CN110470609B - Complex water body multi-parameter quick detection equipment and method based on microfluidic technology - Google Patents

Complex water body multi-parameter quick detection equipment and method based on microfluidic technology Download PDF

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CN110470609B
CN110470609B CN201810449086.4A CN201810449086A CN110470609B CN 110470609 B CN110470609 B CN 110470609B CN 201810449086 A CN201810449086 A CN 201810449086A CN 110470609 B CN110470609 B CN 110470609B
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chip
detection
sample
water body
component
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CN110470609A (en
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孙冰
姜慧芸
王林
朱红伟
石宁
徐伟
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China Petroleum and Chemical Corp
Sinopec Safety Engineering Research Institute Co Ltd
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China Petroleum and Chemical Corp
Sinopec Safety Engineering Research Institute Co Ltd
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
    • B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65—Raman scattering
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01L2200/00—Solutions for specific problems relating to chemical or physical laboratory apparatus
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    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/08—Geometry, shape and general structure
    • B01L2300/0803—Disc shape
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/08—Geometry, shape and general structure
    • B01L2300/0809—Geometry, shape and general structure rectangular shaped
    • B01L2300/0829—Multi-well plates; Microtitration plates

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Abstract

The invention relates to the technical field of microfluidics and discloses complex water body multi-parameter quick detection equipment and a complex water body multi-parameter quick detection method based on a microfluidic technology. The complex water body multi-parameter quick detection device comprises a chip and a detection device; wherein the chip comprises a reaction tank for sample reaction; the detection device is used for detecting signals of the sample in the reaction tank. The complex water body multi-parameter rapid detection equipment and the detection method have the advantages of high detection speed and high flux, and have good processing capacity for complex samples.

Description

Complex water body multi-parameter quick detection equipment and method based on microfluidic technology
Technical Field
The invention relates to the technical field of microfluidics, in particular to complex water body multi-parameter quick detection equipment and a complex water body multi-parameter quick detection method based on a microfluidic technology.
Background
The world economy and industry development brings great convenience to human beings, and simultaneously, the emission of pollutants is continuously increased in quantity and variety, so that the environmental protection problem is becoming serious. The small portable, simple and rapid analysis technology becomes a big research hot spot while various high-precision analysis instruments and detection technologies are greatly developed, so as to supplement the defects of complicated operation, large maintenance workload, high requirements on laboratory environment, difficulty in being used for field detection and the like of the large instrument.
The micro total analysis system is also called a lab-on-a-chip, is an analysis technology aimed at integrating all functions of a laboratory on one chip, and has shown excellent prospects in terms of miniaturization, portability and automation of the analysis technology, and is a big research hotspot in recent years.
The micro full analysis system is still in the development stage at present, and the function of a chip laboratory cannot be actually realized, so that when the analysis experiment of pretreatment is required, the pretreatment part experiment is usually finished manually, and then the micro full analysis system is entered for analysis, so that the development of automation, rapidness and portability of the micro full analysis system is limited.
Disclosure of Invention
The invention aims to solve the problem of high-flux rapid detection of complex samples in the prior art, and provides complex water body multi-parameter rapid detection equipment and a complex water body multi-parameter rapid detection method based on a microfluidic technology.
In order to achieve the above purpose, the present invention provides, on the one hand, a complex water body multi-parameter rapid detection device based on a microfluidic technology, where the complex water body multi-parameter rapid detection device includes a chip and a detection device; the chip is a rotary chip or an inline chip, and comprises a reaction tank for sample reaction; the detection device is used for detecting signals of the sample in the reaction tank.
Preferably, a label for determining the detection signal is arranged on the chip, and the label is arranged corresponding to the reaction tank.
Preferably, the plurality of reaction cells of the rotary chip are disposed on a circumference centered on a center of the chip.
Preferably, the chip comprises a substrate and a cover plate, wherein the substrate is fixedly connected with the cover plate, or the substrate and the cover plate can move mutually, so that the communication relation between the reaction tanks and/or the flow channels in the chip is changed.
Preferably, the complex water body multi-parameter rapid detection device further comprises a sample injection component, wherein the sample injection component is used for injecting a sample into the chip.
More preferably, the sample injection component is a manual sample injector;
More preferably, the sample introduction part includes a pretreatment part for pretreating a sample.
Preferably, the detection means comprises more than one detection member.
More preferably, the detection means is one or more of a chromaticity detection means, an absorbance detection means, a fluorescent signal detection means, a raman signal detection means and an infrared spectrum detection means.
Preferably, the water quality multi-parameter detection device further comprises one or more of a driving component, a signal acquisition component, a data processing component, a data output component and a data transmission component which drive the chip to rotate.
