Chromatographic analysis method and device for food quality control and safety detection
Through the design of multiple gasification chambers and turntable structures, combined with solid-phase extraction and thermal insulation shell, the problem of inefficient continuous operation of gas chromatographs is solved, and efficient food quality and safety inspection is achieved.
Patent Information
- Application Number
- CN202510641220.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-19
- Publication Date
- 2025-08-15
AI Technical Summary
The liquid to gaseous conversion process during continuous operation of existing gas chromatographs takes a long time, resulting in low working efficiency.
Using multiple gasification chambers and turntable structures, the gasification chamber is preheated and gas storage is realized by rotating and switching the communication between the gasification chamber and the connecting pipe. Combined with the solid-phase extraction coating and thermal insulation shell design, the gasification efficiency and continuous operation efficiency are improved.
It reduces the gasification time during a single test, improves the working efficiency of continuous operations, and is suitable for food quality control and large-scale sample testing.
Smart Images
Figure CN120490327A_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of food detection, and in particular relates to a chromatographic analysis method and device for food quality control and safety detection. Background Art
[0002] Food analysis is a very important means for evaluating the nutritional value, freshness and quality of processed products, as well as detecting food additives and pesticide residues. Chromatography, as an important component of analytical and testing instruments, can provide practical separation and analysis methods and is widely used in scientific research, pharmaceuticals, chemicals, environmental monitoring and other fields. Due to the close relationship between food and people's lives, the application of chromatography in the field of food testing has attracted much attention. Gas chromatography is a chromatographic analysis method using gas as the mobile phase, which is mainly used to separate and analyze volatile substances. Gas chromatography has become one of the most important separation and analysis methods, and is widely used in the fields of medicine and health, petrochemicals, environmental monitoring, biochemistry, food safety and so on.
[0003] In the prior art, the vaporization chamber of a gas chromatograph can heat a sample solution to convert it from liquid to gas for gas chromatography detection. However, the liquid-to-gas conversion process takes a long time, resulting in low efficiency during continuous operation. Summary of the Invention
[0004] In order to solve the above problems, the purpose of the present invention is to provide a chromatographic analysis method and device for food quality control and safety testing, which can improve work efficiency during continuous operation.
[0005] To achieve the above-mentioned objectives, the technical solution of the present invention is as follows: A chromatographic analysis method and apparatus for food quality control and safety testing, comprising a housing, a carrier gas generator, a chromatographic column, a detector, and a controller disposed within the housing, a base fixedly connected to one side of the housing, a turntable rotatably connected to the base, the turntable extending through the housing and into the housing, and a drive member disposed within the base for driving the turntable to rotate;
[0006] There are several vaporization chambers on the circumference of the turntable. The top and bottom of the vaporization chambers are both opened. The openings are equipped with valves for closing the vaporization chambers. The base is equipped with a heat source for heating the vaporization chambers. The heat source is an electric heating wire.
[0007] The carrier gas generator is connected with a first connecting pipe, the chromatographic column is connected with a second connecting pipe, the first connecting pipe and the second connecting pipe are connected with the vaporization chamber respectively, and the turntable is used to switch the vaporization chamber connected with the first connecting pipe and the second connecting pipe.
[0008] The above solution achieves the following beneficial effects: The user prepares several food sample solutions to be tested. The food sample solutions must be filtered to remove suspended solids to reduce post-vaporization residue. The food sample solutions are then sequentially injected into the vaporization chambers. The turntable rotates around the vaporization chambers, with each rotation changing the vaporization chamber connected to the first and second connecting tubes in the same direction.
[0009] During rotation, the heat source heats the vaporization chamber, vaporizing the liquid within. The vaporized liquid is then stored within the chamber, sealed by a valve. When the chamber connects to the first and second connecting tubes, the stored gas is released. The carrier gas generator draws the gas into the chromatographic column, where the concentration of each component is detected by a detector. The heat source continues heating until the liquid within the chamber is completely vaporized and the carrier gas generator completely removes the gas from the chamber.
[0010] The released vaporization chamber will continue to rotate and move out of the housing in the direction of rotation. At this time, there is no liquid or gas remaining in the vaporization chamber, and the user can add food sample solution to the vaporization chamber.
