CN210427486U - QuEChERS one-step pretreatment device - Google Patents
QuEChERS one-step pretreatment device Download PDFInfo
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- CN210427486U CN210427486U CN201920618110.2U CN201920618110U CN210427486U CN 210427486 U CN210427486 U CN 210427486U CN 201920618110 U CN201920618110 U CN 201920618110U CN 210427486 U CN210427486 U CN 210427486U
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Images
Abstract
The utility model discloses a QuEChERS one-step pretreatment device, which comprises an outer sleeve 1 and an inner sleeve 2 inserted into the outer sleeve; the inner wall of the opening end of the outer sleeve 1 is provided with outer pipe threads 1-1; the outer wall of the inner sleeve is provided with inner pipe threads 2-1 matched with the outer pipe threads 1-1, the lower end of the inner sleeve is provided with a pushing piston 3, and the middle part of the inner sleeve is provided with a filter screen 4; the pipe wall between the piston 3 and the filter screen 4 is provided with an inner pipe small hole 2-2; the piston 3 is in sealing fit with the inner wall of the inner sleeve 2. The device can successfully realize effective extraction of the medicine in the blood of the biological sample and purification of the blood matrix, obtain an analysis sample in one step and can directly carry out instrument analysis. The QuEChERS pretreatment device can complete QuEChERS method operation only in the casing, saves consumables and space, is a high-efficiency and environment-friendly pretreatment analysis device, and can be widely applied to sample pretreatment of forensic toxicants and forensic clinical analysis.
Description
Technical Field
The utility model relates to a preceding processing apparatus field of amphetamine class drug analysis, concretely relates to one-step preceding processing apparatus of QuEChERS.
Background
Blood is the most common biological test material in clinic, can accurately and timely reflect the concentration of in vivo drugs and the condition of each drug in a target organ, and contains a large amount of organic matters, wherein organic matters such as protein (hemoglobin, plasma protein, enzyme and protein hormone), non-protein nitrogen-containing compounds (nitrogen-containing substances except protein in blood, mainly urea, uric acid, creatine, creatinine, amino acid, ammonia, peptide and bilirubin), sugar and other organic matters, vitamins, lipids (including steroid hormone) and the like often interfere with the analysis of a target object in instrument analysis.
QuEChERS is essentially a derivative and further development of solid phase extraction technology and matrix solid phase dispersion technology. The basic principle of the method is that after a homogenized sample is extracted by acetonitrile (or acidified acetonitrile), extraction salt is adopted for salting out and layering, a matrix dispersion extraction mechanism is utilized, PSA (ethylenediamine-N-propylsilane) or other adsorbents such as C18 (octadecylsilane) and the like are combined with most of interferents (organic acid, fatty acid, carbohydrate and the like) in the matrix, and the interferents are removed in a centrifugal mode, so that the purification purpose is achieved.
Compared with the traditional pretreatment analysis method, the QuEChERS method has the following advantages: (1) the method has the advantages of good reproducibility, high accuracy and precision. The use of the internal standard method can effectively eliminate the difference between commodities and reduce the analysis error between batches. (2) High efficiency, high speed and high analysis flux. The batch treatment of 10-20 samples only needs 30-40 min to complete the relevant pretreatment process. (3) The solvent consumption is low, the use of chlorine-containing organic solvent is avoided, the pollution is low, and the environment-friendly concept of green chemistry is met. (4) The required space of experiment is little, only accomplishes the process in the polytetrafluoroethylene centrifuging tube and adds the solvent after, seals immediately, has reduced the injury to the staff. (5) The method is simple and convenient to operate and low in analysis cost. Reagents, vessels, devices and the like used by the method belong to basic configuration articles in a laboratory, and are cheap and easy to obtain.
