CN114870924B - Combined centrifuge tube for QuEChERS extraction method - Google Patents
Combined centrifuge tube for QuEChERS extraction method Download PDFInfo
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- CN114870924B CN114870924B CN202210472981.4A CN202210472981A CN114870924B CN 114870924 B CN114870924 B CN 114870924B CN 202210472981 A CN202210472981 A CN 202210472981A CN 114870924 B CN114870924 B CN 114870924B
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- tube body
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
- B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
- B01L3/5021—Test tubes specially adapted for centrifugation purposes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/02—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor with moving adsorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
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Abstract
The invention discloses a combined centrifuge tube for QuEChERS extraction, which comprises an upper tube body, a lower tube body, an inner tube body and a puncture rod, wherein the upper tube body can move up and down relative to the lower tube body and stop fixing at any time; after the elastic resetting mechanism is compressed, the liquid inlet hole is exposed outside the sleeve and is in an open state. The invention has convenient use and can improve the operation convenience and the operation efficiency.
Description
Technical Field
The invention relates to a purifying tube, in particular to a combined centrifuge tube for a QuEChERS extraction method.
Background
The detection of pesticide residues in food has long been a difficult challenge, and the detection results are often affected by the inability of the traditional extraction methods to separate the impurities due to the high interference of impurities and low residual content. Since the food contains various impurities and pesticides with various physicochemical properties, and new pesticides are increasingly emerging, the pretreatment of the samples has higher requirements. The QuEChERS (Quick, easy, cheap, effective, rugged and safe) extraction method is a pesticide residue detection sample pretreatment technology which has strong universality and integrates the extraction and purification of pesticide residues in various matrixes.
The basic pretreatment steps of conventional QuEChERS extraction can be summarized as follows: (1) weighing 10g of crushed sample into a 40mL plastic centrifuge tube; (2) After adding 10mL of acetonitrile, the sample is swirled/oscillated for 1min at a maximum rotation speed (greater than 2500 r.min < -1 >; (3) Adding water scavenger (4 g water MgSO) 4 And 1g NaCl), vortexing/shaking for 1min, and then centrifuging for 1min; (4) Remove 1mL of the supernatant (extract) to a solution containing adsorbent (25 mg PSA and 150mg anhydrous MgSO 4 ) Is placed in a small centrifuge tube; (5) Shaking by hand or mixing with a vortex/shaker for 30s, performing dispersed solid phase extraction, and centrifuging for 1min; (6) 5% acetic acid (if necessary) was added and the mixture was subjected to detection by an instrument.
In the existing QuEChERS extraction method, a water removing agent and an adsorbent are required to be manually poured in the operation process, the addition is troublesome, the water removing agent and the adsorbent are very easy to spill, in addition, two different centrifuge tubes are required to be used in the operation, the supernatant is required to be removed in the process, the operation is complicated, and the operation efficiency is low.
Disclosure of Invention
The invention aims to solve the problems that a water removing agent and an adsorbent are easy to spill out in the operation process, the operation is complicated and the efficiency is low in the QuEChERS extraction method in the prior art, and provides a combined centrifuge tube for the QuEChERS extraction method, which is novel and ingenious in structure, convenient to use and capable of improving the operation convenience and the operation efficiency.
