Detection system and method for clenbuterol residues

By providing a detection system including pretreatment and automatic sampling device, the problem of false positive detection of clenbuterol residues and short drug residue period in the prior art is solved, and a rapid and automated detection process is realized, and the detection is improved Efficiency and accuracy.

CN114397150BActive Publication Date: 2025-02-25CHINA INNOVATION INSTR CO LTD
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Patent Information

Application Number
CN202111468196.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2021-12-03
Publication Date
2025-02-25
Estimated Expiration
2041-12-03

AI Technical Summary

Technical Problem

The prior art has false positive problems in detecting clenbuterol residues and short drug residue periods, which are difficult to achieve real-time tracking and monitoring. The chromatography detection process takes a long time and high requirements for equipment and operators.

Method used

A detection system including a pretreatment device and a sampling device is provided. An animal hair sample is processed through steps such as cleaning, cutting, grinding and automatic injection, and the detection is performed using a mass spectrometer to realize automated sampling and detection.

Benefits of technology

Through wet grinding, the sample extract is quickly and simply obtained, which reduces the detection cost and requirements for the professional quality of the operator, realizes a high-throughput, automated detection process, and improves detection efficiency and accuracy.

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Abstract

The present invention provides a detection system and method for clenbuterol residues, the detection system for clenbuterol residues comprising a bracket, an ion source and a mass spectrometer, a first guide rail arranged on the bracket comprising a connected first part and a second part inclined downward, a second guide rail arranged on the bracket, a first bearing member arranged on the second guide rail; a sliding member arranged on the first guide rail and connected to a rotating shaft, the rotating shaft rotatably arranged on the first bearing member, the central axis of the sliding member and the central axis of the rotating shaft arranged in parallel and not in a colinear manner; a first translation device fixed on the bracket, used to drive the first bearing member to move forward and reversely; a second translation device arranged on the bracket, used to drive the dilution unit to move forward and reversely; a second bearing member fixedly connected to the rotating shaft, a third translation device arranged on the second bearing member, used to drive the ion source to move forward and reversely. The present invention has the advantages of automation and the like.
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Description

Technical Field

[0001] The invention relates to clenbuterol detection, and in particular to a detection system and method for clenbuterol residues. Background Art

[0002] Clenbuterol is a general term for a class of drugs. Any substance that can inhibit animal fat production and promote lean meat growth can be called clenbuterol. The substances that can achieve this function are mainly a class of drugs called β-receptor agonists (also known as β-stimulants), the more common ones are clenbuterol, salbutamol, ractopamine, cimaterol and terbutaline. This type of clenbuterol, after entering the body of livestock, can change the metabolic pathway of nutrients, promote animal muscle growth, especially promote the synthesis of skeletal muscle protein, accelerate the conversion and decomposition of fat, and increase the lean meat rate of livestock.

[0003] In recent years, there have been many cases of poisoning caused by eating food contaminated with clenbuterol, and the consequences are extremely serious, which has attracted great attention from countries around the world. In order to ensure the quality and safety of livestock products and protect human health, many countries have banned the use of clenbuterol hydrochloride in the production of food-producing animals. The US Food and Drug Administration (FDA) has made clenbuterol hydrochloride residues in meat a mandatory inspection item, and the EU also strictly prohibits the addition of clenbuterol drugs to feed. Although my country proposed to ban the use of clenbuterol drugs in 2000, the use of clenbuterol in animal husbandry production is still rampant.

[0004] In the prior art, the method for detecting clenbuterol is:

[0005] 1. Detect animal urine. For pig urine, enzyme-linked immunosorbent assay or gold-labeled test paper method is often used for screening, but there are false positive problems, and the method of directly collecting pig urine for testing has the problem of short drug residue cycle, making it difficult to achieve real-time tracking and monitoring of drug residues.

[0006] 2. To detect animal muscle tissue, the internationally common detection method is chromatography, which includes high performance liquid chromatography (HPLC), gas chromatography-mass spectrometry (GC-MS), liquid chromatography-mass spectrometry (LC-MS), thin layer chromatography and gas chromatography-Fourier transform infrared spectroscopy, etc. However, since chromatography has high requirements on instruments and operators and is time-consuming, it is often used as a confirmation test method during the detection process. Summary of the invention

[0007] In order to solve the deficiencies in the above-mentioned prior art solutions, the present invention provides a detection system for clenbuterol residues.

