CN216117016U - QuEChERS dehydrating agent bag for efficiently and homogeneously extracting pesticide and veterinary drug residues - Google Patents
QuEChERS dehydrating agent bag for efficiently and homogeneously extracting pesticide and veterinary drug residues Download PDFInfo
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- CN216117016U CN216117016U CN202122491504.6U CN202122491504U CN216117016U CN 216117016 U CN216117016 U CN 216117016U CN 202122491504 U CN202122491504 U CN 202122491504U CN 216117016 U CN216117016 U CN 216117016U
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Abstract
A QuEChERS dehydrating agent bag for efficiently and homogeneously extracting pesticide and veterinary drug residues consists of an outer tube, a tube cover, an inner tube, a diaphragm, a dehydrating agent and a uniform proton. One end of the inner tube is fixed on the tube cover, the other end of the inner tube is provided with the diaphragm, the dehydrating agent of the inner tube is arranged in the inner tube, the outer tube is positioned outside the inner tube, and the uniform protons are arranged in the outer tube. The diaphragm can be broken or dissolved, and the dehydrating agent is rapidly mixed with the sample and the reagent. The utility model has wide application field, and is suitable for laboratories needing to analyze pesticide residues and veterinary drug residues by using the QuEChERS method, including laboratories in industries of vegetables, fruits, grains, aquatic products, poultry, meat, tea, tobacco, wines and the like.
Description
Technical Field
The utility model relates to a sample pretreatment device in the analytical instrument industry, in particular to a QuEChERS dehydrating agent bag for efficiently and homogeneously extracting pesticide and veterinary drug residues.
Background
The food safety problem is a big matter related to the livelihood, and the safety problem on the tongue tip is increasingly serious, so the detection and the confirmation of chemical harmful substances such as pesticide residues, veterinary drug residues, mycotoxin and the like in food are imperative. At present, the sample pretreatment means for detecting chemical harmful substances such as pesticide residue, veterinary drug residue, mycotoxin and the like in food mainly comprises a solid phase extraction column and a centrifugal tube type QUECHERS.
The term QuEChERS is derived from the abbreviations of Quick, Easy, Cheap, Effective, Rugged and Safe, and is a sample pretreatment method which is rapid, simple, Cheap, Effective, stable and Safe. The QuEChERS technology is mainly used for detecting pesticide residues, veterinary drug residues and mycotoxins, and in the technology, a sample to be detected is beaten into homogenate firstly, acetonitrile is added, dehydrating agents such as magnesium sulfate and sodium chloride are added for dehydration and purification, and finally a purifying material is added for removing interferents and carrying out analysis and detection. The excellent impurity interference elimination capability of the QuEChERS method is combined with the high-sensitivity detection of mass spectrum, so that the QuEChERS method becomes a standard method for multiple governments and organizations all over the world.
Yet another QuEChERS method is based on EMR purification of packing by accurately weighing 5g (to 0.01 g) of the sample into a 50mL centrifuge tube with a lid, adding 10.0 ml of 5% acetonitrile formic acid extract, adding dehydrating agents such as magnesium sulfate, sodium chloride and the like, homogenizing two ceramics, mixing uniformly for 5 minutes by vortex (2000 rpm), centrifuging for 5 minutes (4000rpm), transferring 5.0 ml of ammonium acetate aqueous solution (5 mM) into a 15 ml EMR-Lipid dSPE tube, shake quickly and vortex for 2 minutes (2000 rpm), remove 5.0 ml of centrifuged supernatant into an activated EMR-Lipid dSPE tube, shaken quickly and vortexed for 2 minutes (2000 rpm), centrifuged for 5min (4000rpm), the supernatant poured completely into a 50.0mL centrifuge tube, two ceramic homo protons and EMR polish powder packs (dehydrating agent) were added, shaken rapidly and vigorously and vortexed for 2 minutes (2000 rpm). Centrifuge for 5min (4000rpm), and remove the upper acetonitrile liquid for analysis.