The second aspect of the invention provides a complex water body multi-parameter rapid detection method, wherein the complex water body multi-parameter rapid detection equipment is utilized for detection, samples are injected into the chip, and the detection is carried out through the detection device.
Preferably, the detection of samples in different of said reaction cells is accomplished by rotating said chip or moving said chip relative to said detection means.
Preferably, the detection means used by the detection device is determined by a mark provided on the chip for determining the detection signal.
Through the technical scheme, the complex water body multi-parameter rapid detection equipment and method can properly select the chip, the detection component, the sample injection device and the like according to the detection requirement, have the advantages of high flux, rapid detection and high accuracy, can achieve good detection effect on various samples, and can set proper pretreatment and reaction processes according to the requirement, so that the detection is more simply, conveniently and rapidly completed.
Drawings
FIG. 1 is a schematic diagram of a rotary chip according to the present invention;
FIG. 2 is a schematic diagram of a sliding chip according to the present invention;
FIG. 3 is a schematic diagram of a manual injector according to the present invention;
FIG. 4 is a schematic diagram of a manual injector having a pretreatment component of the present invention;
fig. 5 is a schematic structural view of the detecting device of the present invention.
Description of the reference numerals
1. Manual sample injector 2 and chip
11. Control part 12, sample cell 13, sample outlet part
14. Pretreatment unit
21. Flow channel 22, reaction tank 23 and sample inlet
31. Light source 32, branching optical fiber 33, and spectroscopic apparatus
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The invention provides complex water body multi-parameter quick-detection equipment based on a microfluidic technology, which comprises a chip and a detection device; the chip is a rotary chip or an inline chip, and comprises a reaction tank for sample reaction; the detection device is used for detecting signals of the sample in the reaction tank.
According to the complex water body multi-parameter rapid detection device, the microfluidic technology is adopted, so that synchronous detection of a large number of samples can be completed in a short time by arranging a plurality of reaction tanks on the chip, and operations such as sample pretreatment, reaction and the like can be completed by the structure design in the chip.
According to the present invention, the chip may be a rotary chip or an inline chip, and may have various known shapes such as a circular shape and a rectangular shape.
The rotary chip is capable of rotating around a point on the chip in the plane of the chip. The rotary die is preferably circular or regular polygonal, more preferably circular, from the viewpoint of facilitating rotation. When the rotary chip is circular, the rotary chip preferably rotates around the center of the circle.
According to a preferred embodiment of the present invention, as shown in fig. 1, the plurality of reaction cells are arranged on a circumference centered on the center of the chip. I.e. the reaction cells are equidistant from the center of the chip.
According to another preferred embodiment of the present invention, the reaction cells are divided into a plurality of groups, and each group of reaction cells has a plurality of reaction cells, and the plurality of reaction cells of each group are respectively disposed on a circumference of one of a plurality of concentric circles centering on the center of the chip. I.e. the reaction cells of each group are equidistant from the center of the chip.
The rotation method of the rotary chip is not particularly limited, and the rotary chip is preferably rotatable in the detecting device by manual operation or by driving of a driving member in the detecting device, preferably around the center of the rotary chip. The rotary chip is preferably rotated manually from the viewpoint of simplifying the inspection apparatus, reducing the cost, and facilitating portable operation. In view of improving the detection efficiency and realizing large-scale detection in a short time, the rotary chip is preferably driven to rotate by a driving member in the detection device.
The in-line chip refers to a chip in which reaction cells on the chip are arranged in a row, and is generally rectangular in design and has more than one row of reaction cells. The reaction cells of the inline chip are aligned, and thus, the inline chip can be generally detected by moving the inline chip with respect to the detecting device, for example, by pulling out the inline chip in the detecting device.
In the present invention, the number of reaction cells on the chip may be 2 or more, preferably 5 or more, more preferably 10 to 50. To facilitate the reaction, the chip may also include flow channels for sample flow between the different reaction cells. The flow channel is arranged in a manner which is required to be matched with the detection requirement of the chip, for example, when multi-step reaction is required to be carried out in the chip, the flow channel can be arranged into a structure which sequentially comprises a reaction tank, a flow channel, a reaction tank, a flow channel and a reaction tank, so that different reactions are completed in a plurality of reaction tanks. In order to control the flow of the sample, various mixing promoting structures, micro-valves, etc. may also be provided in the chip for controlling the mixing and flow of the sample.
According to a preferred embodiment of the present invention, the chip is provided with a label for determining a detection signal, the label being provided in correspondence with the reaction cell.
