Device and method for detecting drug residues in aquatic products

Abstract

This invention relates to the field of drug detection technology, and more particularly to a device and method for detecting drug residues in aquatic products, comprising: a separation module for separating aquatic product samples into an extract and a matrix; a conveying module connected to the separation module for conveying the extract; a detection module connected to both the separation module and the conveying module for detecting the weight of the matrix, the weight of the extract, the centrifugation speed of the mixture, and the concentration of residual drugs; and a control module for adjusting the pump start-up mode when the accuracy of drug residue detection is deemed insufficient based on the average difference in residual drug concentration, or for initially determining that the degree of drug loss during the filtration process is insufficient and further determining the degree of drug loss during the filtration process based on the weight difference between the extract and the matrix and the aquatic product raw materials. This invention improves the accuracy of drug residue detection.

Description

Technical Field

[0001] The present invention relates to the technical field of drug detection, and in particular to a device and method for detecting drug residues in aquatic products. Background Art

[0002] In the prior art, aquatic products refer to edible animals or plants captured or cultured from water, including various organisms from the ocean, freshwater or artificially cultured. With the increasing improvement of people's living standards, the market demand for aquatic products continues to expand. While the fishery has achieved great development, it has also brought about the frequent occurrence of fishery diseases. The widespread use of feed, additives, and fishery drugs in aquaculture has posed a severe test to the quality and safety of aquatic products. The safety of aquatic products has received increasing attention from the government and the people.

[0003] Chinese Patent Publication No.: CN116718695A discloses a method and device for determining quinolone drug residues in aquatic products, the method comprising: S1, sample preparation: cutting muscle tissue of the aquatic product to be tested, placing it in a meat grinder and mincing it, and then weighing 5-8g of the minced tissue as a sample; S2, standard solution preparation: weighing a quinolone drug standard, dissolving it in methanol to make a 100mg / L standard stock solution, making a single standard stock solution, and then taking the single standard stock solution and diluting it with acetonitrile to make a 1mg / L mixed standard solution of 16 quinolones and a 1mg / L mixed standard solution of 5 deuterated internal standards, and diluting it again before use. Release to the required concentration; S3, test solution extraction: put the sample into the extraction device, take 25μL from the 1mg / L internal standard mixed standard solution and add it to the sample, add 15mL of acidified acetonitrile, vortex mix, then add 10g of anhydrous sodium sulfate, vortex mix, centrifuge after ultrasonic extraction, then take out the supernatant and squeeze the sample residue to obtain the extruded liquid, take half of the supernatant and mix with the extruded liquid to obtain the extract, the extract is passed through a neutral alumina column in a 50mL pear-shaped bottle, and then evaporated and concentrated, dissolved and fixed, degreased, and filtered to obtain the test solution; S4, liquid chromatography tandem mass spectrometer determination: the test solution is measured by liquid chromatography tandem mass spectrometer. It can be seen that the method and device for determining quinolone residues in aquatic products have the problem that the water pump is initially started by auto-coupling, which generates heat during the operation of the water pump, causing some components in the extract to change, thereby reducing the accuracy of the detection. Summary of the invention

[0004] To this end, the present invention provides a device and method for detecting drug residues in aquatic products, so as to overcome the problem in the prior art that the water pump is initially started by auto-coupling, which causes heat to be generated during the operation of the water pump, causing some components in the extract to change, thereby reducing the accuracy of the detection.

[0005] To achieve the above-mentioned object, the present invention provides a drug residue detection device in aquatic products, comprising: a separation module, used to separate aquatic product samples into extracts and matrixes, including a stirring tank for mixing the aquatic product samples and the extraction solvent to output the mixed solution and a filtering component connected to the stirring tank for filtering the mixed solution to output the extract; a conveying module, which is connected to the separation module and used to convey the extract, including a conveying component connected to the filtering component for conveying the extract to a storage position, wherein the conveying component includes a water pump for controlling the conveying power of the extract; a detection module, which is respectively connected to the separation module and the conveying module, and used to respectively The weight of the matrix, the weight of the extract, the centrifugal speed of the mixed solution and the concentration of the residual drug are detected; a control module is respectively connected to the separation module, the conveying module and the detection module, and is used to adjust the starting mode of the water pump when it is determined that the accuracy of the drug residue detection does not meet the requirements according to the average difference in the residual drug concentration, or to preliminarily determine that the loss degree of the drug in the filtration process does not meet the requirements and secondarily determine the loss degree of the drug in the filtration process according to the weight difference between the extract and the matrix and the aquatic product raw material; and, when it is secondarily determined that the loss degree of the drug in the filtration process does not meet the requirements, adjust the operation mode of the stirring tank, or determine the working mode of the filtration component according to the actual centrifugal speed of the mixed solution.

[0006] Furthermore, the delivery module also includes a liquid storage component connected to the delivery component for storing the extraction liquid, and the liquid storage component is a liquid storage tank.

[0007] Furthermore, the stirring tank comprises:

[0008] A vertical connecting rod, which is arranged inside the stirring tank and is used to control the stirring height;

[0009] A stirring paddle connected to the vertical connecting rod for stirring the aquatic product sample and the extraction solvent;

[0010] The electric telescopic rod is connected to the vertical connecting rod and changes the descending speed of the vertical connecting rod by changing the telescopic speed.