In order to achieve the above purpose, the present invention adopts the following technical scheme: the invention relates to a combined centrifuge tube for a QuEChERS extraction method, which comprises an upper tube body with an open lower end, a lower tube body with an open upper end, an inner tube body and a puncture rod, wherein the upper part of the lower tube body is inserted into the upper tube body, the upper tube body can move up and down relative to the lower tube body and stop fixing at any time, a sleeve is arranged at the bottom of the upper end surface of the upper tube body, the upper end and the lower end of the inner tube body are both closed, the upper end surface of the inner tube body penetrates through the upper end surface of the upper tube body downwards and stretches into the sleeve, the inner tube body can slide up and down in a sealing manner relative to the sleeve, the puncture rod penetrates through the upper end surface of the inner tube body downwards and can move up and down in a sealing manner relative to the inner tube body, a liquid inlet hole is formed in the outer wall of the lower side of the inner tube body, a first sealing film is arranged in the upper tube body, the first sealing film, the upper tube body, the sleeve and the inner tube body are enclosed to form a closed water removing agent storage cavity, a second sealing film is arranged in the inner tube body, a space above the second sealing agent cavity is formed in the inner tube body, the upper space above the second sealing film, the puncture rod penetrates through the upper end surface of the inner tube body and can move up and down in a sealing manner, and a reset state is arranged between the reset mechanism and the reset mechanism is arranged at the upper end of the reset mechanism and the reset mechanism is arranged in the state, and is in a state of the reset state, and is in a state in the state of the inner tube sealing; when the elastic reset mechanism is gradually compressed, the inner pipe body slides downwards, the lower end of the inner pipe body gradually stretches into the lower pipe body, and the liquid inlet is exposed outside the sleeve and is in an open state. The invention is provided with a water scavenger storage cavity and an adsorbent storage cavity which are mutually independent, the water scavenger storage cavity and the adsorbent storage cavity are respectively pre-filled with a water scavenger and an adsorbent with fixed weight according to the requirement, when the water scavenger storage cavity and the adsorbent storage cavity are used for placing a sample and acetonitrile in a lower pipe body, an upper pipe body is connected with the lower pipe body, a first sealing film is positioned between a sleeve and the lower pipe body, the upper pipe body can downwards move for a certain distance relative to the lower pipe body, when the upper pipe body downwards moves, the first sealing film gradually approaches to and contacts with the upper end surface of the lower pipe body, and when the upper end surface of the lower pipe body finally breaks the first sealing film, the water scavenger in the water scavenger storage cavity falls into the lower pipe body, and at the moment, water scavenging operation (swirling/oscillating and centrifuging) can be carried out; after water is removed, the inner tube body is slid downwards to enable the elastic reset mechanism to be gradually compressed, the lower end of the inner tube body is gradually extended into the extracting solution in the lower tube body, the liquid inlet is gradually opened, the extracting solution flows into the inner tube body through the liquid inlet, after enough extracting solution (at least 1 mL) flows into the inner tube body, the elastic reset mechanism is reset, the inner tube body slides upwards, the liquid inlet re-enters the sleeve to be in a closed state, the extracting solution is collected in the inner tube body, at the moment, the puncture rod can be moved downwards to puncture the second sealing film, the adsorbent in the adsorbent storage cavity can fall into the extracting solution in the inner tube body, and at the moment, the purifying operation (swirling/oscillating and centrifuging) can be performed; after purification, the supernatant in the inner tube can be directly removed or poured out for detection; the combined centrifuge tube has novel and ingenious structure, is very convenient to add the water scavenger and the adsorbent, and can avoid scattering of the water scavenger and the adsorbent; during the purification operation, need not to move the extract and get into another centrifuging tube, the operation is more convenient.
Preferably, the outer wall of the lower pipe body is provided with a limiting check ring, the lower end of the upper pipe body is connected with a tearable ring, the tearable ring is in contact with the limiting check ring, and the height of the tearable ring is larger than the distance between the upper end face of the lower pipe body and the first sealing film. The lower end of the upper pipe body is fixed with the tearing ring, which plays a role in supporting and limiting the upper pipe body and is used for reserving the downward moving distance of the upper pipe body relative to the lower pipe body, and the upper pipe body can move downward after the tearing ring is torn off.
Preferably, the upper pipe body and the lower pipe body are connected through threads. The threaded connection structure is simple, firm in connection and convenient to adjust.
Preferably, the detachable pull ring comprises a pull ring, a plurality of connecting sheets fixedly connected with the lower end face of the upper pipe body are arranged on the upper end face of the pull ring at intervals, a pull-open notch is formed in the pull ring, and pull-ring buckles are arranged on any side of the pull-open notch.