[0011] Compared with the existing technology, the use process of the vaporization chamber is improved. The vaporization chamber is set to multiple, and is filled and heated in sequence by rotation. Preheating is performed during the period from filling to gas release, and the gas is stored in the vaporization chamber, which reduces the vaporization time in a single detection process and improves work efficiency in continuous operation. It is suitable for food quality control and testing of a large number of samples.
[0012] Furthermore, the side wall of the vaporization chamber is provided with a solid phase extraction coating.
[0013] Benefits: Food, environmental, and biological sample matrices are very complex, with low levels of target analytes and numerous interfering substances. Sample pretreatment is essential before analysis. Solid-phase extraction (SPE) technology can extract and enrich samples, reducing the levels of interfering components.
[0014] Furthermore, the solid phase extraction coating is made of one or more materials selected from the group consisting of covalent organic framework materials, carbon nanospheres and boron nitride.
[0015] Beneficial effects: Covalent organic framework materials, carbon nanospheres and boron nitride all have porous structures and strong adsorption properties, and can effectively enrich the solution according to the components to be tested.
[0016] Furthermore, the turntable is provided with a shell, which is made of heat-insulating material. The shell is provided with a release port for connecting the first connecting pipe and the second connecting pipe, and the shell is provided with a delivery port for delivering samples.
[0017] Beneficial effect: The shell can insulate heat and reduce heat loss from the heat source, thereby reducing heating power consumption.
[0018] Furthermore, the first connecting tube and the second connecting tube are both provided with a telescopic driving structure, and the first connecting tube and the second connecting tube are both provided with an airtight pad on one side close to the turntable.
[0019] Beneficial effect: The first connecting pipe and the second connecting pipe can press the airtight pad onto the turntable through the telescopic driving structure, thereby improving the airtightness when connected to the vaporization chamber.
[0020] Furthermore, the delivery port is located outside the housing, and the distance between the delivery port and the release port along the direction of rotation of the turntable is greater than the distance from the release port along the opposite direction of rotation of the turntable.
[0021] Beneficial effect: The longer the time from the injection port to the release port is, the better the heating and adsorption effects are.
[0022] Furthermore, the base is provided with a waste liquid collection chamber, and a discharge port is provided at the bottom of the waste liquid collection chamber.
[0023] Beneficial effect: After the solid phase extraction coating is enriched, the sample solution does not need to be vaporized, so the sample solution is discharged at the waste liquid collection chamber to reduce the amount of solution in the vaporization chamber and shorten the time required for vaporization.
[0024] Furthermore, the method of the chromatographic analysis device for food quality control and safety detection based on claims 1 to 7 comprises:
[0025] Step 1: Prepare 10 to 15 g of a food sample, mince the food sample, and then grind it to prepare a homogenate sample. Centrifuge the homogenate sample at 9000 to 12000 rpm for 8 to 10 minutes. Transfer the supernatant after centrifugation to a 25 mL volumetric flask, make up to volume, add 2.5 g of sodium chloride, and perform ultrasonic stirring to obtain a sample solution.
[0026] Step 2: The turntable rotates grid by grid, and the sample solution is injected into the vaporization chamber through the injection port. During the rotation process, the solid phase extraction coating in the vaporization chamber extracts the components to be tested through the adsorption effect of the active sites, and adsorbs the components to be tested on the solid phase extraction coating. When the vaporization chamber rotates to the waste liquid collection chamber, the valve opens to release the sample solution into the waste liquid collection chamber, so that the vaporization chamber retains only the attached liquid on the solid phase extraction coating;
[0027] In step three, after the vaporization chamber passes through the waste liquid collection chamber, the valve is closed, and the attached liquid is heated and vaporized by the heat from the heat source. The generated gas is stored in the vaporization chamber. When the vaporization chamber rotates until it is connected to the first connecting pipe and the second connecting pipe, the valve is opened, and the generated gas is released and enters the chromatographic column for detection under the pumping of the carrier gas generator.
[0028] Beneficial Effects: Users simply wait at the inlet, and the sample solution is injected each time the turntable rotates one grid. During the turntable's rotation, enrichment and adsorption, heating and vaporization, and gas chromatography detection are completed. Furthermore, the enrichment and adsorption process is accelerated by the residual heat from the heating and vaporization process, and the higher extraction temperature accelerates the diffusion of the analyte, thereby improving work efficiency. BRIEF DESCRIPTION OF THE DRAWINGS
[0029] Figure 1 Schematic diagram of an embodiment of the present invention.
[0030] Figure 2 Schematic diagram of the structure of an embodiment of the present invention.