According to a preferred embodiment of the present invention, as shown in fig. 1, the chip has a plurality of reaction cells, a plurality of the reaction cells are arranged on one or more circumferences centering around the center of the chip, and a mark for determining a detection signal is arranged corresponding to the reaction cells. In the use process of the chip, the reaction tank in the chip is positioned at the detection position corresponding to the detection device by rotating the chip, and the corresponding detection component can be determined. Preferably, a mark for determining a detection signal is provided corresponding to each reaction cell, so that detection of a plurality of different detection indexes can be completed in a short time by one chip. And the detection process is simple and convenient to operate, has high accuracy, and can be suitable for various detection methods.
In the present invention, the mark may be a mark having a specific color or shape, for example, may be formed on the chip by printing or pasting, or may be a groove, a notch, or the like having a specific shape on the chip. The shape of the mark is not particularly limited, and may be triangular, square, regular pentagon, star-shaped, or any of various irregular shapes, for example. Only 1 mark can be arranged on the chip, and the mark is used for determining detection signals of the chip (the detection signals can be the same detection signals or detection sequences of different signals in a plurality of reaction tanks), so that the detection mode can be conveniently determined when different chips are used for different tests; corresponding detection signals can be set on the chip corresponding to a group of even each reaction tank, so that detection of different signals can be completed on one chip.
In the present invention, the plurality of reaction tanks may be arranged in such a manner that different reaction tanks may be located in a detection area of the detection device after the chip is rotated. The plurality of reaction tanks are arranged on more than one circumference taking the center of the chip as the center of the circle, so that the detection of the plurality of reaction tanks on the chip can be completed by a single detection part, and the aim of batch detection is fulfilled.
According to the present invention, the chip includes a substrate and a cover plate, the substrate being fixedly connected to the cover plate (also referred to as a "stationary chip"), or the substrate and the cover plate being movable with respect to each other so as to change a communication relationship between reaction cells and/or flow channels in the chip (also referred to as a "slide chip"). Generally, the fixed chip is used in the complex water body multi-parameter quick detection equipment, and a sliding chip can be used according to the requirement.
As the slide chip, there may be a reaction tank and/or a flow channel on the substrate and a reaction tank and/or a flow channel on the cover sheet, and by the mutual movement of the substrate and the cover sheet, the communication relationship between the flow channel and the reaction tank may be changed, for example, two non-communicating reaction tanks are formed on the substrate, a flow channel is formed on the cover sheet, and the flow channel cannot communicate with the two reaction tanks before movement; through the mutual movement of the cover plate and the cover plate, the flow channel can be communicated with the two reaction tanks, so that samples and/or preset reagents in the two reaction tanks can react with each other, and the reaction in the chip can be controlled conveniently. The sliding chip can be provided with a plurality of reaction tanks and a plurality of flow channels according to the needs, so that the requirements of various complex and high-flux reactions in complex water multi-parameter quick detection are met. The movement may be sliding or rotating in a plane.
According to a preferred embodiment of the present invention, as shown in a-d of FIG. 2, the rotatable chip 1 comprises a substrate on which the reaction well is provided and a cover plate on which a reagent well is provided, the substrate and the cover plate being relatively moved so that the reaction well and the reagent well communicate with or are separated from each other. In fig. 2a shows the substrate of the rotatable chip 1 on which the reaction wells are arranged, b shows the cover plate of the rotatable chip 1 on which the reagent wells are arranged. C and d in fig. 2 are two rotation state diagrams of the rotatable chip 1, respectively, showing a state in which the reaction cell is in communication with different reagent cells.
According to the invention, the complex water body multi-parameter rapid detection device further comprises a sample injection component, wherein the sample injection component is used for injecting a sample into the chip. The sample injection part is not particularly limited, and can be used for completing the sample injection operation of the sample, and can be used by adopting any existing sample injection device. From the viewpoint of convenience of operation and portability, preferably, the sample introduction means is a manual sample introduction device.
As a manual sample injector of the present invention, as shown in fig. 3, the manual sample injector 1 includes a sample cell 12, a control part 11, and a sample ejection part 13, the control part 11 being connected to the sample cell 12 for allowing a sample to enter and be held in the sample cell 12 or for allowing a sample to be pushed out of the sample cell 12 through the sample ejection part 13, the sample ejection part 13 being located on the side of the sample cell 12 opposite to the control part 11; the manual sample injector 1 is connected with a sample inlet 23 of the chip 2in a sealing way.
The manual sampler 1 can be matched with the chip 2 to realize the purposes of sampling and controlling the flowing process of samples in the chip 2, and the manual sampler 1 can also be used for sampling, so that devices required by simplified operation are greatly reduced, and the use of sampling devices in various application scenes is very convenient. The above-mentioned process of controlling the flow of the sample in the chip 2 includes a process of pushing the sample forward or backward, so that the functions of the chip can be more diversified, for example, the sample can be repeatedly passed through a certain reaction cell to accelerate the mixing of the sample, or the sample can be mixed with the sample in a certain chamber before being mixed with the sample in another reaction cell.