Preferably, the elastic reset mechanism comprises a spring and a spring retainer ring arranged on the outer wall surface of the inner tube body, and the spring is sleeved outside the part of the inner tube body between the spring retainer ring and the upper tube body. When the inner tube is not subjected to external acting force, the inner tube is supported by the spring to be static relative to the sleeve when the spring is in a natural state; when downward pressure is applied to the inner tube, the spring is compressed, and the inner tube can slide downwards relative to the sleeve, so that the liquid inlet hole is exposed out of the sleeve.
Preferably, an opening limiting snap ring is clamped between the spring retainer ring and the upper pipe body, and the opening limiting snap ring is positioned outside the spring and surrounds the spring. The opening limiting snap ring plays a limiting role on the spring retainer ring, and spring compression caused by mistakenly touching the inner tube is avoided.
Preferably, the upper end of the inner tube body is open and provided with an end cover, and the puncture rod penetrates through the end cover downwards and can move up and down in a sealing way relative to the end cover. The end cover can be opened, and the upper end opening of the inner pipe body can be exposed after the end cover is opened, so that the supernatant in the inner pipe body can be directly removed or poured out.
Preferably, the puncture rod is in threaded connection with the end cover.
Preferably, a limiting plate is fixed at the upper end of the puncture rod.
Preferably, a supporting retainer ring is arranged on the inner wall of the inner pipe body, and the second sealing film is fixed on the supporting retainer ring. The supporting check ring not only plays a role in fixing the second sealing film, but also can keep the second sealing film tensioned when the puncture rod punctures the second sealing film, so that the second sealing film is easier to puncture.
Therefore, the invention has the following beneficial effects:
(1) The addition of the water scavenger and the adsorbent is very convenient, and the scattering of the water scavenger and the adsorbent can be avoided;
(2) During the purification operation, need not to move the extract and get into another centrifuging tube, the operation is more convenient, can improve operating efficiency.
Drawings
Fig. 1 is a cross-sectional view of the present invention.
Fig. 2 is an enlarged view at a in fig. 1.
Fig. 3 is an enlarged view at B in fig. 1.
Fig. 4 is a schematic structural view of the snap ring.
FIG. 5 is a schematic illustration of a connection of the tearable ring to the upper tube body.
In the figure: the water removing agent comprises an upper pipe body 1, a lower pipe body 2, an inner pipe body 3, a puncture rod 4, a liquid inlet 5, a first sealing film 6, a water removing agent storage cavity 7, a second sealing film 8, an adsorbent storage cavity 9, a limiting retainer ring 10, a pull ring 11, a connecting sheet 12, a pull notch 13, a pull ring buckle 14, a spring 15, a spring retainer ring 16, an opening limiting retainer ring 17, an end cover 18, a limiting plate 19, a sleeve 21, a water removing agent 22 and an adsorbent 23.
Detailed Description
The invention is further described below with reference to the drawings and detailed description.