Although the QuEChERS technology which is quite popular at present is continuously applied to the pretreatment of analytical detection in 2003, the literature reports at home and abroad are reviewed, has wider application in other aspects such as pesticide analysis, drug analysis, mycotoxin analysis, polycyclic aromatic hydrocarbon analysis and the like, but has less involvement in the field of toxicant analysis, as for QuEChERS used for drug analysis, there are only a few reports on the QuEChERS method used, Luca et al use Qu ECh ERS to perform liquid quality analysis of benzodiazepines in blood, with the lowest detection limit of 0.5ng/mL and the quantification limit of 0.05-2 ng/mL [ Anzillotti L, Odoardi S, Strano-Rossi S.cleaning up block samples using amplified "QuEChERS" procedure for the determination of drugs of absobenzodiazoledipines by UPLC-MSMS () [ J ] Science International,2014,243:99-106 ]. Matsuta et al, using modified Qu ECh ERS, analyzed 13 toxins such as amphetamine in blood, at an add-on concentration of 0.5ug/mL, the recovery rate reached 59% -93% [ Matsuta S, Nakanishi K, Miki A, equivalent.development of a single one-pot extraction method for variable drugs and materials of sensitive interest in blood by modifying the QuEChERS method [ J ]. Forensic Science International,2013, 232(1-3):40-45 ]. However, the reagents in the QuECh ERS method are improved and optimized, a large number of transfer and liquid-transferring processes are still inevitable in the treatment process, the required consumables are more, and obvious system errors influence the experimental result. For a QuEChERS processing device, a centrifugal tube is used for extraction, purification and separation, and an extraction tube, a syringe type filter membrane filter and a salt adding bag tool in a method bag in the invention of fruits, vegetables, meat, aquatic products, grains, wines, tea and tobacco used in a patent CN 103698195B QuEChERS method bag for efficiently and homogeneously extracting pesticide and veterinary drug residues can only enable an extract liquid of a detected sample to be extruded from a lower layer under air pressure after extraction, so that a tube opening can be blocked, the separation effect of a matrix and the extract liquid is poor, and large errors can be caused by subsequent transfer and liquid transfer.
SUMMERY OF THE UTILITY MODEL
The utility model provides a QuEChERS one-step pretreatment device, which can realize the completion of the extraction, separation, purification and other experimental processes in a sleeve, and avoid the complex liquid taking and transferring processes; meanwhile, the loss generated in sample transfer can be effectively reduced, the system error is reduced, the consumable material is saved, the blood with complex matrix is purified, and the treatment of a single sample can be completed within 10 minutes; or micro solid phase extraction, separation and purification.
The utility model discloses use the big mixed organic reagent of polarity to carry out the extraction of amphetamine class medicine, improve the extraction mode simultaneously for extraction efficiency greatly increased gets rid of macromolecular compounds such as phospholipid, protein in the blood betterly, reduces the influence of interferent to target compound, makes rate of recovery greatly increased, because the complicated matrix obtains obvious purification in the joining of purifying the package makes the blood, and the sample size that consumes is little. The utility model discloses the device has characteristics such as simple, high-efficient, low cost, environment friendly, can use the solid phase extraction to satisfy the multiple preceding processing process that draws the analysis of examining medicine in the material, can arrange this utility model sleeve pipe device and analysis and determination instrument use, realizes high-efficient, quick, automatic drug analysis.
The purpose of the utility model is realized through the following technical scheme.
A QuEChERS one-step pretreatment device comprises an outer sleeve 1 and an inner sleeve 2 inserted into the outer sleeve 1; the inner wall of the opening end of the outer sleeve 1 is provided with outer pipe threads 1-1; the outer wall of the inner sleeve 2 is provided with an inner pipe thread 2-1 matched with the outer pipe thread 1-1, the lower end of the inner sleeve is provided with a pushing piston 3, and the middle part of the inner sleeve is provided with a filter screen 4; the pipe wall between the piston 3 and the filter screen 4 is provided with an inner pipe small hole 2-2; the piston 3 is in sealing fit with the inner wall of the inner sleeve 2.
Preferably, the upper end of the inner sleeve is provided with an organic filter membrane 4-1, and after a sample is subjected to coarse filtration by a filter screen, secondary filtration and purification can be performed by using the organic filter membrane 4-1.
The pore diameter of the inner tube pore can be different according to the sample state and the purifying agent specification selected according to different medicines of the processed sample, and is preferably 20 to 200 um.
Preferably, the outer pipe thread and the inner pipe thread are made of rubber sealing materials. The threads of the inner and outer sleeves are twisted, so that the liquid pressing the outer cavity under the air pressure can enter the inner cavity.
Preferably, the outer sleeve and the inner sleeve have good sealing performance.
Preferably, the volume ratio of the outer sleeve to the inner sleeve is 3: 2-3: 1.
Preferably, the piston is made of rubber with high sealing performance.