The sample inlet 23 may protrude from the outside of the chip or may be disposed inside the chip, and preferably the sample inlet 23 is provided with a screw thread so as to be screwed with the sample outlet 13.
According to the invention, the connection relationship between the manual sample injector 1 and the chip 2 can be selected according to different manual sample injectors.
According to a preferred embodiment of the present invention, in order to facilitate the completion of the sampling process using the manual sample injector 1 alone, the sample outlet 13 of the manual sample injector 1 is detachably and hermetically connected to the sample inlet 23 of the chip 2. During sampling, the manual sampler 1 may be removed, the control part 11 is operated to enable a sample to enter and be kept in the sample cell 12, and then the sample outlet part 13 of the manual sampler 1 is connected with the sample inlet 23 of the chip 2, and the control part 11 is operated to push the sample out of the sample cell 12 through the sample outlet part 13 and enter the sample inlet of the chip 11.
As a specific mode of the above-mentioned detachable sealing connection, the connection may be made by screwing or by an elastic sealing member, and preferably the bottom of the sample outlet portion 13 has a screw structure or a flexible sealing member, and preferably screwing. The thread structure can be an internal thread structure or an external thread structure; the flexible sealing member may be a rubber stopper.
According to another preferred embodiment of the present invention, in order to further simplify the apparatus, the sample outlet 13 of the manual sample injector 1 is fixedly connected to the sample inlet 23 of the chip 2. More preferably, the sample cell 12, the sample outlet 13 and the sample inlet 23 of the chip 2 of the manual sample injector 1 are integrally formed, and when in use, a sample can be directly added into the sample cell 12, and then the control part 11 is mounted in cooperation with the sample cell 12, so that the flow process of the sample in the chip is controlled by operating the control part 11.
According to a further preferred embodiment of the present invention, the control part 11 controls the range of the volume change of the inner cavity of the cuvette 12 (i.e. the chamber for sample storage formed by the cuvette 12 and the control part 11) to be selected according to the internal structure of the chip 2. Therefore, as long as a specified amount of sample is filled in the sample pool, the flow condition of the sample in each flow channel and each reaction pool of the chip 2 can be accurately controlled, the control of the sample flow in the repeated experiment process is facilitated, and the repeatability of the experiment is improved.
According to the present invention, it is preferable that the control section 11 is detachably connected to the sample cell 12. By detachably connecting the control part 11 and the sample cell 12, the two can be separated, facilitating the addition of a sample in the sample cell.
According to the present invention, the shape of the sample cell 12 and the shape of the control section 11 are not particularly limited, and the two may be matched with each other, so that the sample may be introduced into and held in the sample cell 12 or the sample may be pushed out of the sample cell 12 through the sample outlet section 13. Specifically, the sample cell 12 and the control section 11 are preferably each cylindrical. The connection method between the control unit 11 and the sample cell 12 is not particularly limited, and for example, the control unit 11 and the sample cell 12 may be preferably screwed by sealing means, screwing means, or the like, in order to facilitate the operation of the control unit 11.
According to a preferred embodiment of the present invention, the process of controlling the flow of the sample by the control part 11 is accomplished by a change in the volume of the inner cavity of the sample cell 12 caused by a relative movement between the control part 11 and the sample cell 12.
Preferably, the cuvette 12 and the control section 11 may be provided in a sleeve configuration. The control unit 11 may be an outer cylinder or an inner cylinder. More preferably, the control section 11 is provided inside the sample cell 12. Specifically, the sample cell 12 may be an outer tube having an upper opening, and the control portion 11 may be an inner tube having a bottom sealed. Preferably, the control part 11 may be provided as a telescopic piston. By providing the control part 11 as a piston, it is possible to move relatively in the sample cell 12. By making the control part 11 and the sample cell 12 cooperate, the control part 11 moves relatively inside the sample cell 12, so that the size of the inner cavity of the sample cell 12 is changed, and the sample is controlled to enter or flow out of the sample cell 12.
In order to complete the sealing connection between the control part 11 and the sample cell 12, a sealing ring is preferably provided at the bottom of the outer side wall of the control part 11, said sealing ring being used to seal the gap between the control part 11 and the sample cell 12.