The combined centrifuge tube for QuEChERS extraction shown in figure 1 comprises an upper tube body 1 with an open lower end, a lower tube body 2 with an open upper end, an inner tube body 3 and a puncture rod 4, wherein the upper part of the lower tube body is inserted into the upper tube body, the upper tube body and the lower tube body are connected by screw threads, the upper tube body can move up and down relative to the lower tube body and stop fixing at any time by rotating the upper tube body, a limit retainer ring 10 is arranged on the outer wall of the lower tube body, the lower end of the upper tube body is connected with a tearable pull ring which comprises pull rings 11 (shown in figure 5), a plurality of connecting sheets 12 fixedly connected with the lower end face of the upper tube body are arranged on the upper end face of the pull ring at intervals, pull ring buckles 14 are arranged on any side of the pull ring buckles, the lower end face of the pull ring contacts with the limit retainer ring, a sleeve 21 is fixed at the bottom of the upper end face of the upper tube body, an end cover 18 is arranged on the upper end of the inner tube body, the lower end of the inner tube body is closed, the upper end face of the upper pipe body penetrates through the lower pipe body and stretches into the sleeve, the inner pipe body can slide up and down in a sealing manner relative to the sleeve, the puncture rod penetrates through the end cover and is in threaded connection with the end cover, the upper end of the puncture rod is fixedly provided with a limiting plate 19, the outer wall of the lower side of the inner pipe body is provided with a liquid inlet 5 (shown in figure 3), the inside of the sleeve is sealed by liquid inlet Kong Sujin, the upper pipe body is internally provided with a first sealing film 6, the first sealing film is positioned between the sleeve and the lower pipe body, the height of the tearable ring is larger than the distance between the upper end face of the lower pipe body and the first sealing film, the upper pipe body, the sleeve and the inner pipe body are enclosed to form a sealed water remover storage cavity 7, the inner wall of the inner pipe body is provided with a supporting check ring, the supporting check ring is fixedly provided with a second sealing film 8, the space of the inner pipe body above the second sealing film forms a sealed absorbent storage cavity 9, the lower end of the puncture rod is positioned above the second sealing film, an elastic reset mechanism is arranged between the upper part of the inner pipe body and the upper end face of the upper pipe body, the elastic reset mechanism comprises a spring 15 (shown in figure 2) and a spring retainer ring 16 arranged on the outer wall surface of the inner pipe body, the spring is sleeved outside the part of the inner pipe body positioned between the spring retainer ring and the upper pipe body, an opening limit retainer ring 17 (shown in figure 4) is clamped between the spring retainer ring and the upper pipe body, the opening limit retainer ring is positioned outside the spring and surrounds the spring, when the spring is in a natural state, the inner pipe body is static, a gap is arranged between the lower end of the inner pipe body and the first sealing film, and a liquid inlet hole is positioned in a closed state in the sleeve; when the spring is gradually compressed, the inner pipe body slides downwards, the lower end of the inner pipe body gradually stretches into the lower pipe body, and the liquid inlet is exposed outside the sleeve and is in an open state.
The application method of the invention comprises the following steps: filling a crushed sample and solvent acetonitrile into a lower pipe body, connecting an upper pipe body with the lower pipe body in a threaded manner until a pull ring abuts against a limiting retainer ring, and enabling a first sealing film to be positioned between a sleeve and the lower pipe body at the moment so as to perform vortex/oscillation extraction; then tearing off the tearing ring, rotating the upper tube body to enable the upper tube body to move downwards, gradually approaching and contacting the upper end face of the lower tube body in the process, rotating the upper tube body until the upper end face of the lower tube body breaks the first sealing film, and enabling the water removing agent 22 in the water removing agent storage cavity to fall into the lower tube body, wherein water removing operation (swirling/oscillating and centrifuging) can be performed at the moment; after water is removed, the opening limiting snap ring is taken away, the puncture rod is pressed downwards, the inner pipe body is driven to move downwards through the puncture rod, the spring is gradually compressed by the spring retainer ring until the lower end of the inner pipe body gradually stretches into the extracting solution in the lower pipe body, the liquid inlet hole is gradually opened, the extracting solution flows into the inner pipe body through the liquid inlet hole, after enough extracting solution (at least 1 mL) flows into the inner pipe body, the puncture rod is loosened, the spring is reset, the inner pipe body slides upwards, the liquid inlet hole reenters the sleeve and is in a closed state, the extracting solution is collected in the inner pipe body, at the moment, the puncture rod is rotated to enable the puncture rod to move downwards to puncture the second sealing film, the puncture rod is reversely rotated after the sealing film is punctured, the puncture rod is separated from the second sealing film, the adsorbent 23 in the adsorbent storage cavity can fall into the extracting solution in the inner pipe body, and at the moment, the purifying operation (swirling/oscillating and centrifuging) can be performed; after purification, the end cover is taken away, and then the supernatant in the inner pipe can be directly removed or poured out for detection.
The above-described embodiment is only a preferred embodiment of the present invention, and is not limited in any way, and other variations and modifications may be made without departing from the technical aspects set forth in the claims.