In the above-mentioned process of adding the dehydrating agent, rapid addition, rapid capping and rapid shaking are required, otherwise, the dehydrating agent may be agglomerated, the separation of the organic reagent from the sample is poor, and the target compound is lost due to local overheating, thereby causing an error in analysis data.
With the development of the technology, some companies provide an automatic QuEChERS pretreatment platform, such as an AutoMate-Q40 full-automatic QuEChERS pesticide residue sample pretreatment platform of Teledyne Tekmar, and an additional independent module is adopted for adding the dehydrating agent, so that the structure is complex, and the steps are complicated.
Disclosure of Invention
The utility model aims to provide a QuEChERS dehydrating agent method bag for efficiently and homogeneously extracting pesticide and veterinary drug residues, which has the advantages of simple structure, low cost, simple and convenient operation and good extraction effect.
A QuEChERS dehydrating agent bag for efficiently and homogeneously extracting pesticide and veterinary drug residues consists of an outer tube, a tube cover, an inner tube, a diaphragm, a dehydrating agent and a uniform proton. One end of the inner tube is fixed on the tube cover, the other end of the inner tube is provided with the diaphragm, the dehydrating agent of the inner tube is arranged in the inner tube, the outer tube is positioned outside the inner tube, and the uniform protons are arranged in the outer tube.
The diaphragm can be broken or dissolved, and the dehydrating agent is rapidly mixed with the sample and the reagent.
Furthermore, the diaphragm is made of glass, is fixed on the inner tube in a buckling and thread mode or is adhered to the inner tube, and is smashed by the uniform protons through shaking when in use.
Furthermore, the inner tube and the diaphragm are both made of glass and are fixed on the tube cover in a buckling and thread mode or are adhered on the tube cover, and when the glass tube and the diaphragm are used, the glass inner tube and the diaphragm are smashed by the uniform protons through shaking.
Furthermore, the diaphragm is made of water-soluble paper, is fixed on the inner tube in a buckling and thread mode or is adhered to the inner tube, and is dissolved by water in a sample through shaking when the diaphragm is used.
Further, the inner tube and the diaphragm are made of water-soluble paper and are fixed on the tube cover in a buckling or thread mode or are adhered on the tube cover, and when the device is used, the diaphragm and the inner tube are dissolved by water in a sample through shaking.
Furthermore, the diaphragms are arranged at two ends of the inner pipe, and the dehydrating agent is filled in the inner pipe.
Furthermore, the shape of the inner tube is cylindrical or spherical, oval sphere, semi-sphere, cuboid, square, cone, trapezoidal cylinder, prism and polyhedral; the inner tube is made of glass or ceramic.
Further, the inner tube is fixed on the tube cover, or the inner tube is independently placed and is added into the outer tube when in use.
After the diaphragm is dissolved or broken, the dehydrating agent in the inner tube is quickly mixed with the sample and the extraction solvent, the mixture is continuously shaken and dehydrated, and an acetonitrile layer is taken to continue the next operation.
The dehydrating agent comprises one or more of magnesium sulfate, sodium chloride, sodium acetate, sodium citrate and the like.
The QuEChERS dehydrating agent bag for efficiently and homogeneously extracting the pesticide and veterinary drug residues is characterized in that a sample is fruit and vegetable, meat, aquatic product, grain, wine, tea or tobacco.
The utility model provides a contain foretell high-efficient homogeneous phase and draw full-automatic QuEChERS sample pretreatment platform of pesticide animal remedy residue QuEChERS dehydrating agent package, includes outer pipe support, bottle lid frame, robotic arm, by robotic arm will bottle lid on the bottle lid frame move on the outer tube to screw, in continuing on next step shaking up and down the operation, smash or dissolve the diaphragm, accomplish the acetonitrile dehydration.