[0011] Furthermore, the detection module includes:

[0012] A first weight sensor, which is disposed below the stirring tank and is used to detect the weight of the substrate in the stirring tank;

[0013] A second weight sensor is disposed below the liquid storage tank and is used to detect the weight of the extracted liquid in the liquid storage tank;

[0014] A Hall effect sensor connected to the vertical connecting rod to detect the actual centrifugal speed of the mixed liquid;

[0015] A high performance liquid chromatograph is arranged at the output end of the liquid storage tank and is used to detect the concentration of residual drugs in the aquatic product raw materials.

[0016] Further, the control module is connected to the high performance liquid chromatograph to calculate an average difference in residual drug concentrations according to residual drug concentrations detected several times, and to determine that the accuracy of drug residue detection does not meet the requirements when the average difference in residual drug concentrations meets the first difference condition or the second difference condition;

[0017] The control module is connected to the detection module, and is used to preliminarily determine that the loss degree of the drug in the filtration process does not meet the requirements when the average difference amount of the residual drug concentration only meets the first difference amount condition, and to perform a secondary determination on the loss degree of the drug in the filtration process according to the weight difference between the extract and the matrix and the aquatic product raw material;

[0018] Among them, the first difference condition is that the average difference in residual drug concentration is greater than the preset first difference and less than or equal to the preset second difference; the second difference condition is that the average difference in residual drug concentration is greater than the preset second difference.

[0019] Furthermore, the control module is connected to the water pump to adjust the start-up mode of the water pump when the average difference in the residual drug concentration only satisfies the second difference condition;

[0020] Wherein, the starting mode of the water pump is adjusted from auto-coupling starting to star-delta starting.

[0021] Further, the control module is connected to the detection module, and is used to make a secondary determination that the degree of drug loss in the filtration process does not meet the requirements when the weight difference between the extract and the matrix and the aquatic product raw material meets the first weight difference condition or the second weight difference condition, and to preliminarily determine that the stirring intensity of the stirring tank does not meet the requirements when the weight difference between the extract and the matrix and the aquatic product raw material only meets the second weight difference condition, and to make a secondary determination on the stirring intensity of the stirring tank according to the actual centrifugal speed of the mixed solution;

[0022] The control module is connected to the stirring tank, and is used to stir the aquatic product sample and the extraction solvent according to the operation mode when the weight difference between the extract and the matrix and the aquatic product raw material only meets the first weight difference condition;

[0023] Among them, the first weight difference condition is that the weight difference between the extract and the matrix and the aquatic product raw material is greater than the preset first weight difference and less than or equal to the preset second weight difference; the second weight difference condition is that the weight difference between the extract and the matrix and the aquatic product raw material is greater than the preset second weight difference.

[0024] Further, the working mode is that the vertical connecting rod stirs the aquatic product sample and the extraction solvent according to the adjusted descending rate;

[0025] The adjusted decreasing rate is determined by the difference between the weight difference of the extract and the matrix and the aquatic product raw material and a preset first weight difference.

[0026] Furthermore, the filtering component includes a liquid outlet pipe for outputting the extract, and the control module is connected to the detection module and the liquid outlet pipe respectively, so as to secondarily determine that the stirring intensity of the stirring tank does not meet the requirements when the actual centrifugal speed of the mixed liquid is greater than the preset speed, and output the extract according to the working mode;

[0027] Wherein, the working mode is that the liquid outlet pipe outputs the extract according to the adjusted valve opening; the adjusted valve opening is determined by the difference between the actual centrifugal speed of the mixed liquid and the preset speed.

[0028] The present invention also provides a method for detecting drug residues in aquatic products, comprising the following steps:

[0029] Using a stirring tank to mix the crushed aquatic product sample and the extraction solvent to output a mixed solution, and using a sieve to filter the mixed solution to output an extract and a matrix;

[0030] Outputting the extract using a liquid outlet pipe, transporting the extract to a liquid storage tank using a water pump, and detecting the concentration of residual drugs in the extract using a high performance liquid chromatograph;

[0031] When the accuracy of drug residue detection is determined to be not satisfactory based on the average difference in residual drug concentration, the water pump startup method is adjusted, or the weight of the extract and the matrix and the weight of the aquatic product raw material are obtained respectively;

[0032] Adjusting the descending rate of the vertical connecting rod based on the average difference in residual drug concentration and the weight difference between the extract and the matrix and the aquatic product raw material, or obtaining the actual centrifugal speed of the mixed solution;

[0033] The valve opening of the liquid outlet pipe is adjusted based on the actual centrifugal speed of the mixed liquid.

