2 copy paper cured in the step e, and drying for 30 minutes at the temperature of 60 ℃ by using an oven, wherein the water-based pressure-sensitive adhesive is 3M SP-7533 screen printing adhesive and is mixed with water in a proportion of 5% by mass;
g. and f, covering 65g of glassine release paper 1 on the surface of the paper base 2 copy paper dried in the step f, and cutting by using a paper cutter to obtain the adhesive sampling detection paper for array colorimetric analysis.
Example 4
The sampling test paper obtained in any one of the examples 1 to 3 is used in an XJ-TW-001 explosive development reagent box:
tearing the release paper 1 attached to the surface of the obtained sampling paper, and wiping or sticking the explosive or raw material powder sample thereof by using the side with the viscosity of the detection paper base (taking a chlorate powder sample as an example);
after the acquisition is finished, placing the paper base surface of the acquired sample of the detection paper upwards, and dropwise adding and judging the reagents in the XJ-TW-001 explosive display reagent box according to the instructions in sequence, wherein the detection reagents No. 1-7 are all commercially available products;
dripping the No. 1 detection reagent to the No. 1 area of the detection paper, wherein the No. 1 detection reagent does not develop color, and removing substances detected by the No. 1 detection reagent;
dripping No. 1+2 detection reagent to the No. 1+2 area of the detection paper, not developing color, and removing substances detected by the No. 1+2 reagent;
dripping No. 3 detection reagent to the No. 3 area of the detection paper, not developing color, and removing the substance detected by the No. 3 reagent;
dripping No. 4 detection reagent to the No. 4 area of the detection paper, and removing substances detected by the No. 4 reagent without color development;
dripping No. 5 detection reagent to the No. 5 area of the detection paper, wherein the detection paper does not develop color, and removing substances detected by the No. 5 reagent;
dripping No. 6 detection reagent to the No. 6 area of the detection paper, not developing color, and removing the substance detected by the No. 6 reagent;
and (4) dropwise adding a No. 7 detection reagent to the No. 7 area of the detection paper, displaying purple red, and judging that the collected sample contains explosive component chlorate or perchlorate.
Example 5
The sampling detection paper obtained in any one of the embodiments 1 to 3 is used in a ZK-ONSITE A-003 drug rapid detection box:
tearing the release paper 1 attached to the surface of the sampling paper, and wiping or sticking the drug powder sample by using the sticky side of the detection paper base (taking a hemp powder sample as an example);
after the collection is finished, placing the paper base face of a sample collected by the detection paper upwards, and dropwise adding and judging the reagents in the ZK-ONSITE A-003 drug rapid detection box according to the instructions in sequence, wherein the detection reagents No. 1-6 are all commercially available products;
dripping the No. 1 detection reagent to the No. 1 area of the detection paper, wherein the No. 1 detection reagent does not develop color, and removing substances detected by the No. 1 detection reagent;
dripping No. 2 detection reagent to the No. 2 area of the detection paper, not developing color, and removing the substance detected by the No. 2 reagent;
dripping No. 3+5 detection reagent to No. 3+5 area of the detection paper, not developing color, and removing substances detected by the No. 3+5 reagent;
dripping No. 4+5 detection reagent to No. 4+5 area of the detection paper, displaying reddish brown, and judging that the collected sample contains hemp;
and dripping No. 6 detection reagent to the No. 6 area of the detection paper, not developing color, and removing substances detected by the No. 6 reagent.
The adhesive sampling detection paper for the arrayed colorimetric analysis, which is obtained by the method, has the advantages of clear pattern, neat edge, strong adhesion, convenience in holding and storage. The invention provides a multi-region, independent preservation, reaction and display colorimetric unit environment in powder sample collection, mixed sample analysis, sample type identification and the like. The device can be used for on-site rapid detection of single and mixed samples and products. After a piece of detection paper is used for collecting a sample once, complete investigation and judgment can be made after a dripping test. The waterproof layer on the back of the detection paper keeps the sample and the detection reagent on the detection paper, and the reagent permeates and flows to cause pollution.
Claims (5)
1. The preparation method of the sticky sampling detection paper for the arrayed colorimetric analysis is characterized in that the detection paper consists of release paper (1), a paper base (2), water-based pressure-sensitive adhesive (3), a hydrophilic unit (4), a hydrophobic unit (5) and a waterproof layer (6), and the specific operation is carried out according to the following steps:
a. designing a hydrophilic and hydrophobic pattern of the microfluidic chip of the paper base (2), and preparing a first screen printing plate; designing a pattern for printing the water-based pressure-sensitive adhesive (3), and preparing a second screen printing plate;
b. coating the back of the paper base (2) by using a film coating machine to form a waterproof layer (6), wherein the paper base (2) is industrial fast filter paper, medium-speed filter paper, slow-speed filter paper or copy paper, the average thickness is 0.18mm, and the average pore diameter is 100 mu m; the film is made of matte PVC material, the thickness is 0.09mm, and release paper (1) is attached to the surface of the paper base (2);
c. preparing a mixture of a prepolymer of polydimethylsiloxane and a curing agent according to a mass ratio of 10:1 at room temperature;
d. c, printing the polydimethylsiloxane mixture prepared in the step c on the surface of the paper base (2) by using the first screen printing plate manufactured in the step a by using a screen printing machine, wherein hydrophobic units (6) are formed on the surface of the paper base (2) through the polydimethylsiloxane mixture of the screen printing plate, and hydrophilic units (4) are formed on the polydimethylsiloxane mixture which does not penetrate through the screen printing plate;
e. d, placing the paper base (2) printed in the step d into an oven, and curing at the temperature of 100 ℃ and 150 ℃ for 40 min;
f. c, printing the water-based pressure-sensitive adhesive (3) on the surface of the paper base (2) by using the second screen printing plate manufactured in the step a through the screen printing machine on the paper base (2) cured in the step e, and drying for 30 minutes at the temperature of 40-60 ℃ through an oven;
g. and f, covering the release paper (1) on the surface of the paper base (2) dried in the step f, and cutting by using a paper cutter to obtain the viscous sampling detection paper for the arrayed colorimetric analysis.
2. The method for preparing a sticky sampling test paper for arrayed colorimetric analysis according to claim 1, wherein the first screen printing plate in the step a is 300 mesh and has a diameter of about 50 μm; the second screen printing plate was 150 mesh and had a diameter of about 100 μm.
3. The method for preparing the sticky sampling test paper for the arrayed colorimetric analysis of claim 1, wherein the aqueous pressure-sensitive adhesive in the step f is 3M SP-7533 silk screen printing adhesive, and the water adding proportion is 5% by mass.
4. The method of claim 1, wherein the release paper in step g is 65g glassine release paper.
5. Use of a sticky sampling test paper for arrayed colorimetric analysis obtained according to the method of claim 1 for collecting solid explosives or drugs.
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