According to another preferred embodiment of the present invention, the process of controlling the flow of the sample by the control part 11 is performed by a deformation process of the control part 11 itself. The control part 11 has a deformable portion, and changes the volume of the inner cavity of the sample cell 12 by deformation of the deformable portion. The shape and arrangement of the deformable portion are not particularly limited, and preferably the deformable portion of the control portion 11 is a stretchable side wall with a variable height. Specifically, the side wall may be a foldable side wall, for example, a structure in which a deformable portion formed in a tubular shape having a continuous N-shaped longitudinal section or a middle portion connects upper and lower non-deformable portions (wherein the deformable portion may be made of a flexible material, and the mutual positional relationship of the upper and lower non-deformable portions is changed by deformation of the deformable portion, for example, a horizontal connection structure is changed to a mutual embedded structure), or the like. When the side wall of the control part 11 is used as the deformable part, the top of the control part is preferably not deformed, and when in use, a compressive force or a tensile force can be applied to the top to control the height change of the side wall of the control part 11.
The material of the deformable portion of the control portion 11 is preferably a flexible material, more preferably a flexible polymer, and specifically, one or more of polyethylene, polypropylene, polytetrafluoroethylene, and among these, polyethylene and/or polypropylene are preferable.
The material of the manual injector 1 is preferably a material having light transmittance and chemical inertness. To facilitate the observation of the sample introduction process, the sample cell 12 is preferably a transparent or translucent sample cell. As the material of the sample cell 12, a polymer is preferable, and specifically, one or more of polyethylene, polypropylene, polystyrene, polyvinyl chloride, polytetrafluoroethylene, polycarbonate, polymethyl methacrylate, ABS plastic, phenol resin, epoxy resin, glass, and quartz is preferable, and one or more of polyethylene, polypropylene, polystyrene, and polyvinyl chloride is preferable. The control portion 11 is preferably formed of the above-described material except for the deformable portion and the sample ejection portion 13.
As shown in fig. 3, the complex water body multi-parameter quick-detection device comprises a manual sample injector 1 and a chip 2. In fig. 3 g, the structure of the chip 2 is shown, where the chip 2 is a circular scattering multi-runner chip, and includes 1 sample inlet 23 and 6 reaction tanks 22,6 runners 21 distributed equidistant to the sample inlet 23 are respectively connected to each reaction tank 22 and the sample inlet 23; only the sample inlet 23 of the chip 2 is shown in fig. 3 a-d, and only one set of flow channels 21 and reaction cells 22 of the chip 2 is shown in e-f; the manual sampler 1 comprises a cylindrical sample cell 12 made of polyethylene, a cup-shaped control part 11 and a sample outlet part 13, wherein the control part 11 is arranged inside the sample cell 12 and is detachably connected with the sample cell 12 in a sealing way, and is used for enabling a sample to enter and be held in the sample cell 12 or enabling the sample to be pushed out of the sample cell 12 through the sample outlet part 13, a rubber sealing ring is arranged at the bottom of the outer side wall of the control part 11, and the sample outlet part 13 is positioned at the bottom of the sample cell 12; the manual injector 1 is formed integrally with the injection port 23 of the chip 2. When in sample injection, firstly, a liquid sample is added into the sample tank 12, the control part 11 is placed in the sample tank 12, the sealing ring is contacted with the inner side wall of the sample tank 12, and the control part 11 is pushed until the sealing ring is contacted with the bottom of the interface. The sample enters the flow channel 21 of the chip 2 under the action of pressure, the flow rate of the sample gradually decreases in the flowing process, the liquid fills the first reaction tank after a period of time (such as 10-60 s), and the sample does not overflow continuously because the pressure at the end of the sample inlet 23 is smaller than the pressure for pushing the liquid out of the reaction tank 22 into the gap between the two layers of the chip, and all the reaction tanks are filled after a period of time (such as 10-60 s), so that the sample stops flowing.
According to a preferred embodiment of the present invention, as shown in fig. 4, the sample introduction part may further include a pretreatment part 14, and the pretreatment part 14 is used for pretreating a sample. The sample outlet portion 13 is located at a side of the pretreatment portion 14 opposite to the control portion 11, and the sample is pressed out of the manual sample injector after being treated by the pretreatment portion by the movement of the control portion 11.
According to the present invention, the pretreatment unit 14 preferably includes 1 or more pretreatment modules (14 a, 14b, 14 c), preferably 2 or more, more preferably 2 to 5, and even more preferably 2 to 3 pretreatment modules, for adapting to various pretreatment operations required for the sample.
As the pretreatment operation performed in each pretreatment module, selection can be made according to the sample to be introduced. Specifically, the pretreatment module is selected from one or more of a filtration module, an enrichment module, a separation module, a pH adjustment module, and a reaction module. As the filtration module, there may be provided therein fibers, porous solids, a stacking medium, etc., for example, one or more of polypropylene fibers, glass fibers, activated carbon, gravel, among which polypropylene fibers, glass fibers are preferable; as an enrichment module, alumina, silica, targeting vectors can be provided therein; as a reaction module, a desired reactant, such as mercury sulfate, which is precipitated with chloride, may be included. For example, when pretreatment of a phosphate measurement sample in sewage is performed, the pretreatment module comprises a filtration module, a pH adjustment module and a pre-reaction module; when the pretreatment of the sample for measuring the polycyclic aromatic hydrocarbon in the water is carried out, the pretreatment module comprises a filtration module and an enrichment module.