[0034] Compared with the prior art, the beneficial effect of the present invention lies in that the device of the present invention, by setting a separation module, a conveying module, a detection module and a control module, adjusts the starting mode of the water pump according to the average difference in the residual drug concentration. Since the starting mode of the water pump is initially auto-start, heat is generated during the operation of the water pump, causing some components in the extract to change, thereby causing the accuracy of the detection to decrease. By changing the starting mode of the water pump, the influence of the change of the extract components due to the influence of the water pump and the decrease in the detection accuracy is reduced. By adjusting the operating mode of the stirring tank according to the weight difference between the extract and the matrix and the aquatic product raw material, since the extract is in the filtration process, the Frictional heat is generated when passing through the screen, and bubbles appear in some of the screen holes, resulting in some extract residue in the screen. By increasing the descending rate of the vertical connecting rod and increasing the downward impact of the stirring paddle, the bubbles are burst, thereby reducing the impact of the loss of drug components in the extract due to the appearance of bubbles. By adjusting the working mode of the filter component according to the actual centrifugal speed of the mixed liquid, the stirring intensity of the stirring device decreases due to the wear of the stirring device, resulting in some drugs still remaining in the crushed aquatic products. By increasing the valve opening of the liquid outlet pipe, the impact of inaccurate detection due to problems with the stirring device is reduced, thereby achieving improved accuracy in drug residue detection.

[0035] Furthermore, the device described in the present invention adjusts the starting mode of the water pump by setting a preset first difference amount and a preset second difference amount. Since the starting mode of the water pump is initially auto-start, heat is generated during the operation of the water pump, causing some components in the extract to change, thereby resulting in a decrease in detection accuracy. By changing the starting mode of the water pump, the impact of changes in the extract components due to the influence of the water pump, thereby reducing detection accuracy, further achieving improved accuracy in drug residue detection.

[0036] Furthermore, the device described in the present invention adjusts the descending rate of the vertical connecting rod by setting a preset first weight difference and a preset second weight difference. Since friction heat is generated when the extract passes through the screen during the filtration process, bubbles appear in some of the screen holes, resulting in some extract remaining in the screen. By increasing the descending rate of the vertical connecting rod and increasing the downward impact of the stirring paddle, the bubbles burst, thereby reducing the impact of the loss of drug components in the extract due to the appearance of bubbles, and further achieving improved accuracy in drug residue detection.

[0037] Furthermore, the device described in the present invention adjusts the valve opening of the liquid outlet pipe by setting a preset rotation speed. Due to the wear of the stirring device, the stirring intensity of the stirring device decreases, which causes some drugs to remain in the crushed aquatic product. By increasing the valve opening of the liquid outlet pipe, the impact of inaccurate detection caused by problems with the stirring device is reduced, thereby further achieving improved accuracy in drug residue detection. BRIEF DESCRIPTION OF THE DRAWINGS

[0038] Figure 1 This is a schematic diagram of the overall structure of a device for detecting drug residues in aquatic products according to an embodiment of the present invention;

[0039] Figure 2 This is a block diagram of the overall structure of a device for detecting drug residues in aquatic products according to an embodiment of the present invention;

[0040] Figure 3 This is an overall flow chart of the method for detecting drug residues in aquatic products according to an embodiment of the present invention;

[0041] Figure 4 This is a specific structural block diagram of a conveying module of a device for detecting drug residues in aquatic products according to an embodiment of the present invention;

[0042] The accompanying drawings are marked as follows: 1-workbench, 2-support rod, 3-screen, 4-stirring paddle, 5-stirring tank, 6-Hall effect sensor, 7-electric telescopic rod, 8-vertical connecting rod, 9-first weight sensor, 10-liquid storage tank, 11-high performance liquid chromatograph, 12-second weight sensor, 13-water pump, 14-delivery pipe, 15-electric valve, 16-liquid outlet pipe. DETAILED DESCRIPTION

[0043] In order to make the objects and advantages of the present invention more clearly understood, the present invention is further described below in conjunction with embodiments; it should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0044] The preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only used to explain the technical principles of the present invention and are not intended to limit the protection scope of the present invention.

[0045] It should be noted that, in the description of the present invention, terms such as "up", "down", "left", "right", "inside" and "outside" indicating directions or positional relationships are based on the directions or positional relationships shown in the drawings. This is merely for the convenience of description and does not indicate or imply that the device or element must have a specific orientation, be constructed and operated in a specific orientation. Therefore, it cannot be understood as a limitation on the present invention.

[0046] In addition, it should be noted that in the description of the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For those skilled in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0047] See also Figure 1 , Figure 2 , Figure 3 as well as Figure 4 As shown, they are respectively an overall structural schematic diagram, an overall structural block diagram, an overall flow chart, and a specific structural block diagram of a conveying module of a drug residue detection device and method in an embodiment of the present invention. A drug residue detection device in aquatic products of the present invention comprises:

[0048] A separation module, used to separate the aquatic product sample into an extract and a matrix, including a stirring tank 5 for mixing the aquatic product sample and the extraction solvent to output a mixed solution and a filtering component connected to the stirring tank 5 for filtering the mixed solution to output an extract;

[0049] A conveying module connected to the separation module for conveying the extract, including a conveying component connected to the filter component for conveying the extract to a storage location, wherein the conveying component includes a water pump 13 for controlling the conveying power of the extract;

[0050] A detection module, which is connected to the separation module and the delivery module, respectively, and is used to detect the weight of the matrix, the weight of the extract, the centrifugal speed of the mixed solution, and the concentration of the residual drug;

[0051] A control module, which is respectively connected to the separation module, the delivery module and the detection module, and is used to adjust the start mode of the water pump 13 when it is determined that the accuracy of the drug residue detection does not meet the requirements according to the average difference in the residual drug concentration, or to preliminarily determine that the loss degree of the drug in the filtration process does not meet the requirements and to secondarily determine the loss degree of the drug in the filtration process according to the weight difference between the extract and the matrix and the aquatic product raw material;

[0052] Also, when it is determined that the loss degree of the drug in the filtration process does not meet the requirements, the operation mode of the stirring tank is adjusted, or the working mode of the filtration component is determined according to the actual centrifugal speed of the mixed liquid.