[0031] Figure 3 Schematic diagram of the structure of the turntable.
[0032] Figure 4 for Figure 2 Enlarged schematic diagram of part A. DETAILED DESCRIPTION
[0033] The following is further described in detail through specific implementation methods:
[0034] The figure marks in the drawings of the specification include: housing 1, carrier gas generator 2, chromatographic column 3, detector 4, controller 5, base 6, turntable 7, drive part 8, vaporization chamber 9, valve 10, heat source 11, first connecting pipe 12, second connecting pipe 13, solid phase extraction coating 14, release port 15, injection port 16, waste liquid collection chamber 17, discharge port 18, telescopic drive structure 19, and airtight gasket 20.
[0035] Example 1
[0036] The embodiment is basically as shown in the attached Figure 1 To the attached Figure 4 As shown:
[0037] A chromatographic analysis method and device for food quality control and safety testing, comprising a housing 1, within which are mounted a carrier gas generator 2, a chromatographic column 3, a detector 4, and a controller 5. The carrier gas generator 2, the chromatographic column 3, and the detector 4 are all components of a conventional gas chromatograph. The controller 5 is model YM-SMP01. A base 6 is fixed to one side of the housing 1 by screws. A turntable 7 is rotatably connected to the base 6 and extends through the housing 1 into the housing 1. A drive member 8 for driving the turntable 7 to rotate is disposed within the base 6. The drive member 8 is a motor, model CC-M3H075.
[0038] A plurality of vaporization chambers 9 are provided on the upper circumference of the turntable 7. The vaporization chambers 9 are provided with openings at the top and bottom. Valves 10 are provided in the openings for closing the vaporization chambers 9. A heat source 11 is provided on the base 6 for heating the vaporization chambers 9.
[0039] The carrier gas generator 2 is connected to a first connecting pipe 12 , and the chromatographic column 3 is connected to a second connecting pipe 13 . The first connecting pipe 12 and the second connecting pipe 13 are respectively connected to the vaporization chamber 9 . The turntable 7 is used to switch the vaporization chamber 9 connected to the first connecting pipe 12 and the second connecting pipe 13 .
[0040] The specific implementation process is as follows: The user prepares several food sample solutions to be tested. The food sample solutions must be filtered to remove suspended solids to reduce post-vaporization residue. The food sample solutions are then sequentially injected into vaporization chambers 9. The turntable 7 rotates around the vaporization chambers 9, with each rotation changing the vaporization chamber 9 connected to the first and second connecting tubes 12, 13 in the same direction.
[0041] During rotation, heat source 11 heats vaporization chamber 9, vaporizing the liquid within. The vaporized liquid is then stored within vaporization chamber 9, sealed by valve 10. When vaporization chamber 9 is connected to first connecting tube 12 and second connecting tube 13, the stored gas is released. Under the action of carrier gas generator 2, the gas is carried into chromatographic column 3, where the concentration of each component to be measured is detected by detector 4. During the release process, heat source 11 continues heating until the liquid within vaporization chamber 9 is completely vaporized and carrier gas generator 2 completely removes the gas from vaporization chamber 9.
[0042] The released gasification chamber 9 will continue to rotate and move along the rotation direction to the outside of the housing 1. At this time, there is no liquid or gas remaining in the gasification chamber 9, and the user can add the food sample solution to the gasification chamber 9.
[0043] This invention improves the use process of the vaporization chamber 9, provides multiple vaporization chambers 9, and fills and heats them in sequence by rotating. Preheating is performed during the period from filling to releasing gas, and the gas is stored in the vaporization chamber 9, which reduces the vaporization time during a single detection process and improves work efficiency in continuous operation. It is suitable for food quality control and testing of a large number of samples.
[0044] Example 2
[0045] The difference from the above embodiment is that a solid phase extraction coating 14 is provided on the side wall of the vaporization chamber 9 .
[0046] The specific implementation process is as follows: The matrices of food, environmental and biological samples are very complex and the target analytes are present at very low levels and have many interfering substances.
[0047] Sample pretreatment is necessary before analysis. Solid phase extraction technology has the ability to extract and enrich samples, which can reduce the content of interfering components.
[0048] Example 3
[0049] The difference from the above embodiment is that the solid phase extraction coating 14 is made of one or more materials selected from the group consisting of covalent organic framework materials, carbon nanospheres and boron nitride.