The using method comprises the following steps:
the diaphragm is made of glass, is fixed on the inner tube, and when in use:
the method comprises the following steps: adding a sample and a reagent into an outer tube, homogenizing and uniformly mixing, adding a homogenizing proton,
step two: covering a pipe cover with an inner pipe, screwing,
step three: breaking the glass diaphragm by using a homogenizer through violent shaking by relaxing parallel to the outer tube,
step four: continuously shaking, rapidly and fully mixing the sample, the reagent and the dehydrating agent, centrifuging,
step five: taking the supernatant and continuing the next detection.
Further, the diaphragm is made of glass and fixed on the inner tube, and when the diaphragm is used, the diaphragm comprises the following steps:
the method comprises the following steps: adding sample and reagent into the outer tube, adding homogeneous proton, covering the tube cover with inner tube, screwing,
step two: the mixture is evenly mixed by vortex,
step three: breaking the glass diaphragm by using a homogenizer through violent shaking by relaxing parallel to the outer tube,
step four: continuously shaking, rapidly and fully mixing the sample, the reagent and the dehydrating agent, centrifuging,
step five: taking the supernatant and continuing the next detection.
Further, the diaphragm is made of water-soluble paper and is fixed on the inner tube, and when the diaphragm is used:
the method comprises the following steps: adding a sample and a reagent into an outer tube, homogenizing and uniformly mixing, adding a homogenizing proton,
step two: covering a pipe cover with an inner pipe, screwing,
step three: the diaphragm is cracked and dissolved under the combined action of water and homogeneous protons in the sample by violent shaking parallel to the outer tube,
step four: continuously shaking, rapidly and fully mixing the sample, the reagent and the dehydrating agent, centrifuging,
step five: taking the supernatant and continuing the next detection.
Further, the diaphragm is made of water-soluble paper and is fixed on the inner tube, and when the diaphragm is used:
the method comprises the following steps: adding a sample and a reagent into the outer tube, homogenizing and uniformly mixing,
step two: covering a pipe cover with an inner pipe, screwing,
step three: the diaphragm is dissolved under the combined action of water and solvent in the sample by shaking violently parallel to the outer tube,
step four: continuously shaking, rapidly and fully mixing the sample, the reagent and the dehydrating agent, centrifuging,
step five: taking the supernatant and continuing the next detection.
Further, a use method for efficiently extracting QuEChERS dehydrating agent packets of veterinary drug residues in a homogeneous phase comprises the following steps:
the method comprises the following steps: accurately weighing 5g (accurately to 0.01 g) of sample, adding 10.0 ml of 5% acetonitrile formic acid extract into a method package tube, adding two ceramic homogeneous protons, and covering a tube cover with an inner tube;
step two: vortex (2000 rpm) and mix for 5 minutes;
step three: violently shaking in the direction parallel to the outer pipe body, crushing the glass diaphragm by using a homogenizer, continuously shaking for 1 minute, quickly and fully mixing the sample, the reagent and the dehydrating agent, and centrifuging for 5min (4000 rpm);
step four: transferring 5.0 ml of ammonium acetate aqueous solution (5 mM) into a 15 ml EMR-Lipid dSPE tube, quickly shaking and vortexing for 2 minutes (2000 rpm), transferring 5.0 ml of centrifuged upper layer extract into an activated EMR-Lipid dSPE tube, quickly shaking and vortexing for 2 minutes (2000 rpm), centrifugating for 5 minutes (4000rpm), completely pouring the supernatant in the third step into a tube body of the method bag, adding two ceramic protons, covering a tube cover with an inner tube, quickly and violently shaking, breaking a glass diaphragm, and vortexing for 2 minutes (2000 rpm);
step five: centrifuge for 5min (4000rpm), and remove the upper acetonitrile liquid for analysis.
The QuEChERS dehydrating agent bag for efficiently and homogeneously extracting the pesticide and veterinary drug residue is different from the prior art in that: the QuEChERS dehydrating agent bag for efficiently and homogeneously extracting the pesticide and veterinary drug residues is based on the basic principle of QuEChERS, the dehydrating agent is arranged in the inner pipe, the device, the materials and the operation steps are reasonable, and the defects in the prior art are overcome.