[0053] Specifically, the filtering components also include:

[0054] A screen 3, which is arranged above the liquid outlet pipe 16 and is used to filter the mixed liquid;

[0055] The electric valve 15 is connected to the liquid outlet pipe 16 to control the output flow rate of the extraction liquid.

[0056] Specifically, the delivery assembly further includes a delivery pipe 14 connected to the liquid outlet pipe 16 for delivering the extraction liquid.

[0057] Specifically, a device for detecting drug residues in aquatic products also includes:

[0058] A support rod 2, which is connected to the mixing tank 5 and is used to support the mixing tank 5;

[0059] The workbench 1 is connected to the support rod 2 to provide a detection position.

[0060] Specifically, aquatic products include salmon, scallops, and prawns.

[0061] Specifically, the residual drugs in aquatic products include chloramphenicol, furazolidone, and florfenicol. When the aquatic product is scallop, the chloramphenicol content is the highest.

[0062] Specifically, the extraction solvent is used to separate the residual drugs in the aquatic product from the aquatic product. The extraction solvent includes methanol, acetonitrile, and ethyl acetate. The preferred embodiment of the present invention is acetonitrile, and its chemical formula is CH3CN.

[0063] Specifically, the reaction mechanism of acetonitrile extraction of residual drugs in aquatic products is to separate hydrophobic drug molecules from aquatic products through hydrophobic interactions.

[0064] Specifically, the components of the mixed liquid include protein, fat, amino acid and acetonitrile.

[0065] Specifically, the components of the extract include chloramphenicol, amino acids, and acetonitrile.

[0066] In practice, the device of the present invention is provided with a separation module, a conveying module, a detection module and a control module, and the starting mode of the water pump 13 is adjusted according to the average difference in the residual drug concentration. Since the starting mode of the water pump 13 is initially auto-start, heat is generated during the operation of the water pump 13, causing some components in the extract to change, thereby causing the detection accuracy to decrease. By changing the starting mode of the water pump 13, the influence of the change in the extract components due to the influence of the water pump 13 and the decrease in detection accuracy is reduced. By adjusting the operation mode of the stirring tank according to the weight difference between the extract and the matrix and the aquatic product raw material, since the extract passes through the screen during the filtration process, the 3, friction heat is generated, bubbles appear in some holes of the screen 3, resulting in some extract residue in the screen 3. By increasing the descending rate of the vertical connecting rod 8 and increasing the downward impact of the stirring paddle 4, the bubbles are broken, thereby reducing the impact of the loss of drug components in the extract due to the appearance of bubbles. By adjusting the working mode of the filter assembly according to the actual centrifugal speed of the mixed solution, the stirring intensity of the stirring device decreases due to the wear of the stirring device, resulting in some drugs still remaining in the crushed aquatic product. By increasing the valve opening of the liquid outlet pipe 16, the impact of inaccurate detection due to problems with the stirring device is reduced, thereby achieving improved accuracy in drug residue detection.

[0067] Specifically, the delivery module further includes a liquid storage component connected to the delivery component for storing the extraction liquid, and the liquid storage component is a liquid storage tank 10.

[0068] Specifically, the stirring tank 5 comprises:

[0069] A vertical connecting rod 8, which is arranged inside the stirring tank 5 and is used to control the stirring height;

[0070] A stirring paddle 4, which is connected to the vertical connecting rod 8 and is used to stir the aquatic product sample and the extraction solvent;

[0071] The electric telescopic rod 7 is connected to the vertical connecting rod 8 and changes the descending speed of the vertical connecting rod 8 by changing the telescopic speed.

[0072] Specifically, the detection module includes:

[0073] A first weight sensor 9, which is arranged below the stirring tank 5 and is used to detect the weight of the substrate in the stirring tank 5;

[0074] A second weight sensor 12, which is disposed below the liquid storage tank 10 and is used to detect the weight of the extracted liquid in the liquid storage tank 10;

[0075] A Hall effect sensor 6 connected to the vertical connecting rod 8 for detecting the actual centrifugal speed of the mixed liquid;

[0076] A high performance liquid chromatograph 11 is disposed at the output end of the liquid storage tank 10 and is used to detect the concentration of residual drugs in the aquatic product raw material.

[0077] Specifically, the control module is connected to the high performance liquid chromatograph 11, and is used to calculate the average difference of the residual drug concentration according to the residual drug concentrations detected several times, and to determine that the accuracy of the drug residue detection does not meet the requirements when the average difference of the residual drug concentration meets the first difference condition or the second difference condition;

[0078] The control module is connected to the detection module, and is used to preliminarily determine that the loss degree of the drug in the filtration process does not meet the requirements when the average difference amount of the residual drug concentration only meets the first difference amount condition, and to perform a secondary determination on the loss degree of the drug in the filtration process according to the weight difference between the extract and the matrix and the aquatic product raw material;

[0079] Among them, the first difference condition is that the average difference in residual drug concentration is greater than the preset first difference and less than or equal to the preset second difference; the second difference condition is that the average difference in residual drug concentration is greater than the preset second difference.