[0008] The objective of the present invention is achieved through the following technical solutions:

[0009] A detection system for clenbuterol residues, the detection system for clenbuterol residues comprising a bracket and a mass spectrometer, wherein the mass spectrometer is arranged on the bracket; the detection system for clenbuterol residues further comprises:

[0010] A pre-treatment device, the pre-treatment device comprising a cleaning unit, a shearing unit and a grinding unit, the cleaning unit is used to clean the collected animal hair, the shearing unit is used to cut the cleaned animal hair, and the grinding unit is used to grind the cut animal hair;

[0011] A sampling device, the sampling device comprising:

[0012] A first guide rail, the first guide rail is arranged on the bracket, the first guide rail comprises a first part and a second part connected, and the second part is inclined downward;

[0013] a second guide rail and a first bearing member, wherein the second guide rail is arranged on the bracket, and the first bearing member is arranged on the second guide rail;

[0014] A sliding member and a rotating shaft, wherein the sliding member is disposed on the first guide rail and connected to the rotating shaft, the rotating shaft is rotatably disposed on the first bearing member, and the central axis of the sliding member and the central axis of the rotating shaft are disposed in parallel and are not collinear;

[0015] A first translation device, the first translation device is fixed to the bracket and is used to drive the first bearing member to move forward and reversely;

[0016] a second translation device and a dilution unit, wherein the second translation device is disposed on the bracket and is used to drive the dilution unit to move forward and backward, and an angle between a moving direction of the dilution unit and a moving direction of the first carrier is an acute angle or a right angle;

[0017] A second carrier and a third translation device, the second carrier is fixedly connected to the rotating shaft, and the third translation device is arranged on the second carrier, and is used to drive the capillary needle to move forward and reverse; when the sliding member moves from the first part to the working point of the second part, the capillary needle rotates with the rotating shaft, and rotates from a vertical state to a horizontal state.

[0018] Another object of the present invention is to provide a method for detecting clenbuterol residues using the above-mentioned clenbuterol residue detection system, and the object of the invention is achieved through the following technical solutions:

[0019] A method for detecting clenbuterol residues, the method comprising a cleaning stage, a shortening stage, a grinding stage, an automatic sampling stage and a detection stage;

[0020] The cleaning stage is to use a deionized water solution containing a surfactant and / or an organic solvent to clean the animal hair;

[0021] The shearing stage is to use a shearing unit to cut the cleaned animal hair into segments of 0.1 to 3 cm;

[0022] The grinding stage comprises grinding and centrifuging the cut animal hair, and reserving the supernatant for later use;

[0023] The automatic injection stage comprises the following steps:

[0024] (A1) The first translation device drives the first carrier to translate, the sliding member is in the first part of the first guide rail, and the capillary needle is in a vertical state;

[0025] The capillary needle is connected to a rotating shaft, the rotating shaft is rotatably disposed on the first bearing member and is fixedly connected to the sliding member, and the central axis of the sliding member and the central axis of the rotating shaft are arranged in parallel and not in a colinear relationship;

[0026] (A2) the second translation device drives the dilution unit so that the dilution unit is located at the lower side of the capillary needle;

[0027] (A3) The third translation device drives the capillary needle to move vertically downward, and the capillary needle enters the dilution unit to obtain the detection liquid;

[0028] (A4) the third translation device drives the capillary needle to move vertically upward, and the capillary needle is separated from the dilution unit;

[0029] (A5) The first translation device drives the first bearing member to translate, and the sliding member enters the second part of the inclined first guide rail and descends;

[0030] During the descending process, the capillary needle rotates around the rotation axis;

[0031] (A6) The sliding member moves to the working point of the second part, and the capillary needle is in a horizontal state.