In the existing method, when the dehydrating agent bag is opened and the dehydrating agent is added, 5 seconds are needed from the time when the dehydrating agent bag is completely added and the centrifugal tube cover is covered to the time when the dehydrating agent bag is shaken, and the dehydrating agent is caked within the 5 seconds. The reagent is spilled when poured manually, and reagent particles splash to damage the health of detection personnel; the dehydrating agent is added manually, so that the quantity is inaccurate, and the result repeatability is poor; local temperature increases may lose part of the thermally labile compound.
The QuEChERS dehydrating agent bag for efficiently and homogeneously extracting the pesticide and veterinary drug residues has the following advantages:
(1) the dehydrating agent is arranged in the inner tube, the inner tube is fixed on the bottle cap, and the dehydrating agent is not required to be added manually during the experiment, so that the time and the labor are saved.
(2) The reagent is prevented from splashing when being poured manually, and the reagent particles are prevented from splashing to damage the body health of detection personnel. (note: the dehydrating reagent contains many fine particles, and when splashed, it easily floats in the air, and the examiner easily inhales).
(3) The dehydrating agent is quantitatively placed in the inner tube, so that the problem of inaccurate quantity caused by manual addition of the dehydrating agent, and poor result repeatability is avoided.
(4) After the inner tube is covered on the outer tube along with the bottle cap, the diaphragm is rapidly removed, and the dehydrating agent is rapidly shaken after being mixed with a sample, so that the coagulation time of the dehydrating agent is reduced, and the coagulation of the dehydrating agent is effectively prevented. Because the target compound may be wrapped after the water removal agent is coagulated, the result accuracy is affected.
(5) Fast mixing and fast shaking are beneficial to protecting the heat-labile compound. The dehydrating agents, when combined with water, release a significant amount of heat and if not immediately shaken, locally increase in temperature and lose some of the heat labile compounds.
(6) The broken glass pieces can play a role in homogenizing the broken samples and the blocks when being shaken, so that the extraction efficiency is improved, and the accuracy of the result is ensured. The fragments can be positioned at the lower layer together with the sample dehydrating agent after centrifugation, and the extraction of the acetonitrile at the upper layer can not be influenced. The water-soluble paper can not enter the organic reagent layer after being dissolved and crushed, and can not interfere the detection result.
(7) The utility model is more suitable for automatic equipment.
The method provided by the utility model has wide application field, and is suitable for laboratories which need to use the QuEChERS method for analyzing pesticide residues and veterinary drug residues, including laboratories in the industries of vegetables, fruits, grains, aquatic products, poultry meat, tea, tobacco, wines and the like.
Drawings
The QuEChERS method for efficiently and homogeneously extracting pesticide and veterinary drug residues is further described below by combining the attached drawings.
FIG. 1 is a schematic diagram of a QuEChERS dehydrating agent bag for efficient homogeneous extraction of pesticide and veterinary drug residues.
FIG. 2 is a schematic diagram of a package of QuEChERS dehydrating agents for efficient homogeneous extraction of pesticide and veterinary drug residues.
In the figure: the device comprises an outer tube 1, a tube cover 2, an inner tube 3, a diaphragm 4, a dehydrating agent 5 and a homogenizer 6.
Detailed Description
The utility model is further illustrated with reference to specific embodiments below.
A QuEChERS dehydrating agent bag for efficiently and homogeneously extracting pesticide and veterinary drug residues comprises: the device comprises an outer tube 1, a tube cover 2, an inner tube 3, a diaphragm 4, a dehydrating agent 5 and a homogenizer 6.