[0080] It can be understood that the three intervals corresponding to the preset first difference amount and the preset second difference amount correspond to three situations respectively. The first situation is that the average difference amount of residual drug concentration is less than or equal to the preset first difference amount, and it is judged that the accuracy of drug residue detection meets the requirements; the second situation is that the average difference amount of residual drug concentration is greater than the preset first difference amount and less than or equal to the preset second difference amount, and it is preliminarily judged that the degree of drug loss in the filtration process does not meet the requirements, and a secondary judgment is made on the degree of drug loss in the filtration process based on the weight difference between the extract and the matrix and the aquatic product raw material; the third situation is that the average difference amount of residual drug concentration is greater than the preset second difference amount, and the starting method of the water pump 13 is adjusted.

[0081] Optionally, a preferred embodiment of the preset first difference amount Q1 is Q1=0.3 mg / L, and a preferred embodiment of the preset second difference amount Q2 is Q2=0.5 mg / L.

[0082] Specifically, the average difference in residual drug concentration is recorded as Q, and the difference between the average difference in residual drug concentration and a preset second difference is recorded as ΔQ, and ΔQ=Q-Q2 is set.

[0083] Specifically, the average difference in residual drug concentration was calculated as:

[0084]

[0085] Among them, Q is the average difference in residual drug concentration, |X a -X a-1 | is the absolute value of the difference between the concentration of residual drugs detected at the a-th time and the concentration of residual drugs detected at the a-1-th time, n is the number of detections of the residual drug concentration, and n is a natural number greater than or equal to 2.

[0086] In implementation, the device of the present invention determines the accuracy of drug residue detection by setting a preset first difference amount and a preset second difference amount, thereby reducing the impact of the decreased stability of drug residue detection due to inaccurate judgment of the accuracy of drug residue detection, and further achieving an improvement in the accuracy of drug residue detection.

[0087] Specifically, the control module is connected to the water pump 13, and is used to adjust the start-up mode of the water pump 13 when the average difference amount of the residual drug concentration only meets the second difference amount condition;

[0088] The starting mode of the water pump 13 is adjusted from auto-coupling starting to star-delta starting.

[0089] Specifically, the specific process of adjusting the starting mode of the water pump from auto-coupling starting to star-delta starting is as follows: the frequency converter connected to the water pump motor adjusts the operating state of the water pump accordingly according to the load condition of the water pump. When the heat increases during the operation of the water pump, the starting mode of the water pump is changed by changing the voltage and frequency of the water pump motor, and adjusted from auto-coupling starting to star-delta starting.

[0090] In implementation, the device of the present invention adjusts the starting mode of the water pump 13 by setting a preset first difference amount and a preset second difference amount. Since the starting mode of the water pump 13 is initially auto-start, heat is generated during the operation of the water pump 13, causing some components in the extract to change, thereby resulting in a decrease in the accuracy of detection. By changing the starting mode of the water pump 13, the influence of the change in the extract components caused by the influence of the water pump 13 and the decrease in detection accuracy is reduced, thereby further achieving an improvement in the accuracy of drug residue detection.

[0091] Specifically, the control module is connected to the detection module, and is used to make a secondary determination that the degree of drug loss in the filtration process does not meet the requirements when the weight difference between the extract and the matrix and the aquatic product raw material meets the first weight difference condition or the second weight difference condition, and to preliminarily determine that the stirring intensity of the stirring tank 5 does not meet the requirements when the weight difference between the extract and the matrix and the aquatic product raw material only meets the second weight difference condition, and to make a secondary determination on the stirring intensity of the stirring tank 5 according to the actual centrifugal speed of the mixed solution;

[0092] The control module is connected to the stirring tank, and is used to stir the aquatic product sample and the extraction solvent according to the operation mode when the weight difference between the extract and the matrix and the aquatic product raw material only meets the first weight difference condition;

[0093] Among them, the first weight difference condition is that the weight difference between the extract and the matrix and the aquatic product raw material is greater than the preset first weight difference and less than or equal to the preset second weight difference; the second weight difference condition is that the weight difference between the extract and the matrix and the aquatic product raw material is greater than the preset second weight difference.

[0094] It can be understood that the three intervals corresponding to the preset first weight difference and the preset second weight difference correspond to three situations respectively. The first situation is that the weight difference between the extract and the matrix and the aquatic product raw material is less than or equal to the preset first weight difference, and the secondary judgment is that the degree of drug loss in the filtration process meets the requirements; the second situation is that the weight difference between the extract and the matrix and the aquatic product raw material is greater than the preset first weight difference and less than or equal to the preset second weight difference, and the aquatic product sample and the extraction solvent are stirred according to the operating mode; the third situation is that the weight difference between the extract and the matrix and the aquatic product raw material is greater than the preset second weight difference, and it is preliminarily judged that the stirring intensity of the stirring tank 5 does not meet the requirements, and the stirring intensity of the stirring tank 5 is secondary judged according to the actual centrifugal speed of the mixed liquid.