[0032] Compared with the prior art, the present invention has the following beneficial effects:

[0033] 1. By processing the cut animal hair by wet grinding, the required animal hair sample extract can be obtained quickly, simply and with high throughput;

[0034] 2. Only cleaning, shortening and grinding are used in the pre-treatment. This treatment method does not require ultrasonic instruments, purge instruments and digestion solutions, thus reducing costs;

[0035] 3. The first translation device, the second translation device, the third translation device and the rotating device (composed of a sliding member, a first guide rail, a rotating shaft, a first bearing member and a second guide rail) are used to realize the relative three-dimensional movement of the capillary needle, such as the up and down, left and right translation and rotation of the capillary needle, and the front and back translation of the dilution unit, so that the dilution and injection (including sampling) of the solid sample are carried out automatically without manual intervention, which improves the work efficiency and reduces the professional quality requirements for the operator. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] The disclosure of the present invention will become easier to understand with reference to the accompanying drawings. It is easy for those skilled in the art to understand that these drawings are only used to illustrate the technical solution of the present invention and are not intended to limit the scope of protection of the present invention. In the drawings:

[0037] Figure 1 is a schematic structural diagram of a detection system for clenbuterol residues according to an embodiment of the present invention;

[0038] Figure 2 is a schematic structural diagram of a sample injection device according to an embodiment of the present invention;

[0039] Figure 3 is a schematic diagram of a partial structure of a sample injection device according to an embodiment of the present invention;

[0040] Figure 4 is a flow chart of a mass spectrometry analysis method based on automatic sampling according to an embodiment of the present invention;

[0041] Figure 5 is a schematic diagram of the consumable replacement state of the sampling device according to an embodiment of the present invention;

[0042] Figure 6 is a schematic diagram of a sampling state of a sampling device according to an embodiment of the present invention;

[0043] Figure 7 Schematic diagram of the injection state of the injection device according to an embodiment of the present invention. DETAILED DESCRIPTION

[0044] Figure 1-7 The following description describes the optional embodiments of the present invention to teach those skilled in the art how to implement and reproduce the present invention. In order to explain the technical solution of the present invention, some conventional aspects have been simplified or omitted. Those skilled in the art will understand that variations or replacements derived from these embodiments will be within the scope of the present invention. Those skilled in the art will understand that the following features can be combined in various ways to form multiple variations of the present invention. Thus, the present invention is not limited to the following optional embodiments, but is only limited by the claims and their equivalents.

[0045] Example 1

[0046] Figure 1 The structure diagram of the detection system for clenbuterol residues in Example 1 of the present invention is schematically shown. Figure 1 As shown, the detection system for clenbuterol residues comprises:

[0047] A pre-treatment device, the pre-treatment device comprising a cleaning unit, a shearing unit and a grinding unit, the cleaning unit is used to clean the collected animal hair, the shearing unit is used to cut the cleaned animal hair, and the grinding unit is used to grind the cut animal hair;

[0048] Injection device, such as Figure 2 As shown, the sample injection device comprises:

[0049] A support 11, on which a mass spectrometer 61 is arranged;

[0050] A first guide rail 21, wherein the first guide rail 21 is disposed on the bracket 11, and the first guide rail 21 includes a first portion and a second portion connected to each other, and the second portion is inclined downward;

[0051] A second guide rail 22 and a first bearing member 31, wherein the second guide rail 22 is disposed on the bracket 11, and the first bearing member 31 is disposed on the second guide rail 22;

[0052] A sliding member 81 and a rotating shaft 82, wherein the sliding member 81 is disposed on the first guide rail 21 and connected to the rotating shaft 82. Figure 3 As shown, the rotating shaft 82 is rotatably disposed on the first bearing member 31, and the central axis of the sliding member 81 and the central axis of the rotating shaft 82 are disposed in parallel and not in a colinear relationship, so that when the sliding member 81 slides in the second portion, the rotating shaft 82 is driven to rotate;

[0053] A first translation device 41, which is fixed to the bracket 11 and is used to drive the first bearing member 31 to move forward and backward, such as left and right translation, and the first bearing member 31 is translated to drag the sliding member 81 to move in the first guide rail 21, thereby driving the rotating shaft 82 to rotate;

[0054] A second translation device 42 and a dilution unit 71, wherein the second translation device 42 is disposed on the bracket 11 and is used to drive the dilution unit 71 to move forward and backward, such as to translate forward and backward, and the angle between the moving direction of the dilution unit 71 and the moving direction of the first carrier 31 is an acute angle or a right angle;

[0055] A second carrier 32 and a third translation device 43, wherein the second carrier 32 is fixedly connected to the rotating shaft 82, and the third translation device 43 is arranged on the second carrier 32, and is used to drive the ion source 51 (including the capillary needle) to move forward and reverse; when the sliding member 81 moves from the first part to the working point of the second part, the capillary needle rotates with the rotating shaft 82, and rotates from a vertical state (when the sliding member 81 is in the first part) to a horizontal state (when the sliding member 81 is at the working point).