[0050] The specific implementation process is as follows: covalent organic framework materials, carbon nanospheres and boron nitride all have porous structures and strong adsorption properties, and can effectively enrich the solution according to the components to be tested.
[0051] Example 4
[0052] The difference from the above embodiment is that the turntable 7 is provided with a shell made of heat-insulating material, the shell is provided with a release port 15 for connecting the first connecting pipe 12 and the second connecting pipe 13, and the shell is provided with a delivery port 16 for delivering samples.
[0053] The specific implementation process is as follows: the casing can insulate and retain heat, reducing heat loss from the heat source 11 and thus reducing heating power consumption.
[0054] Example 5
[0055] The difference from the above embodiment is that the first connecting tube 12 and the second connecting tube 13 are both provided with a telescopic driving structure 19, which is a push rod, and an airtight pad 20 is bonded and fixed to one side of the first connecting tube 12 and the second connecting tube 13 close to the turntable 7.
[0056] The specific implementation process is as follows: the first connecting pipe 12 and the second connecting pipe 13 can press the airtight pad 20 onto the turntable 7 through the telescopic driving structure 19 to improve the airtightness when connected to the vaporization chamber 9.
[0057] Example 6
[0058] The difference from the above embodiment is that the feeding port 16 is located outside the casing 1, and the distance between the feeding port 16 and the release port 15 along the rotation direction of the turntable 7 is greater than the distance from the release port 15 along the opposite rotation direction of the turntable 7.
[0059] The specific implementation process is as follows: the longer the time it takes for the delivery port 16 to rotate to the release port 15 , the better the heating and adsorption effects.
[0060] Example 7
[0061] The difference from the above embodiment is that the base 6 is provided with a waste liquid collecting chamber 17 , and a discharge port 18 is provided at the bottom of the waste liquid collecting chamber 17 .
[0062] The specific implementation process is as follows: after the solid phase extraction coating 14 is enriched, the sample solution does not need to be vaporized, so the sample solution is discharged from the waste liquid collection chamber 17 to reduce the amount of solution in the vaporization chamber 9 and shorten the time required for vaporization.
[0063] Example 8
[0064] The difference from the above embodiment is that the method based on the chromatographic analysis device for food quality control and safety detection according to claims 1 to 7 comprises:
[0065] Step 1: Prepare 10 to 15 g of a food sample, mince the food sample, and then grind it to prepare a homogenate sample. Centrifuge the homogenate sample at 9000 to 12000 rpm for 8 to 10 minutes. Transfer the supernatant after centrifugation to a 25 mL volumetric flask, make up to volume, add 2.5 g of sodium chloride, and perform ultrasonic stirring to obtain a sample solution.
[0066] Step 2: The turntable 7 rotates grid by grid, and the sample solution is injected into the vaporization chamber 9 through the injection port 16. During the rotation process, the solid phase extraction coating 14 in the vaporization chamber 9 extracts the components to be tested through the adsorption action of the active sites, and adsorbs the components to be tested on the solid phase extraction coating 14. When the vaporization chamber 9 rotates to the waste liquid collection chamber 17, the valve 10 opens to release the sample solution into the waste liquid collection chamber 17, so that the vaporization chamber 9 retains only the attached liquid on the solid phase extraction coating 14;
[0067] In step three, after the vaporization chamber 9 passes through the waste liquid collection chamber 17, the valve 10 is closed, and the attached liquid is heated and vaporized by the heat from the heat source 11. The generated gas is stored in the vaporization chamber 9. When the vaporization chamber 9 rotates until it is connected to the first connecting pipe 12 and the second connecting pipe 13, the valve 10 is opened, and the generated gas is released and enters the chromatographic column 3 for detection under the pumping of the carrier gas generator 2.
[0068] The specific implementation process is as follows: the user simply waits at the injection port 16, and the sample solution is injected each time the turntable 7 rotates one grid. During the rotation of the turntable 7, enrichment and adsorption, heating and vaporization, and gas chromatography detection are completed. Furthermore, the enrichment and adsorption process can be accelerated by the residual heat from the heating and vaporization process. The higher extraction temperature can accelerate the diffusion of the analyte, thereby improving work efficiency.