[0095] Optionally, a preferred embodiment of the preset first weight difference P1 is P1=1 kg, and a preferred embodiment of the preset second weight difference P2 is P2=2 kg.

[0096] Specifically, the weight difference between the extract and the matrix and the aquatic product raw material is recorded as P, and the difference between the weight difference between the extract and the matrix and the aquatic product raw material and the preset first weight difference is recorded as △P, and △P=P-P1 is set.

[0097] Specifically, the weight difference between the extract and the matrix and the aquatic product raw material is calculated as follows:

[0098] P=S1-S2

[0099] Wherein, P is the weight difference between the extract and the matrix and the aquatic product raw material, S1 is the sum of the weight of the extract in the storage tank and the weight of the matrix in the stirring tank, and S2 is the weight of the aquatic product raw material.

[0100] In implementation, the device of the present invention performs a secondary judgment on the degree of drug loss in the filtration process by setting a preset first weight difference and a preset second weight difference, thereby reducing the impact of the reduced accuracy of drug residue detection due to inaccurate secondary judgment on the degree of drug loss in the filtration process, and further improving the accuracy of drug residue detection.

[0101] Specifically, the working method is that the vertical connecting rod 8 stirs the aquatic product sample and the extraction solvent according to the adjusted descending rate;

[0102] The adjusted decreasing rate is determined by the difference between the weight difference of the extract and the matrix and the aquatic product raw material and a preset first weight difference.

[0103] Specifically, the specific process of determining the descending rate of the vertical connecting rod 8 by the difference between the weight difference of the extract and the matrix and the aquatic product raw material and the preset first weight difference is:

[0104] If ΔP≤ΔP0, the control module uses a preset first descent rate adjustment coefficient to adjust the descent rate of the vertical connecting rod 8 to a first descent rate;

[0105] If ΔP>ΔP0, the control module uses a preset second descent rate adjustment coefficient to adjust the descent rate of the vertical connecting rod 8 to a second descent rate;

[0106] Wherein, the preset first descent rate adjustment coefficient is smaller than the preset second descent rate adjustment coefficient.

[0107] Optionally, a preferred embodiment of the preset weight difference value ΔP0 is ΔP0=0.5 kg.

[0108] Specifically, the preset first descent rate adjustment coefficient is recorded as α1, and α1 is set to 1.2. The preset second descent rate adjustment coefficient is recorded as α2, and α2 is set to 1.4. The descent rate of the vertical connecting rod 8 is recorded as V, wherein 1<α1<α2. The descent rate of the adjusted vertical connecting rod 8 is recorded as V', and V' is set to V×(1+αi) / 2, wherein αi is the preset i-th descent rate adjustment coefficient, and i is set to 1, 2.

[0109] In practice, the device of the present invention adjusts the descending rate of the vertical connecting rod 8 by setting a preset first weight difference and a preset second weight difference. Since the extract generates friction heat when passing through the screen 3 during the filtration process, bubbles appear in some holes of the screen 3, resulting in some extract remaining in the screen 3. By increasing the descending rate of the vertical connecting rod 8 and increasing the downward impact of the stirring paddle 4, the bubbles are burst, thereby reducing the impact of the loss of drug components in the extract due to the appearance of bubbles, and further achieving improved accuracy in drug residue detection.

[0110] Specifically, the filtering component includes a liquid outlet pipe 16 for outputting the extract, and the control module is respectively connected to the detection module and the liquid outlet pipe 16, so as to secondary determine that the stirring intensity of the stirring tank 5 does not meet the requirements when the actual centrifugal speed of the mixed liquid is greater than the preset speed, and output the extract according to the working mode.

[0111] It can be understood that the two intervals corresponding to the preset speed correspond to two situations respectively. The first situation is that the actual centrifugal speed of the mixed liquid is less than or equal to the preset speed, and the secondary judgment is that the stirring intensity of the stirring tank 5 meets the requirements; the second situation is that the actual centrifugal speed of the mixed liquid is greater than the preset speed, and the extract is output according to the working mode.

[0112] Optionally, a preferred embodiment of the preset rotation speed Y0 is Y0=50 r / min.

[0113] Specifically, the actual centrifugal speed of the mixed liquid is recorded as Y, and the difference between the actual centrifugal speed of the mixed liquid and the preset speed is recorded as ΔY, and ΔY=Y0-Y is set.

[0114] In practice, the device of the present invention performs a secondary determination on the stirring intensity of the stirring tank 5 by setting a preset rotation speed, thereby reducing the impact of the reduced accuracy of drug residue detection due to inaccurate secondary determination of the stirring intensity of the stirring tank 5, and further improving the accuracy of drug residue detection.

[0115] Specifically, the working method is that the liquid outlet pipe 16 outputs the extraction liquid according to the adjusted valve opening;

[0116] The adjusted valve opening is determined by the difference between the actual centrifugal speed of the mixed liquid and the preset speed.