[0056] In order to ensure that the capillary needle rotates from the vertical state to the horizontal state, further, the sliding member 81, the rotating shaft 82 and the first guide rail 21 meet the following conditions:

[0057] H=L(sinθ+cosθ), H is the height difference between the first part and the working point, L is the distance between the central axis of the sliding member 81 and the central axis of the rotating shaft 82, and θ is the angle between the connecting line between the central axis of the sliding member 81 and the central axis of the rotating shaft 82 and the vertical direction when the sliding member 81 is in the first part.

[0058] In order to make the end of the capillary needle correspond to the mass spectrometer injection port, further, the first guide rail 21 also includes:

[0059] The third part, the second guide rail 22 and the first part are respectively arranged horizontally, and the third part, the second part and the first part are connected in sequence.

[0060] In order to ensure that the dilution unit 71 moves in a straight line and adapt the capillary needle to be inserted into the dilution unit 71, the detection system for clenbuterol residue further includes:

[0061] A third guide rail 23, wherein the dilution unit 71 is disposed on the third guide rail 23;

[0062] A fourth guide rail 24, wherein the fourth guide rail 24 is disposed on the second carrier 32, the capillary needle is disposed on the fourth guide rail 24, and the third translation device 43 is used for driving the ion source 51 to move forward and backward along the fourth guide rail 24;

[0063] The third carrier 90 includes a fourth part 91, a fifth part 92 and a sixth part 93, the capillary needle is arranged on the fourth part 91, the fifth part 92 is arranged on the fourth guide rail 24, and the third translation device 43 is used to drive the sixth part 93 to move forward and reverse.

[0064] In order to improve the analysis accuracy, further, the capillary needle includes a dipping needle 52 and a sampling needle 53 arranged along a direction parallel to the translation direction of the first translation device 41, and the dilution unit 71 includes a first container and a second container.

[0065] The detection method of clenbuterol residues of the embodiment of the present invention comprises a cleaning stage, a shearing stage, a grinding stage, an automatic sampling stage and a detection stage;

[0066] The cleaning stage is to use a deionized water solution containing a surfactant and / or an organic solvent to clean the animal hair;

[0067] The shearing stage is to use a shearing unit to cut the cleaned animal hair into segments of 0.1 to 3 cm;

[0068] The grinding stage comprises grinding and centrifuging the cut animal hair, and reserving the supernatant for later use;

[0069] like Figure 4 As shown, the automatic injection stage includes the following steps:

[0070] (A1) The first translation device 41 drives the first carrier 31 to translate left and right, the sliding member 81 is in the first part of the first guide rail 21, and the capillary needle is in a vertical state;

[0071] The capillary needle is connected to a rotating shaft 82, and the rotating shaft 82 is rotatably disposed on the first carrier 31 and fixedly connected to the sliding member 81. The central axis of the sliding member 81 and the central axis of the rotating shaft 82 are arranged in parallel and not in a colinear relationship.

[0072] (A2) The second translation device 42 drives the dilution unit 71 to translate forward or backward so that the dilution unit 71 is located at the lower side of the capillary needle;

[0073] (A3) The third translation device 43 drives the capillary needle to move vertically downward, and the capillary needle enters the dilution unit 71 to obtain the detection liquid, such as Figure 6 As shown;

[0074] (A4) The third translation device 43 drives the capillary needle to move vertically upward, and the capillary needle is separated from the dilution unit 71;

[0075] (A5) The first translation device 41 drives the first bearing member 31 to translate, and the sliding member 81 enters the second portion of the inclined first guide rail 21 and descends;

[0076] During the descending process, the capillary needle rotates around the rotating shaft 82;

[0077] (A6) The sliding member 81 moves to the working point of the second part, and the capillary needle is in a horizontal state. Figure 7 shown.

[0078] In order to ensure that the capillary needle can rotate from a vertical state to a horizontal state, further, the sliding member 81, the rotating shaft 82 and the first guide rail 21 meet the following requirements:

[0079] H=L(sinθ+cosθ), H is the height difference between the first part and the working point, L is the distance between the central axis of the sliding member 81 and the central axis of the rotating shaft 82, and θ is the angle between the connecting line between the central axis of the sliding member 81 and the central axis of the rotating shaft 82 and the vertical direction when the sliding member 81 is in the first part.