[0069] The above is only an embodiment of the present invention. Common knowledge such as the known specific structures and characteristics in the scheme is not described in detail here. Ordinary technicians in the field are aware of all common technical knowledge in the technical field of the invention before the application date or priority date, can obtain all existing technologies in the field, and have the ability to apply conventional experimental means before that date. Ordinary technicians in the field can improve and implement this scheme in combination with their own abilities under the inspiration given by this application. Some typical known structures or known methods should not become obstacles for ordinary technicians in the field to implement this application. It should be pointed out that for those skilled in the art, without departing from the structure of the present invention, several variations and improvements can be made, which should also be regarded as the scope of protection of the present invention. These will not affect the effect of the implementation of the present invention and the practicality of the patent. The scope of protection required by this application shall be based on the content of its claims, and the specific implementation methods and other records in the specification can be used to interpret the content of the claims.
Claims
1. A chromatographic analysis device for food quality control and safety testing, characterized by: The invention comprises a casing, wherein a carrier gas generator, a chromatographic column, a detector and a controller are arranged in the casing, a base is fixedly connected to one side of the casing, a turntable is rotatably connected to the base, the turntable extends through the casing into the casing, and a driving member for driving the turntable to rotate is arranged in the base; Several vaporization chambers are opened on the circumference of the turntable. The top and bottom of the vaporization chambers are both provided with openings. Valves are provided in the openings for closing the vaporization chambers. A heat source for heating the vaporization chambers is provided on the base. The carrier gas generator is connected with a first connecting pipe, the chromatographic column is connected with a second connecting pipe, the first connecting pipe and the second connecting pipe are connected with the vaporization chamber respectively, and the turntable is used to switch the vaporization chamber connected with the first connecting pipe and the second connecting pipe.
2. The chromatographic analysis device for food quality control and safety testing according to claim 1, characterized in that: The side wall of the vaporization chamber is provided with a solid phase extraction coating.
3. The chromatographic analysis device for food quality control and safety testing according to claim 2, characterized in that: The solid phase extraction coating is made of one or more materials selected from the group consisting of covalent organic framework materials, carbon nanospheres and boron nitride.
4. The chromatographic analysis device for food quality control and safety testing according to claim 3, characterized in that: The turntable is provided with a shell which is made of heat-insulating material. The shell is provided with a release port for connecting the first connecting pipe and the second connecting pipe. The shell is provided with a delivery port for delivering samples.
5. The chromatographic analysis device for food quality control and safety testing according to claim 4, characterized in that: The first connecting pipe and the second connecting pipe are both provided with a telescopic driving structure, and the first connecting pipe and the second connecting pipe are both provided with an airtight pad on one side close to the turntable.
6. The chromatographic analysis device for food quality control and safety testing according to claim 5, characterized in that: The feeding port is located outside the casing, and the distance between the feeding port and the release port along the rotation direction of the turntable is greater than the distance between the feeding port and the release port along the opposite rotation direction of the turntable.
7. The chromatographic analysis device for food quality control and safety testing according to claim 6, characterized in that: The base is provided with a waste liquid collecting chamber, and a discharge port is provided at the bottom of the waste liquid collecting chamber.
8. A chromatographic analysis method for food quality control and safety testing, characterized by: The method of the chromatographic analysis device for food quality control and safety detection based on claims 1 to 7 comprises: Step 1: Prepare 10 to 15 g of a food sample, mince the food sample, and then grind it to prepare a homogenate sample. Centrifuge the homogenate sample at 9000 to 12000 rpm for 8 to 10 minutes. Transfer the supernatant after centrifugation to a 25 mL volumetric flask, make up to volume, add 2.5 g of sodium chloride, and perform ultrasonic stirring to obtain a sample solution. Step 2: The turntable rotates grid by grid, and the sample solution is injected into the vaporization chamber through the injection port. During the rotation process, the solid phase extraction coating in the vaporization chamber extracts the components to be tested through the adsorption effect of the active sites, and adsorbs the components to be tested on the solid phase extraction coating. When the vaporization chamber rotates to the waste liquid collection chamber, the valve opens to release the sample solution into the waste liquid collection chamber, so that the vaporization chamber retains only the attached liquid on the solid phase extraction coating; In step three, after the vaporization chamber passes through the waste liquid collection chamber, the valve is closed, and the attached liquid is heated and vaporized by the heat from the heat source. The generated gas is stored in the vaporization chamber. When the vaporization chamber rotates until it is connected to the first connecting pipe and the second connecting pipe, the valve is opened, and the generated gas is released and enters the chromatographic column for detection under the pumping of the carrier gas generator.