[0117] Specifically, the specific process of determining the valve opening of the discharge pipe by the difference between the actual centrifugal speed of the mixed liquid and the preset speed is as follows:

[0118] If △Y≤△Y0, the control module uses a preset first valve opening adjustment coefficient to adjust the valve opening of the discharge pipe to the first valve opening;

[0119] If △Y>△Y0, the control module uses a preset second valve opening adjustment coefficient to adjust the valve opening of the discharge pipe to the second valve opening;

[0120] Wherein, the preset first valve opening adjustment coefficient is smaller than the preset second valve opening adjustment coefficient.

[0121] Optionally, a preferred embodiment of the preset rotation speed difference ΔY0 is ΔY0=10 r / min.

[0122] Specifically, the preset first valve opening adjustment coefficient is recorded as β1, and β1 is set to 1.1. The preset second valve opening adjustment coefficient is recorded as β2, and β2 is set to 1.3. The valve opening of the discharge pipe is recorded as H, wherein 1<β1<β2. The valve opening of the discharge pipe after adjustment is recorded as H', and H' is set to H×(1+2βj) / 3, wherein βj is the preset jth valve opening adjustment coefficient, and j is set to 1, 2.

[0123] In practice, the device of the present invention adjusts the valve opening of the liquid outlet pipe 16 by setting a preset rotation speed. Due to the wear of the stirring device, the stirring intensity of the stirring device decreases, which causes some drugs to remain in the crushed aquatic product. By increasing the valve opening of the liquid outlet pipe 16, the impact of inaccurate detection caused by problems with the stirring device is reduced, thereby further achieving improved accuracy in drug residue detection.

[0124] A method for detecting drug residues in aquatic products comprises the following steps:

[0125] Step S1, using a stirring tank 5 to mix the crushed aquatic product sample and the extraction solvent to output a mixed solution, and using a sieve 3 to filter the mixed solution to output an extract and a matrix;

[0126] Step S2, outputting the extract using the liquid outlet pipe 16, conveying the extract to the liquid storage tank 10 using the water pump 13, and detecting the concentration of residual drugs in the extract using the high performance liquid chromatograph 11;

[0127] Step S3, when it is determined based on the average difference in the residual drug concentration that the accuracy of the drug residue detection does not meet the requirements, the starting mode of the water pump 13 is adjusted, or the weight of the extract and the matrix and the weight of the aquatic product raw material are obtained respectively;

[0128] Step S4, adjusting the descending speed of the vertical connecting rod 8 based on the average difference in residual drug concentration and the weight difference between the extract and the matrix and the aquatic product raw material, or obtaining the actual centrifugal speed of the mixed solution;

[0129] Step S5, adjusting the valve opening of the liquid outlet pipe 16 based on the actual centrifugal speed of the mixed liquid.

[0130] Example 1

[0131] In this embodiment 1, a device for detecting drug residues in aquatic products is used to detect aquatic products. The control module adjusts the descending rate of the vertical connecting rod according to the difference between the weight difference between the extract and the matrix and the aquatic product raw material and the preset first weight difference, wherein the preset first descending rate adjustment coefficient is recorded as α1, the preset second descending rate adjustment coefficient is recorded as α2, and the descending rate of the vertical connecting rod is recorded as V, wherein 1<α1<α2, α1=1.2, α2=1.4, △P0=0.5kg, V=4cm / min, P=2.5kg, P1=1kg, △P=P-P1.

[0132] In this embodiment 1, ΔP=1.5 kg is obtained, the control module determines that ΔP>ΔP0 and uses the preset first descent rate adjustment coefficient to adjust the descent rate of the vertical connecting rod to the second descent rate, and calculates that V'=4 cm / min×(1+1.2) / 2=4.4 cm / min.

[0133] So far, the technical solutions of the present invention have been described in conjunction with the preferred embodiments shown in the accompanying drawings. However, it is easy for those skilled in the art to understand that the protection scope of the present invention is obviously not limited to these specific embodiments. Without departing from the principle of the present invention, those skilled in the art can make equivalent changes or substitutions to the relevant technical features, and the technical solutions after these changes or substitutions will fall within the protection scope of the present invention.