[0080] In order to make the end of the capillary needle in a horizontal state correspond to the mass spectrometer injection port, further, the automatic injection stage further includes the following steps:

[0081] (A7) The first translation device 41 drives the first carrier 31 to translate, the sliding member 81 enters the third portion of the first guide rail 21 , and the capillary needle translates horizontally until it corresponds to the injection port of the mass spectrometer 61 .

[0082] In order to improve the analysis accuracy, the automatic injection stage further includes the following steps between step (A2) and step (A3):

[0083] The third translation device 43 drives the capillary needle to move vertically downward. The capillary needle includes a sample dipping needle and a sampling needle. The sample dipping needle 52 enters the diluent container in the dilution unit 71, and the solid sample on the sample dipping needle 52 is dissolved in the diluent.

[0084] The third translation device 43 drives the capillary needle to move vertically upward, and the second translation device 42 drives the dilution unit 71 to translate, so that the diluent container is located at the lower side of the sampling needle 53;

[0085] In steps (A3) to (A6), the capillary needle is the sampling needle 53.

[0086] Example 2

[0087] An example of application of the system and method for detecting clenbuterol residues according to Example 1 of the present invention in pig hair detection.

[0088] In this application example, the shear unit adopts the device in patent CN 2021105243692;

[0089] like Figure 2As shown, the first guide rail 21 adopts a guide groove, which is arranged on the bracket 11, and includes a first part, a second part and a third part which are connected in sequence. The first part and the third part are both straight and horizontally arranged, and the position of the first part is higher than the third part, and the second part is inclined downward; the sliding member 81 adopts a bearing, which is suitable for sliding in the guide groove;

[0090] The second guide rail 22 is in a straight line shape and is horizontally arranged on the bracket 11 and is located at the lower side of the third part. The first bearing member 31 is arranged on the second guide rail 22. The first translation device 41 adopts an electric screw and is fixed on the bracket 11 to drive the first bearing member 31 to move forward and backward on the second guide rail 22, that is, to translate left and right.

[0091] The third guide rail 23 is a linear guide rail, fixed on the bracket 11, and the dilution unit 71 is arranged on the third guide rail 23; the second translation device 42 is an electric screw, arranged on the bracket 11, and is used to drive the dilution unit 71 to move forward and backward on the third guide rail 23, that is, to translate forward and backward, and the angle between the moving direction of the dilution unit 71 (the extension direction of the third guide rail 23) and the moving direction of the first carrier 31 is a right angle; the dilution unit 71 includes a first container and a second container arranged front and back;

[0092] like Figure 3 As shown, the rotating shaft 82 is rotatably disposed on the first bearing member 31 and is fixedly connected to the sliding member 81, and the rotating shaft 82 is perpendicular to the first guide rail 21; the central axis of the sliding member 81 and the central axis of the rotating shaft 82 are arranged in parallel and not in a colinear manner, so that when the sliding member 81 slides in the second part, the rotating shaft 82 is driven to rotate; when the first translation device 41 drives the first bearing member 31 to translate, the moving track of the rotating shaft 82 in the horizontal direction is linear, and is located between the first part and the third part in terms of height;

[0093] The second carrier 32 is fixedly connected to the rotating shaft 82, and the fourth guide rail 24 is in a straight line shape and is arranged on the second carrier 32, and the angle between the fourth guide rail 24 and the rotating shaft 82 is a right angle; the third carrier 90 includes a fourth part 91, a fifth part 92 and a sixth part 93, the ion source 51 is arranged on the fourth part 91, and the fifth part 92 is arranged on the fourth guide rail 24. The third translation device 43 adopts an electric screw to drive the sixth part 93 to move forward and reverse, that is, the fifth part 92 translates on the fourth guide rail 24, thereby driving the ion source 51 to translate; the ion source 51 includes a dip sample needle 52 and a sampling needle 53;

[0094] The sliding member 81, the rotating shaft 82 and the first guide rail 21 satisfy: H=L(sinθ+cosθ), H is the height difference between the first part and the working point, L is the distance between the central axis of the sliding member 81 and the central axis of the rotating shaft 82, θ is the angle between the line between the central axis of the sliding member 81 and the central axis of the rotating shaft 82 and the vertical direction when the sliding member 81 is in the first part, such as zero or an acute angle. In this embodiment, the angle is zero; when the sliding member 81 moves from the first part to the working point of the second part, the capillary needle rotates with the rotating shaft 82, and rotates from a vertical state (when the sliding member 81 is in the first part) to a horizontal state (when the sliding member 81 is at the working point).