One end of the inner tube 3 is fixed on the tube cover 2, the other end is provided with a diaphragm 4, a dehydrating agent 5 is arranged in the inner tube, and the outer tube 1 is positioned outside the inner tube 3 and contains a uniform proton 6. The inner tube 1 and the tube cover 2 are respectively provided with threads 1.1 and 2.1 for combining the inner tube 1 and the tube cover 2, and a wedge-shaped sealing ring 3.1 is arranged at the joint of the inner tube 3 and the tube cover 2, so that the inner tube 1 and the tube cover 2 are convenient to combine and seal when screwed, and reagent leakage is prevented. In the experimental process, a sample and a reagent are added into the outer tube, the tube cover is covered, the diaphragm 4 is removed, the removal mode can be that the diaphragm is broken by the homogenizer 6 or dissolved, and the dehydrating agent 6 is rapidly mixed with the sample and the reagent.
Example 1.
The diaphragm is made of glass, is fixed on the inner tube or is stuck on the inner tube through a buckle and a thread mode, when the glass diaphragm is used, a sample and a reagent are added into the outer tube, the glass diaphragm is smashed by the homogenizer, the vibration is continued, the sample, the reagent and the dehydrating agent are rapidly and fully mixed, the centrifugation is carried out, and the supernatant is taken to continue the next detection.
Example 2.
The inner tube and the diaphragm are made of glass and can be made into a whole, the inner tube and the diaphragm are fixed on the tube cap or adhered to the tube cap in a buckling and thread mode, when the device is used, a sample and a reagent are added into the outer tube, the inner tube and the diaphragm are uniformly homogenized, the tube cap with the inner tube is covered and screwed, the inner tube and the diaphragm are violently shaken by being parallel to the outer tube, the glass inner tube and the diaphragm are broken by using a homogenizer, the shaking is continued, the sample, the reagent and the dehydrating agent are rapidly and sufficiently mixed, the centrifugation is carried out, and the supernatant is taken to continue the next detection.
Example 3.
The diaphragm is made of water-soluble paper, is fixed on the inner tube or is stuck on the inner tube through a buckle and a thread mode, when the diaphragm is used, a sample and a reagent are added into the outer tube, the sample and the reagent are homogenized and mixed, a tube cover with the inner tube is covered, the tube cover is screwed, the sample is cracked and dissolved under the combined action of water and protons in the sample through shaking, the shaking is continued, the sample, the reagent and the dehydrating agent are rapidly and fully mixed, the diaphragm is centrifuged, and the supernatant is taken to continue the next detection.
Example 4.
The inner tube and the diaphragm are made of water-soluble paper and are fixed on the tube cap or adhered on the tube cap in a buckling and thread mode, when the device is used, a sample and a reagent are added into the outer tube, the sample and the reagent are homogenized and mixed, the tube cap with the inner tube is covered, the tube cap is screwed, the sample is cracked and dissolved under the combined action of water and protons in the sample through shaking, the shaking is continued, the sample, the reagent and the dehydrating agent are rapidly and sufficiently mixed, the sample, the reagent and the dehydrating agent are centrifuged, and the supernatant is taken to continue to be detected on the next step.
Example 5
The full-automatic QuEChERS sample pretreatment platform comprises an outer pipe frame, a bottle cap frame and a mechanical arm. The sample and reagents are added to the outer tube, or the purified sample solution from the EMR-Lipid dSPE tube is added to the outer tube. And the mechanical arm moves the bottle cap on the bottle cap frame onto the outer tube, screws the bottle cap, continues to operate in the next step, and breaks or dissolves the diaphragm in the up-down shaking operation process to complete the separation of acetonitrile and water.