According to the invention, by detachably connecting the pretreatment part 14 with the sample cell 12, different pretreatment modules can be conveniently arranged, so that the manual sample injector meets the requirements of pretreatment and sample injection of different samples. As a means of removable connection, the cuvette 12 may be removably connected to the pretreatment section 14 by means of a plug-in section, screw threads, snap-in or groove.
In order to improve the sealability between the sample cell 12 and the pretreatment portion 14, for example, a sealing performance between the connection portion between the sample cell 12 and the pretreatment portion 14 may be further provided with a sealing auxiliary member such as a sealing gasket therebetween as needed, thereby improving the sealability of the sample injector and ensuring smooth progress of the process.
As shown in fig. 4, the manual sample injector includes a control portion 11, a sample cell 12, a pretreatment portion 14, and a sample outlet portion 13, wherein the control portion 11, the sample cell 12, and the pretreatment portion 14 are made of cylindrical transparent glass materials. The preprocessing unit 14 is a filter module. The inside of the filter module is provided with a polypropylene fiber filter disc; the top of the device is provided with a sample inlet, and the side wall of the sample inlet is provided with internal threads. A sample outlet is provided at the bottom of the sample cell 12, an external thread is provided on the side wall of the sample outlet, and the sample inlet of the pretreatment unit 14 is screwed with the sample outlet of the sample cell 12, so that the pretreatment unit 14 is detachably and hermetically connected with the sample cell 12. The sample outlet of the pretreatment part 14 is used as a sample outlet part 13, the sample outlet part 13 is positioned at the middle part of the bottom of the pretreatment part 14, and the side wall of the sample outlet part is provided with external threads for screwing with a micro full analysis chip. The control part 11 can seal the sample cell 12 to form a sample cavity, the volume of the sample cavity can be changed by moving the control part 11 through manual pushing, and the sample in the sample cavity passes through the pretreatment part 14 and is extruded through the sample outlet part 13. Before starting sample injection, the control part 11 is opened, a sample is injected into the sample injector, the control part 11 is closed, the sample injector is screwed with the sample injection port of the chip, then the control part 11 is pushed to reduce the volume of the sample cavity, and the sample enters the chip after being filtered by the filter disc of the pretreatment part 14. And observing the water sample entering the chip, and no granular impurities are found.
According to the invention, the detection device comprises more than one detection means. The detection component is used for detecting signals of samples on the chip.
In the present invention, the detection means is not particularly limited, and various detection means can be used for chip detection, and for example, the detection means may be one or more of a chromaticity detection means, an absorbance detection means, a fluorescent signal detection means, a raman signal detection means, and an infrared spectrum detection means. Wherein one or more of an absorbance detection component and a fluorescence detection component are preferred.
According to a preferred embodiment of the invention, the detection means consist of a light source 31, a shunt fiber 32 and a spectroscopic device 33, as shown in fig. 5. The light source 31 is used for generating light with a wavelength required for testing, the shunt optical fiber 32 is used for simultaneously detecting optical signals in a plurality of reaction cells, and the spectrum device 33 is used for collecting the optical signals after passing through the reaction cells. When the chip is provided with two or more reaction cells having different distances from the center of the chip, the branching optical fiber 32 may divide the incident light for detection into multiple paths, thereby realizing the detection of the reaction cells having different distances from the center of the chip.
According to the invention, in order to realize the functions of data processing, data transmission and the like, the water quality multi-parameter detection equipment also comprises one or more of a mechanical component, a signal acquisition component, a data processing component, a data output component and a data transmission component, wherein the mechanical component drives the chip to rotate. As a preferred embodiment of the water quality multi-parameter detection device, the device further comprises a data processing component, a data output component and a data transmission component. As the data processing means, for example, a central processing unit including a controller, an operator, and a register, or the like; as the data output means, a display screen having a graphic output function, a touch screen, a voice output, or the like; as the data transmission component, the original data can be uploaded to a remote server for remote processing, then the result is directly returned to the designated terminal, and the processed information generated by the data processing component can be remotely transmitted to the cloud for information collection.
According to the invention, in order to cooperate with the chip with the mark, detection of multiple parameters is realized, the complex water body multiple-parameter quick detection equipment is provided with the identification component and more than one detection part, the identification part is used for detecting the mark on the chip for determining the detection signal, and the detection part corresponds to the mark on the chip for determining the detection signal. In the rotation process of the chip, the identification part identifies the marks arranged on the chip corresponding to the reaction tanks, and then respectively determines the detection mode to be adopted by each reaction tank, thereby realizing the respective detection of different markers.