[0095] The method for detecting the residue of clenbuterol in the embodiment of the present invention comprises:

[0096] The cleaning stage is:

[0097] The pig hair is first washed with a deionized water solution containing a surfactant, wherein the volume percentage of the surfactant is 0.5-5%, and the surfactant comprises at least sodium dodecyl sulfate or sodium dodecylbenzene sulfonate;

[0098] Then, the pig hair washed for the second time is washed with an organic solvent, wherein the organic solvent is one or more of the following organic reagents: acetone, methanol, ethanol, dichloromethane, acetonitrile or ethyl acetate;

[0099] In the shearing stage, the shearing unit is used to automatically shorten the cleaned pig hair into small segments of 0.1 to 3 cm;

[0100] Grinding stage, the grinding stage is:

[0101] Put the cut pig hair into a grinding tube containing 1 to 10 grinding beads; the amount of pig hair used is 15 to 35 mg, the grinding beads used can be made of zirconium oxide or stainless steel, and the grinding tube used can be made of stainless steel or a polymer material of a certain strength;

[0102] Add 0.1-1 mL of grinding liquid, place in a grinder and grind at a frequency of 20-100 Hz for 1-30 minutes. The grinding liquid is a mixture of one or more of the following solutions: water, methanol, ethanol, acetonitrile, acetone, propanol;

[0103] After centrifugation at 5000-15000 rpm for 1-10 minutes, the supernatant was transferred to another centrifuge tube for testing;

[0104] The tip of the sample dipping needle 52 of the ion source is inserted into the extract liquid level of the centrifuge tube by 1 to 10 mm, and stays there for 0.2 to 2 seconds after being inserted into the liquid level;

[0105] Automatic injection stage, such as Figure 4 As shown, the automatic injection stage includes the following steps:

[0106] (A0) The first translation device 41 drives the first carrier 31 to translate, and the sliding member 81 is at one end in the first part of the first guide rail 21. At this time, the fourth part 91 extends out of the bracket 11, and the ion source 51 (specifically, the sample dipping needle 52) dipped in the liquid sample is manually fixed on the fourth part 91. Figure 5 As shown;

[0107] (A1) The first translation device 41 drives the first carrier 31 to translate rightward on the second guide rail 22, the sliding member 81 is in the first part of the first guide rail 21, and the dipping needle 52 and the sampling needle 53 are both in a vertical state until the ion source 51 is on the upper side of the dilution unit 71;

[0108] (A2) The second translation device 42 drives the dilution unit 71 to translate forward or backward, so that the first container is located directly below the sample dipping needle 52;

[0109] (B1) The third translation device 43 drives the ion source 51 to move vertically downward, and the sample dipping needle 52 enters the first container, and the solid sample on the sample dipping needle 52 is dissolved in the diluent;

[0110] The third translation device 43 drives the ion source 51 to move vertically upward, and the second translation device 42 drives the dilution unit 71 to move horizontally, so that the second container is located directly below the sample dipping needle 52;

[0111] The third translation device 43 drives the ion source 51 to move vertically downward, and the sample dipping needle 52 enters the second container. The solid sample on the sample dipping needle 52 that has not yet completely dissolved in the container is dissolved in the diluent, and the sample concentration in the second container is lower than that in the first container;

[0112] The third translation device 43 drives the ion source 51 to move vertically upward, and the second translation device 42 drives the dilution unit 71 to move horizontally, so that the second container is located directly below the sampling needle 53;

[0113] (A3) The third translation device 43 drives the sampling needle 53 to move vertically downward, and the sampling needle 53 enters the second container to obtain the test liquid. Figure 6 As shown;

[0114] (A4) The third translation device 43 drives the sampling needle 53 to move vertically upward, and the sampling needle 53 is separated from the dilution unit 71;