Example 6
Accurately weighing 5g (accurate to 0.01 g) of a sample, adding 10.0 ml of 5% acetonitrile formate extract into an outer tube of the method package, adding two ceramic protons, covering a tube cover with an inner tube, vortexing (2000 rpm) for 5 minutes, violently shaking in a direction parallel to the tube body of the outer tube, crushing a glass diaphragm by using a homogenizer, continuously shaking for 1 minute, rapidly and fully mixing the sample, a reagent and a dehydrating agent, centrifuging for 5 minutes (4000rpm), transferring 5.0 ml of ammonium acetate aqueous solution (5 mM) into a 15 ml EMR-Lipid dSPE tube, rapidly shaking and vortexing for 2 minutes (2000 rpm), transferring 5.0 ml of centrifuged upper layer extract into an activated EMR-Lipid dSPE tube, rapidly shaking and vortexing for 2 minutes (2000 rpm), centrifuging for 5 minutes (4000rpm), completely pouring the upper layer extract into the tube body of the method package, adding two ceramic protons, covering the tube cover with the inner tube, shake rapidly and vigorously, break the glass membrane, and vortex for 2 minutes (2000 rpm). Centrifuge for 5min (4000rpm), and remove the upper acetonitrile liquid for analysis.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (6)
1. A QuEChERS dehydrating agent bag for efficiently and homogeneously extracting pesticide and veterinary drug residues is characterized in that: the dehydrating agent-containing water quality testing device is composed of an outer tube, a tube cover, an inner tube, a diaphragm, a dehydrating agent and a homogenizing unit, wherein one end of the inner tube is fixed on the tube cover, the diaphragm is arranged at the other end of the inner tube, the dehydrating agent is arranged in the inner tube, the outer tube is positioned outside the inner tube, and uniform protons are contained in the outer tube.
2. The QuEChERS dehydrating agent bag for efficient homogeneous extraction of veterinary drug residues according to claim 1, which is characterized in that: the diaphragm is made of glass and is fixed on the inner tube in a buckling or thread mode or is stuck on the inner tube, and when the diaphragm is used, the glass diaphragm is smashed by the uniform protons through shaking.
3. The QuEChERS dehydrating agent bag for high efficiency homogeneous extraction of pesticide and veterinary drug residues as claimed in claim 2, wherein the inner tube and the membrane are made of glass and are fixed on the tube cap by means of a snap or a thread or are adhered on the tube cap, and when in use, the inner tube and the membrane are broken by shaking with the homogeneous protons.
4. The QuEChERS dehydrating agent bag for high efficiency homogeneous extraction of pesticide and veterinary drug residues as claimed in claim 1, wherein the membrane is made of water soluble paper, and is fixed on the inner tube by means of snap or screw, or is adhered on the inner tube, and when in use, the membrane is dissolved by water in a sample by shaking.
5. The QuEChERS dehydrating agent bag for high efficiency homogeneous extraction of pesticide residue according to claim 4, wherein the inner tube and the membrane are made of water soluble paper and are fixed on the tube cap by means of snap or screw, or are adhered on the tube cap, and when in use, the membrane and the inner tube are dissolved by water in a sample by shaking.
6. The QuEChERS dehydrating agent bag for efficient homogeneous extraction of veterinary drug residues according to claim 1, which is characterized in that: the diaphragms are arranged at two ends of the inner pipe, and the dehydrating agent is hermetically filled in the inner pipe; the shape of the inner tube is cylindrical or spherical, oval sphere, semi-spherical, cuboid, square, conical, trapezoidal cylinder and prism; the inner tube is made of glass or ceramic.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202122491504.6U CN216117016U (en) | 2021-10-16 | 2021-10-16 | QuEChERS dehydrating agent bag for efficiently and homogeneously extracting pesticide and veterinary drug residues |
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| CN202122491504.6U CN216117016U (en) | 2021-10-16 | 2021-10-16 | QuEChERS dehydrating agent bag for efficiently and homogeneously extracting pesticide and veterinary drug residues |
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| CN216117016U true CN216117016U (en) | 2022-03-22 |
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| CN202122491504.6U Active CN216117016U (en) | 2021-10-16 | 2021-10-16 | QuEChERS dehydrating agent bag for efficiently and homogeneously extracting pesticide and veterinary drug residues |
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