Claims

1. A drug residue detection device in aquatic products, characterized in that: include: A separation module, used for separating the aquatic product sample into an extract and a matrix, comprising a stirring tank for mixing the aquatic product sample and the extraction solvent to output a mixed solution and a filtering component connected to the stirring tank for filtering the mixed solution to output an extract; A conveying module connected to the separation module for conveying the extract, comprising a conveying component connected to the filter component for conveying the extract to a storage location, wherein the conveying component comprises a water pump for controlling the conveying power of the extract; A detection module, which is connected to the separation module and the delivery module, respectively, and is used to detect the weight of the matrix, the weight of the extract, the centrifugal speed of the mixed solution, and the concentration of the residual drug; A control module, which is connected to the separation module, the delivery module and the detection module respectively, and is used to adjust the starting mode of the water pump when it is determined that the accuracy of the drug residue detection does not meet the requirements according to the average difference in the residual drug concentration, or to preliminarily determine that the loss degree of the drug in the filtration process does not meet the requirements and to secondarily determine the loss degree of the drug in the filtration process according to the weight difference between the extract and the matrix and the aquatic product raw material; and, when it is determined that the loss degree of the drug in the filtration process does not meet the requirements, adjusting the operation mode of the stirring tank, or determining the working mode of the filtration component according to the actual centrifugal speed of the mixed liquid; The stirring tank comprises: A vertical connecting rod, which is arranged inside the stirring tank and is used to control the stirring height; A stirring paddle connected to the vertical connecting rod for stirring the aquatic product sample and the extraction solvent; An electric telescopic rod connected to the vertical connecting rod, which changes the descending rate of the vertical connecting rod by changing the telescopic rate; The control module is used to calculate an average difference amount of the residual drug concentration according to the residual drug concentrations detected several times, and to determine that the accuracy of the drug residue detection does not meet the requirements when the average difference amount of the residual drug concentration meets the first difference amount condition or the second difference amount condition; The control module is used to preliminarily determine that the loss degree of the drug in the filtration process does not meet the requirements when the average difference amount of the residual drug concentration only meets the first difference amount condition, and to perform a secondary determination on the loss degree of the drug in the filtration process according to the weight difference between the extract and the matrix and the aquatic product raw material; The first difference condition is that the average difference of the residual drug concentration is greater than the preset first difference and less than or equal to the preset second difference; the second difference condition is that the average difference of the residual drug concentration is greater than the preset second difference; The control module is connected to the water pump and is used to adjust the start-up mode of the water pump when the average difference in the residual drug concentration only meets the second difference condition; Wherein, the starting mode of the water pump is adjusted from auto-coupling starting to star-angle starting; The control module is used to make a secondary determination that the degree of drug loss during the filtration process does not meet the requirements when the weight difference between the extract and the matrix and the aquatic product raw material meets the first weight difference condition or the second weight difference condition, and to make a preliminary determination that the stirring intensity of the stirring tank does not meet the requirements when the weight difference between the extract and the matrix and the aquatic product raw material only meets the second weight difference condition, and to make a secondary determination on the stirring intensity of the stirring tank according to the actual centrifugal speed of the mixed solution; The control module is connected to the stirring tank, and is used to stir the aquatic product sample and the extraction solvent according to the operation mode when the weight difference between the extract and the matrix and the aquatic product raw material only meets the first weight difference condition; Wherein, the first weight difference condition is that the weight difference between the extract and the matrix and the aquatic product raw material is greater than the preset first weight difference and less than or equal to the preset second weight difference; the second weight difference condition is that the weight difference between the extract and the matrix and the aquatic product raw material is greater than the preset second weight difference; The operation mode is that the vertical connecting rod stirs the aquatic product sample and the extraction solvent according to the adjusted descending rate; Wherein, the adjusted decreasing rate is determined by the difference between the weight difference of the extract and the matrix and the aquatic product raw material and the preset first weight difference; The filtering component includes a liquid outlet pipe for outputting the extract, and the control module is connected to the detection module and the liquid outlet pipe respectively, so as to secondarily determine that the stirring intensity of the stirring tank does not meet the requirements when the actual centrifugal speed of the mixed liquid is greater than the preset speed, and output the extract according to the working mode; Wherein, the working mode is that the liquid outlet pipe outputs the extract according to the adjusted valve opening; the adjusted valve opening is determined by the difference between the actual centrifugal speed of the mixed liquid and the preset speed.

2. The drug residue detection device in aquatic products according to claim 1, characterized in that: The delivery module also includes a liquid storage component connected to the delivery component for storing the extraction liquid, and the liquid storage component is a liquid storage tank.

3. The drug residue detection device in aquatic products according to claim 2, characterized in that: The detection module comprises: A first weight sensor, which is disposed below the stirring tank and is used to detect the weight of the substrate in the stirring tank; A second weight sensor is disposed below the liquid storage tank and is used to detect the weight of the extracted liquid in the liquid storage tank; A Hall effect sensor connected to the vertical connecting rod to detect the actual centrifugal speed of the mixed liquid; A high performance liquid chromatograph is arranged at the output end of the liquid storage tank and is used to detect the concentration of residual drugs in the aquatic product raw materials.

4. The drug residue detection device in aquatic products according to claim 3, characterized in that: The control module is connected to the high performance liquid chromatograph.

5. A method for detecting drug residues in aquatic products applied to the drug residue detection device in aquatic products according to any one of claims 1 to 4, characterized in that: The following steps are involved: Using a stirring tank to mix the crushed aquatic product sample and the extraction solvent to output a mixed solution, and using a sieve to filter the mixed solution to output an extract and a matrix; Outputting the extract using a liquid outlet pipe, delivering the extract to a liquid storage tank using a water pump, and detecting the concentration of residual drugs in the extract using a high performance liquid chromatograph; When the accuracy of drug residue detection is determined to be not satisfactory based on the average difference in residual drug concentration, the water pump startup method is adjusted, or the weight of the extract and the matrix and the weight of the aquatic product raw material are obtained respectively; Adjusting the descending rate of the vertical connecting rod based on the average difference in residual drug concentration and the weight difference between the extract and the matrix and the aquatic product raw material, or obtaining the actual centrifugal speed of the mixed solution; The valve opening of the liquid outlet pipe is adjusted based on the actual centrifugal speed of the mixed liquid.

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