[0115] (A5) The first translation device 41 drives the first bearing member 31 to translate to the right, and the sliding member 81 enters the second portion of the inclined first guide rail 21 and descends;

[0116] During the descending process, the sampling needle 53 (ion source 51) rotates around the rotating shaft 81;

[0117] (A6) The sliding member 81 moves to the working point of the second part, that is, the lowest point of the second part, and the sampling needle 53 is in a horizontal state;

[0118] (A7) The first translation device 41 drives the first carrier 31 to translate to the right, the sliding member 81 enters the third portion of the first guide rail 21, and the sampling needle 53 translates horizontally until it corresponds to the injection port of the mass spectrometer 61. The distance between the needle tip of the sampling needle 53 and the injection port of the mass spectrometer is 2 to 10 mm. Figure 7 As shown;

[0119] In the detection stage, the voltage applied to the electrode of the sampling needle 53 is 1~5 kV, the ion source 51 discharges, the liquid on the sampling needle 53 is atomized, and the ions enter the injection port of the mass spectrometer 61; the parameters set during the operation of the mass spectrometer are: transmission voltage: 85±20 V; voltage before the funnel: 80±20 V; voltage after the funnel: 12±20 V; front focusing lens voltage: 9±10 V; guide bias voltage: 6.6±10 V; rear exit lens voltage: 6.5.±10 V; ion trap bias voltage: 4±10 V; rear end cover voltage: 90±20 V; injection port temperature: 200±50℃;

[0120] The mass spectrometry data model in the mass spectrometer is to establish a standard curve by adding an internal standard or an external standard method, specifically including: adding a clenbuterol standard to blank hair, performing mass spectrometry detection after pre-treatment to obtain standard data, and constructing a mass spectrometry data model after summarizing the standard data. The qualitative analysis is to refer to the mass spectrometry data model, compare the ion information and ion ratio of the target object in the sample to be tested for qualitative analysis, so as to obtain whether there is clenbuterol in the pig hair;

[0121] The mass spectrometer 61 outputs the result. If the result does not meet the requirements, then:

[0122] The first translation device 41 drives the first carrier 31 to translate to the left until the ion source 51 is located on the upper side of the dilution unit 71 , and the sampling needle 53 is vertical at this time;

[0123] The second translation device 42 drives the dilution unit 71 to translate so that the first container is located directly below the sampling needle 53;

[0124] Execute steps (A3)-(A7), and then enter the detection phase.

Claims

1. A detection system for clenbuterol residues, comprising a bracket, an ion source and a mass spectrometer, wherein the ion source comprises a capillary needle and the mass spectrometer is arranged on the bracket; characterized in that: The detection system for clenbuterol residues also includes: A pretreatment device, the pretreatment device comprising a cleaning unit, a shearing unit and a grinding unit, the cleaning unit is used to clean the collected animal hair, the shearing unit is used to cut the cleaned animal hair short, and the grinding unit is used to grind the cut animal hair; A sampling device, the sampling device comprising the support, further comprising: A first guide rail, the first guide rail is arranged on the bracket, the first guide rail comprises a first part and a second part connected, and the second part is inclined downward; a second guide rail and a first bearing member, wherein the second guide rail is arranged on the bracket, and the first bearing member is arranged on the second guide rail; A sliding member and a rotating shaft, wherein the sliding member is disposed on the first guide rail and connected to the rotating shaft, the rotating shaft is rotatably disposed on the first bearing member, and the central axis of the sliding member and the central axis of the rotating shaft are disposed in parallel and are not collinear; A first translation device, the first translation device is fixed to the bracket and is used to drive the first bearing member to move forward and reversely; a second translation device and a dilution unit, wherein the second translation device is disposed on the bracket and is used to drive the dilution unit to move forward and backward, and an angle between a moving direction of the dilution unit and a moving direction of the first carrier is an acute angle or a right angle; a second bearing member and a third translation device, wherein the second bearing member is fixedly connected to the rotating shaft, and the third translation device is arranged on the second bearing member, and is used to drive the ion source to move forward and reversely; when the sliding member moves from the first part to the working point of the second part, the capillary needle rotates along with the rotating shaft, and rotates from a vertical state to a horizontal state; The sliding member, the rotating shaft and the first guide rail meet the following requirements: H=L(sinθ+cosθ), H is the height difference between the first part and the working point, L is the distance between the central axis of the sliding member and the central axis of the rotating shaft, and θ is the angle between the line between the central axis of the sliding member and the central axis of the rotating shaft and the vertical direction when the sliding member is in the first part.