The second aspect of the invention provides a complex water body multi-parameter rapid detection method, which utilizes the complex water body multi-parameter rapid detection equipment to detect, samples are injected into the chip, and the detection is performed through the detection device.
In order to rapidly complete the multi-parameter detection, in the present invention, the detection of samples in different of the reaction cells may be accomplished by rotating the chip or moving the chip relative to the detection device. For the rotary chip, detection can be completed through the rotary chip; for the direct-discharge chip, detection can be completed through the drawing chip.
According to a preferred embodiment of the invention, the detection means used by the detection device are determined by means of a marker provided on said chip for determining the detection signal. By using the chip with the mark, the method can process the detection process of various sample signals in a short time, thereby improving the detection speed.
The index which can be detected by the method comprises COD, total nitrogen, sulfide, total phosphorus and the like, and the corresponding reagent can be used for detecting the sample after the sample is treated. The reagent can be preset in the chip for the reaction requiring the reagent addition, so that the detection precision is improved, and the operation is more convenient.
The method can properly select the chip, the detection component, the sample injection device and the like according to the detection requirement, so that good detection effect can be achieved for various samples, and proper pretreatment and reaction processes can be set according to the requirement, so that the detection can be more simply, conveniently and rapidly finished. The method is particularly suitable for detecting the water sample.
The present invention will be described in detail by examples. In the following examples, the specific detection reagents were commercially available products of WAK, co-physical and chemical company, japan, and the samples were mixed solutions of COD, total nitrogen, sulfide, and total phosphorus standard solutions.
Example 1
The complex water body multi-parameter rapid detection equipment used in the embodiment comprises a manual sample injector 1, a chip 2 and a hand-held spectrophotometer with a built-in rotary fixing frame as shown in fig. 3.
Feeding with a manual feeding device 1 as shown in fig. 3; a rotary chip with four different marked circles was used, all 12 reaction cells being equally dispersed on the circumference at equal distance R from the centre of the chip (12 reaction cells were arranged on the basis of the schematic g in fig. 3). The chip 2 is a circular scattering multi-runner chip and comprises 1 sample inlet 23 and 12 reaction tanks 22 which are distributed at equal intervals with the sample inlet 23, and 12 runners 21 are respectively communicated with the reaction tanks 22 and the sample inlet 23; only the sample inlet 23 of the chip 2 is shown in fig. 3 a-d, and only one set of flow channels 21 and reaction cells 22 of the chip 2 is shown in e-f;
The manual sampler 1 comprises a cylindrical sample cell 12 made of polyethylene, a cup-shaped control part 11 and a sample outlet part 13, wherein the control part 11 is arranged inside the sample cell 12 and is detachably connected with the sample cell 12 in a sealing way, and is used for enabling a sample to enter and be held in the sample cell 12 or enabling the sample to be pushed out of the sample cell 12 through the sample outlet part 13, a rubber sealing ring is arranged at the bottom of the outer side wall of the control part 11, and the sample outlet part 13 is positioned at the bottom of the sample cell 2;
The manual injector 1 is formed integrally with the injection port 23 of the chip 2.
First, a liquid sample is added into the sample cell 12, the control part 11 is placed in the sample cell 12, the sealing ring is contacted with the inner side wall of the sample cell 12, and the control part 11 is pushed until the control part contacts the bottom of the interface. The sample enters the flow channel 21 of the chip 2 under the action of pressure, the flow rate of the sample gradually decreases in the flowing process, the liquid fills the first reaction tank after 32s, and the sample does not overflow continuously because the pressure at the end of the sample inlet 23 is smaller than the pressure for pushing the liquid out of the reaction tank 22 and into the gap between the two layers of the chip, all the reaction tanks are filled after 19s, and the sample stops flowing.
The hand-held spectrophotometer with the built-in rotary holder is composed of a light source 31, a branching optical fiber 32 and a spectroscopic device 33, and is preset with measurement wavelengths of 410nm (total nitrogen), 620nm (COD), 665nm (sulfide), 880nm (total phosphorus) which are selectable. During testing, a manual rotation method is adopted to enable the chip to rotate around the circle center. The specific detection reagent is preset on the identifiable chip, the sample solution is introduced into the reaction tank and reacts with the preset reaction reagent, and the absorbance value is read after 30 min.