Preferably, the aperture of the filter screen is 10 um-100 um, and more preferably 20 um-60 um.
Preferably, the extraction reagent liquid and the extraction reagent bag are placed in the outer sleeve cavity.
Preferably, the extraction reagent solution comprises acetonitrile; the extraction reagent contains grinding beads, anhydrous magnesium sulfate and sodium borate.
Preferably, a purification bag is placed in the inner sleeve, and the sample can be purified in the cavity of the inner sleeve.
Preferably, the extraction reagent bag, the extraction reagent solution and the purification bag are wrapped by photophobic tinfoil.
Preferably, the purge comprises PSA and C18.
Preferably, the piston bottom is larger than the middle.
The device can be applied to the pretreatment of liquid samples, preferably blood; it can also be used for analyzing medicine, pesticide residue, toxin, etc.
The device is used for realizing one-step pretreatment of the QuEChERS suitable for analyzing the drugs in the blood, which is mainly divided into 3 parts, namely the processes of sample loading extraction, separation, purification and filtration, and specifically comprises the following steps:
1) sample loading extraction process
Adding a sample into a cavity of an outer sleeve, opening an extraction reagent solution which is pre-filled with an outer package, adding the extraction reagent solution into the cavity of the outer sleeve, adding grinding beads in the extraction reagent package, manually shaking for 5-10 s, adding anhydrous magnesium sulfate and sodium borate in the extraction reagent package, inserting an inner sleeve into the outer sleeve, wherein an inner pipe thread is arranged on the inner sleeve, a matched outer pipe thread is arranged on the outer sleeve, screwing the inner sleeve to a certain scale, completing the whole sample loading process, keeping a certain distance between the bottom of a piston and liquid at the moment, screwing the inner sleeve to a certain scale, standing for 1min after swirling for 30s at 2500r/min, layering the liquid to obtain a supernatant and a waste liquid, and completing the extraction process;
2) separation process
And after extraction is finished, the inner sleeve is continuously screwed to a certain scale, so that the bottom of the piston is contacted with the bottom of the outer sleeve and stops rotating, at the moment, the supernatant is extruded and rises, the liquid level is higher than the purifying agent, air in the cavity of the outer sleeve is compressed, and the internal pressure is higher than the atmospheric pressure. Because the pipe wall of the inner sleeve pipe which is provided with the purifying agent part is provided with a plurality of small holes, the extracted supernatant liquid is under the action of liquid level pressure difference and atmospheric pressure difference. The supernatant enters a purifying agent layer through the small holes of the inner pipe to complete the separation process, and then enters a next purifying bag for purification;
3) purification and filtration process
The purified supernatant liquid rises in the inner sleeve cavity, after the supernatant liquid completely enters the inner sleeve 2 cavity, the supernatant liquid is vortexed and vibrated for 1min, but the liquid level height at the moment is below the filtering membrane, and the purified liquid cannot penetrate through the filtering membrane with small holes due to the small acting force of the liquid level pressure difference and the atmospheric pressure difference. So the sleeve pipe can overturn, make when freely filtering filter screen 4 because of the action of gravity, continue rotatory interior sleeve pipe, relative make the piston push away the supernatant downstream of purification, cross the inner tube aperture when the piston, just form a confined space, when continuing to twist interior sleeve pipe downwards, the piston pushes away liquid forward, and the pressure in confined space is big more, consequently, continue twisting interior sleeve pipe's in-process, the thrust and the internal pressure of production, make the liquid after the purification can pass through the great filter screen of resistance, liquid after purifying the coarse filtration has accomplished whole extraction process through the liquid of organic filter membrane promptly, obtain the sample after the purification, directly carry out instrument testing.
Compared with the prior art, the utility model has the advantages of as follows and effect:
1. the utility model discloses a device can successfully realize the purification of the extraction of getting one's appearance, extract and matrix separation and sample like blood matrix of medicine in the biological sample blood, and the one-step obtains analysis sample, can directly carry out the instrument analysis.
2. The utility model discloses use QuEChERS one-step device and reagent package can be to complicated sample matrix medicine in like blood, effectively draw like the amphetamine class medicine to purify complicated sample matrix like blood with the material package, carry out the sample detection analysis at last. The single sample can be processed within 10 minutes, so that the complicated liquid taking and liquid transferring processes are reduced, the loss generated in the sample transfer can be effectively reduced, and the system error is reduced.