2. The detection system for clenbuterol residue according to claim 1, characterized in that: The first guide rail also includes: The third part, the second guide rail and the first part are respectively arranged horizontally, and the third part, the second part and the first part are connected in sequence.

3. The detection system for clenbuterol residue according to claim 1, characterized in that: The detection system for clenbuterol residues also includes: a third guide rail, the dilution unit being arranged on the third guide rail; a fourth guide rail, wherein the fourth guide rail is arranged on the second carrier, the capillary needle is arranged on the fourth guide rail, and the third translation device is used for driving the capillary needle to move forward and reversely along the fourth guide rail; The third carrier comprises a fourth part, a fifth part and a sixth part, the capillary needle is arranged on the fourth part, the fifth part is arranged on the fourth guide rail, and the third translation device is used for driving the sixth part to move forward and reversely.

4. The detection system for clenbuterol residue according to claim 1, characterized in that: The capillary needle comprises a dipping needle and a sampling needle arranged in parallel with the translation direction of the first translation device, and the dilution unit comprises a first container and a second container.

5. The detection system for clenbuterol residue according to claim 1, characterized in that: The sliding member adopts a bearing, and the first guide rail adopts a guide groove for accommodating the sliding member.

6. A method for detecting clenbuterol residues, comprising a cleaning stage, a shearing stage, a grinding stage, an automatic sampling stage and a detection stage; characterized in that: The cleaning stage is to use a deionized water solution containing a surfactant and / or an organic solvent to clean the animal hair; The shearing stage is to use a shearing unit to cut the cleaned animal hair into segments of 0.1 to 3 cm; The grinding stage comprises grinding and centrifuging the cut animal hair, and reserving the supernatant for later use; The automatic injection stage comprises the following steps: (A1) The first translation device drives the first carrier to translate left and right, the sliding member is in the first part of the first guide rail, and the capillary needle is in a vertical state; The capillary needle is connected to a rotating shaft, the rotating shaft is rotatably disposed on the first bearing member and is fixedly connected to the sliding member, and the central axis of the sliding member and the central axis of the rotating shaft are arranged in parallel and not in a colinear relationship; (A2) the second translation device drives the dilution unit to translate forward or backward so that the dilution unit is located at the lower side of the capillary needle; (A3) The third translation device drives the capillary needle to move vertically downward, and the capillary needle enters the dilution unit to obtain the detection liquid; (A4) the third translation device drives the capillary needle to move vertically upward, and the capillary needle is separated from the dilution unit; (A5) The first translation device drives the first bearing member to translate, and the sliding member enters the second part of the inclined first guide rail and descends; During the descending process, the capillary needle rotates around the rotation axis; (A6) the sliding member moves to the working point of the second part, and the capillary needle is in a horizontal state; The sliding member, the rotating shaft and the first guide rail meet the following requirements: H=L(sinθ+cosθ), H is the height difference between the first part and the working point, L is the distance between the central axis of the sliding member and the central axis of the rotating shaft, and θ is the angle between the line between the central axis of the sliding member and the central axis of the rotating shaft and the vertical direction when the sliding member is in the first part.

7. The method for detecting clenbuterol residue according to claim 6, characterized in that: The automatic injection stage also includes the following steps: (A7) The first translation device drives the first carrier to translate, the sliding member enters the third portion of the first guide rail, and the capillary needle translates horizontally until it corresponds to the injection port of the mass spectrometer.

8. The method for detecting clenbuterol residue according to claim 6, characterized in that: The automatic injection stage also includes the following steps between step (A2) and step (A3): The third translation device drives the capillary needle to move vertically downward, the capillary needle includes a sample dipping needle and a sampling needle, the sample dipping needle enters the diluent container in the dilution unit, and the solid sample on the sample dipping needle is dissolved in the diluent; The third translation device drives the capillary needle to move vertically upward, and the second translation device drives the dilution unit to translate, so that the diluent container is located at the lower side of the sampling needle; In steps (A3) to (A6), the capillary needle is a sampling needle.

Citation Information

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