1-3 Of the 12 reaction tanks are total nitrogen detection tanks, 4-6 of the 12 reaction tanks are COD detection tanks, 7-9 of the 12 reaction tanks are sulfide detection tanks, 10-12 of the 12 reaction tanks are total phosphorus detection tanks, and different marks are respectively arranged in the 4 groups of corresponding reaction tanks. The manual rotation chip passes through the reaction tanks one by one, the spectrophotometers detect the marks and then determine the measurement wavelength corresponding to the index to be detected, and then the wavelength of the light source is changed and the measurement is carried out. The corresponding concentrations measured are shown in Table 1 below.
TABLE 1
Example 2
The complex water body multi-parameter quick detection equipment used in the embodiment comprises a circular identifiable chip and a handheld spectrophotometer with a built-in rotary fixing frame as shown in fig. 3.
The circular identifiable chip with four different marks is adopted, 4 reaction tanks are evenly dispersed and arranged on the circumference with the distance R1 from the center of the chip, and in addition, 4 reaction tanks are evenly dispersed and arranged on the circumference with the distance R2 from the center of the chip. The hand-held spectrophotometer with built-in rotary holder is composed of a light source 31, a branching optical fiber 32 and a spectroscopic device 33, and preset measurement wavelengths of 410nm (total nitrogen), 620nm (COD), 665nm (sulfide), 880nm (total phosphorus) which are selectable. During testing, a manual rotation method is adopted to enable the chip to rotate around the circle center. The specific detection reagent is preset on the identifiable chip, the sample solution is introduced into the reaction tank and reacts with the preset reaction reagent, and the absorbance value is read after 30 min.
The distances from the circle center of the chip to the circle center of the 8 reaction tanks are 1 and 2 on the circumference of the chip, wherein the distances from the circle center of the chip to the circle center of the chip are R1, 3 and 4 are COD detection tanks, 5 and 6 on the circumference of the reaction tank are R2, and 7 and 8 are total phosphorus detection tanks. Different marks are respectively arranged in the corresponding reaction tanks in the 4 groups. The manual rotation chip passes through the reaction tanks one by one, and after the spectrophotometer detects the marks, the measurement wavelength corresponding to the index to be detected is determined, and then the measurement is carried out. The corresponding concentrations measured are shown in Table 2 below:
TABLE 2
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.

Claims (9)

1. The complex water body multi-parameter quick-detection equipment based on the microfluidic technology is characterized by comprising a chip and a detection device;
The chip is a rotary chip or an inline chip, and comprises a reaction tank for sample reaction;
The detection device is used for detecting signals of the sample in the reaction tank;
The chip is provided with a mark for determining a detection signal, and the mark is arranged corresponding to the reaction tank;
The reaction tanks of the rotary chip are arranged on the circumference taking the center of the chip as the center of a circle;
The chip comprises a substrate and a cover plate, the reaction tank is arranged on the substrate, a reagent tank is arranged on the cover plate, and the substrate and the cover plate relatively move so that the reaction tank and the reagent tank are mutually communicated or separated;
The reaction tanks are divided into a plurality of groups, each group of reaction tanks is provided with a plurality of reaction tanks, and the plurality of reaction tanks of each group are respectively arranged on the circumference of one of a group of concentric circles taking the center of the chip as the center of the circle;
the complex water body multi-parameter quick detection equipment is provided with an identification component and more than one detection part, wherein the identification part is used for detecting marks on the chip for determining detection signals, and the detection part corresponds to the marks on the chip for determining the detection signals and determines a detection mode;
The detection component is one or more of a chromaticity detection component, an absorbance detection component, a fluorescent signal detection component, a Raman signal detection component and an infrared spectrum detection component.
2. The complex water body multi-parameter rapid inspection device of claim 1, further comprising a sample introduction component for introducing a sample into the chip.
3. The complex water body multi-parameter rapid inspection device of claim 2, wherein the sample introduction component is a manual sample injector.
4. The complex water body multi-parameter rapid inspection device according to claim 3, wherein the sample introduction part comprises a pretreatment part for pretreating a sample.
5. The complex water body multi-parameter rapid inspection device according to claim 1, wherein the detection means comprises more than one detection component.
6. The complex water body multi-parameter rapid inspection device according to claim 1, wherein the water body multi-parameter rapid inspection device further comprises one or more of a driving component, a signal acquisition component, a data processing component, a data output component and a data transmission component for driving the chip to rotate.
7. A complex water body multi-parameter rapid detection method, which is characterized in that the complex water body multi-parameter rapid detection equipment according to any one of claims 1-6 is used for detection, a sample is injected into the chip, and the detection is carried out through the detection device.
8. The complex water multi-parameter rapid detection method of claim 7, wherein sample detection in different reaction cells is accomplished by rotating the chip or moving the chip relative to the detection device.
9. The complex water body multi-parameter quick detection method according to claim 7 or 8, wherein the detection component used by the detection device is determined through the mark used for determining the detection signal arranged on the chip.
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