3. This method is to the easy operation of the toxic medicine analytical method in the blood sample the utility model discloses an alright accomplish QuEChERS method operation in the bushing apparatus, practice thrift the consumptive material, practice thrift the space, be a high-efficient environmental protection's pretreatment analytical equipment, but wide application in forensic poison, the sample pretreatment of forensic clinical analysis.
Drawings
Fig. 1 is an overall schematic diagram of the extraction casing of the queechers method of the present invention.
FIG. 2 is a schematic view of the sample and extract portions of the present invention.
Fig. 3 is a schematic diagram of the sample and extract assembly sleeve portion of the present invention.
Fig. 4 is a schematic diagram of the extraction layering part of the present invention.
Fig. 5 is a schematic diagram of a part of the pressure difference generation device of the present invention.
FIG. 6 is a schematic view of the process of the present invention, wherein the extracting solution enters the inner tube through the inner tube aperture and is purified by the purifying agent.
Fig. 7 is a schematic view of the supernatant fluid of the present invention passing through the filter screen.
Fig. 8 is a schematic view of the supernatant of the present invention entering the organic filtration membrane after being filtered.
Detailed Description
The following description will further describe a specific embodiment of the present invention with reference to the drawings, but the present invention is not limited thereto.
The structure schematic diagram of the QuEChERS one-step pretreatment device of the utility model is shown in fig. 1, and comprises an outer sleeve 1 and an inner sleeve 2 inserted into the outer sleeve 1; the inner wall of the opening end of the outer sleeve 1 is provided with outer pipe threads 1-1; the outer wall of the inner sleeve 2 is provided with an inner pipe thread 2-1 matched with the outer pipe thread 1-1, the lower end of the inner sleeve is provided with a pushing piston 3, and the middle part of the inner sleeve is provided with a filter screen 4; the pipe wall between the piston 3 and the filter screen 4 is provided with an inner pipe small hole 2-2; the piston 3 is in sealing fit with the inner wall of the inner sleeve 2; the upper end of the inner sleeve is provided with an organic filter membrane 4-1.
Example 1
As shown in fig. 2, the QuEChERS method for efficiently and homogeneously extracting amphetamines and other drugs of the present invention comprises: an outer tube containing an extraction reagent solution (acetonitrile mixed reagent) and an extraction reagent pack 6 (salting-out pack such as beads, anhydrous magnesium sulfate, and sodium borate); the inner sleeve is filled with filler such as PSA, C18, etc., and has detailed structure shown in FIG. 2, one end provided with porous outer wall, middle part provided with filter screen, and the other end provided with organic filter membrane.
Example 2
As shown in fig. 2, the QuEChERS method for efficiently and homogeneously extracting amphetamines and other drugs of the present invention comprises: an outer casing containing therein an extraction reagent solution (acetonitrile mixed reagent) and an extraction reagent pack (salting-out pack such as beads, anhydrous magnesium sulfate, and sodium borate); the inner sleeve is filled with filler such as PSA, C18, etc., and has detailed structure as shown in FIG. 2, one end with porous outer wall, middle filter screen, and the other end with organic filter membrane. The outer package of the extraction reagent liquid and the extraction reagent bag 6 is a lightproof and moisture-proof tin foil bag.
The specification of the outer sleeve is 5mL, a reagent solution (1mL acetonitrile mixed reagent) is extracted, and an extraction reagent bag 6 comprises salting-out bags of 4-6 grinding beads, 150mg anhydrous magnesium sulfate, 30mg sodium borate and the like; the inner sleeve is internally provided with 20mg of PSA, 10mg of C18 and other fillers, the inner part of the inner sleeve is 4mL, the outer wall of the inner sleeve is provided with threads and small holes, the lower end of the inner sleeve is provided with a piston, a filter screen is arranged in the inner sleeve, and the other end of the inner sleeve is provided with an organic filter screen.
Example 3
As shown in fig. 1, the QuEChERS method for efficiently and homogeneously extracting amphetamines and other drugs of the present invention comprises: an outer casing containing therein an extraction reagent solution (acetonitrile mixed reagent) and an extraction reagent pack (salting-out pack such as beads, anhydrous magnesium sulfate, and sodium borate); the inner sleeve is filled with filler such as PSA, C18, etc., and has detailed structure shown in FIG. 2, one end with porous outer wall, middle part with filter membrane, and the other end with organic filter membrane. The specification of the outer sleeve 1 is 15mL, a reagent solution (1mL acetonitrile mixed reagent) is extracted, and an extraction reagent bag 6 comprises salting-out bags of 4-6 grinding beads, 150mg anhydrous magnesium sulfate, 30mg sodium borate and the like; the inner sleeve is internally provided with fillers such as 20mg PSA, 10mg C18 and the like, the inner part of the sleeve is 10mL, the outer wall of the inner sleeve is provided with threads and small holes, the lower end of the inner sleeve is provided with a piston, a filter screen is arranged in the inner sleeve, and the other end of the inner sleeve is provided with an organic filter screen.
Example 4
As shown in fig. 1, the QuEChERS method for efficiently and homogeneously extracting amphetamines and other drugs of the present invention comprises: an outer casing containing an extraction reagent solution (acetonitrile mixed reagent) and an extraction reagent pack (salting-out pack such as beads, anhydrous magnesium sulfate, and sodium borate); the inner sleeve is filled with filler such as PSA, C18, etc., and has detailed structure shown in FIG. 2, one end with porous outer wall, middle part with filter membrane, and the other end with organic filter membrane. The specification of the outer sleeve is 50mL, the reagent solution (1mL acetonitrile mixed reagent) is extracted, and the extraction reagent bag 6 comprises salting-out bags of 4-6 grinding beads, 150mg anhydrous magnesium sulfate, 30mg sodium borate and the like; the inner sleeve comprises fillers such as 20mgPSA and 10mg C18, the inner part of the inner sleeve is 40mL, the outer wall of the inner sleeve is provided with threads and small holes, the lower end of the inner sleeve is provided with a piston, a filter screen is arranged in the inner sleeve, and the other end of the inner sleeve contains an organic filter screen.
Example 5
As shown in fig. 1, a QuEChERS method for extracting amphetamines and other drugs with high efficiency and homogeneous phase according to the present invention comprises the following steps:
1) sample loading extraction process
As shown in figure 1, unscrewing the QuECHERS extraction sleeve, adding a certain amount of sample into the cavity of the outer sleeve 1, opening the extraction reagent solution which is pre-filled with the outer package, adding the extraction reagent solution into the cavity of the outer sleeve 1, adding the grinding beads in the extraction reagent package, manually shaking for 5-10 s, and adding other reagents such as anhydrous magnesium sulfate, sodium borate and the like in the extraction reagent package, as shown in figure 2. The inner sleeve 2 is inserted into the outer sleeve 1, the inner sleeve is provided with inner sleeve threads 2-1, the outer sleeve is provided with outer sleeve threads 1-1 which are matched tightly, and the inner sleeve is screwed to a certain scale, as shown in figure 3. The whole sample loading process is completed, the bottom of the piston 3 and liquid at the moment are kept at a certain distance, the bottom of the piston is large, and the liquid is prevented from splashing into the purification bag 5 in vortex oscillation. And (4) screwing the inner sleeve to a certain scale, then, swirling for 30s at 2500r/min, and standing for 1 min. The liquid layers are shown in figure 4, supernatant and waste liquid, and the extraction process is completed.
2) Separation process
After extraction, the inner sleeve 2 is screwed to a certain scale, so that the bottom of the piston 3 contacts the bottom of the outer sleeve 1, and the rotation is stopped, as shown in fig. 5. At the moment, the supernatant is extruded and rises, the liquid level is higher than the purification bag, and the air in the cavity of the outer sleeve 1 is compressed, and the internal pressure is higher than the atmospheric pressure. Because the pipe wall of the inner sleeve 2 at the position where the purifying bag is arranged is provided with a plurality of small holes 5-1. Therefore, the extracted supernatant liquid is under the action of the liquid level pressure difference and the atmospheric pressure difference. The supernatant enters a purifying agent layer through the inner pipe small hole 2-2 to complete the separation process, and then enters a next purifying bag for purification.
3) Purification and filtration process
The purified supernatant liquid rises in the cavity of the inner sleeve 2 as shown in fig. 6 and 7. After the supernatant liquid completely enters the cavity of the inner sleeve 2, vortex and shake for 1min, but the liquid level at the moment is below the filter screen 4. Because the acting force of the liquid level pressure difference and the atmospheric pressure difference is too small, the purified liquid can not penetrate through the filter screen 4 with small holes. The sleeve can be inverted so that it continues to rotate the inner sleeve 2 while freely passing through the screen 4 due to gravity, and the opposite causes the piston 3 to push the purified supernatant liquid downward. When the piston 3 passes through the small hole 2-2 of the inner tube, a closed space is formed. When the inner sleeve 2 is screwed downwards continuously, the piston 3 pushes the liquid forwards, and the pressure of the closed space is higher, so that in the process of screwing the inner sleeve 2 continuously, the thrust and the internal pressure are generated, so that the purified liquid can sequentially pass through the filter screen 4 and the organic filter membrane 4-1 (see fig. 8) with relatively high resistance, and when the purified liquid passes through the liquid of the filter membrane 4-1, the whole extraction process is finished, a purified sample is obtained, and instrument detection is directly carried out.
Wherein the sample is whole blood, plasma, serum, also can use this device to carry out the analysis of medicine in the biological samples such as urine, saliva, also can use the utility model discloses a pretreatment analysis is carried out to the device.
Wherein the medicine is abuse medicine such as listed amphetamine class medicine, also can use this device to carry out other kinds of pharmaceutical analysis of complicated matrix sample, other analysis detection such as pesticide and veterinary drug residue, mycotoxin also can use the utility model discloses a pretreatment analysis is carried out to the device.
The above-mentioned embodiments are only intended to describe the preferred embodiments of the present invention, but not to limit the scope of the present invention, and all modifications and improvements of the technical method of the present invention, including the used casing specification, reagent pack, reagent contained in the pack, should fall within the scope of the present invention defined by the claims.
Claims (10)
1. The QuEChERS one-step pretreatment device is characterized by comprising an outer sleeve (1) and an inner sleeve (2) inserted into the outer sleeve (1); the inner wall of the opening end of the outer sleeve (1) is provided with outer pipe threads (1-1); the outer wall of the inner sleeve (2) is provided with inner pipe threads (2-1) matched with the outer pipe threads (1-1), the lower end of the inner sleeve is provided with a pushing piston (3), and the middle part of the inner sleeve is provided with a filter screen (4); an inner pipe small hole (2-2) is formed in the pipe wall between the piston (3) and the filter screen (4); the piston (3) is in sealing fit with the inner wall of the inner sleeve (2).
2. The QuEChERS one-step pretreatment device according to claim 1, wherein the upper end of said inner casing is provided with an organic filter (4-1).
3. The QuEChERS one-step pretreatment device according to claim 1, wherein said outer and inner tube threads are rubber-tight.
4. The QuEChERS one-step pretreatment device according to claim 1, wherein the volume of the inner casing is smaller than the volume of the outer casing.
5. The QuEChERS one-step pretreatment device of claim 1, wherein the piston is made of rubber with high sealing property.
6. The QuEChERS one-step pretreatment device according to claim 1, wherein the aperture of said filter screen is 10 um-100 um.
7. The QuEChERS one-step pretreatment device according to claim 1, wherein an extraction reagent solution and an extraction reagent pack are placed in the outer sleeve cavity; a purification bag is placed in the inner sleeve.
8. The QuEChERS one-step pretreatment apparatus according to claim 7, wherein said extraction reagent comprises acetonitrile; the extraction reagent contains grinding beads, anhydrous magnesium sulfate and sodium borate.
9. The QuEChERS one-step pretreatment device according to claim 7, wherein said purification comprises PSA and C18.
10. The QuEChERS one-step pretreatment device of claim 1, wherein the piston bottom is larger than the middle.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110031578A (en) * | 2019-04-30 | 2019-07-19 | 华南理工大学 | A kind of QuEChERS single step pretreating device |
CN113295801A (en) * | 2021-06-04 | 2021-08-24 | 国家烟草质量监督检验中心 | Method for determining fluorosulfonyl in plant-derived food |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110031578A (en) * | 2019-04-30 | 2019-07-19 | 华南理工大学 | A kind of QuEChERS single step pretreating device |
CN113295801A (en) * | 2021-06-04 | 2021-08-24 | 国家烟草质量监督检验中心 | Method for determining fluorosulfonyl in plant-derived food |
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