Claims (10)
1. The QuEChERS extraction method is characterized by comprising an upper tube body (1) with an open lower end, a lower tube body (2) with an open upper end, an inner tube body (3) and a puncture rod (4), wherein the upper part of the lower tube body is inserted into the upper tube body, the upper tube body can move up and down relative to the lower tube body and stop to be fixed at any time, a sleeve (21) is arranged at the bottom of the upper end surface of the upper tube body, the upper end and the lower end of the inner tube body are both closed, the inner tube body penetrates through the upper end surface of the upper tube body and stretches into the sleeve, the inner tube body can slide up and down in a sealing manner relative to the sleeve, a liquid inlet (5) is formed in the outer wall of the lower side of the inner tube body, a first sealing film (6) is arranged in the upper tube body, a sealed water remover storage cavity (7) is formed by the first sealing film, the upper tube body and the inner tube body are enclosed, a second sealing film (8) is arranged in the inner tube body, the second sealing film is arranged in the inner tube body, the upper sealing film is positioned in the upper end surface of the inner tube body, a reset mechanism is positioned at the upper end of the inner tube body, and is positioned at the upper end of the reset cavity, and is positioned at the upper end of the reset mechanism is positioned at the upper end of the inner tube body, and is in the reset position, and is positioned at the upper sealing mechanism is positioned at the upper sealing film sealing mechanism, and is positioned at the reset position; when the elastic reset mechanism is gradually compressed, the inner pipe body slides downwards, the lower end of the inner pipe body gradually stretches into the lower pipe body, and the liquid inlet is exposed outside the sleeve and is in an open state.
2. The QuEChERS extraction method combined centrifuge tube according to claim 1, wherein a limiting check ring (10) is arranged on the outer wall of the lower tube body, the lower end of the upper tube body is connected with a tearable ring, the tearable ring is in contact with the limiting check ring, and the height of the tearable ring is larger than the distance between the upper end face of the lower tube body and the first sealing film.
3. A modular centrifuge tube for use in a QuEChERS extraction process according to claim 1 or 2 wherein the upper and lower tubular bodies are threadably connected.
4. The QuEChERS extraction method used combined centrifuge tube according to claim 2, wherein the tearable pull ring comprises pull rings (11), a plurality of connecting sheets (12) fixedly connected with the lower end face of the upper tube body are arranged on the upper end face of the pull rings at intervals, pull-open notches (13) are arranged on the pull rings, and pull-ring buckles (14) are arranged on any side of the pull-open notches.
5. The QuEChERS extraction method combined centrifugal tube according to claim 1, wherein the elastic reset mechanism comprises a spring (15) and a spring retainer ring (16) arranged on the outer wall surface of the inner tube body, and the spring is sleeved outside the part of the inner tube body between the spring retainer ring and the upper tube body.
6. The QuEChERS extraction method combined centrifugal tube according to claim 5, wherein an opening limiting clamp ring (17) is clamped between the spring retainer ring and the upper tube body, and the opening limiting clamp ring is positioned outside and surrounds the spring.
7. The QuEChERS extraction method of claim 1, wherein the inner tube body is open at the upper end and provided with an end cap (18), and the piercing rod passes through the end cap downwards and can move up and down in a sealing manner relative to the end cap.
8. The modular centrifuge tube of claim 7, wherein the piercing rod is threadably coupled to the cap.
9. A modular centrifuge tube for use in the QuEChERS extraction process according to claim 1, 7 or 8 wherein a stop plate (19) is secured to the upper end of the piercing rod.
10. The modular centrifuge tube for use in a QuEChERS extraction process of claim 1 wherein a backup ring is provided on the inner wall of the inner tube body and the second sealing membrane is secured to the backup ring.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210472981.4A CN114870924B (en) | 2022-04-29 | 2022-04-29 | Combined centrifuge tube for QuEChERS extraction method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210472981.4A CN114870924B (en) | 2022-04-29 | 2022-04-29 | Combined centrifuge tube for QuEChERS extraction method |
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| Publication Number | Publication Date |
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| CN114870924A CN114870924A (en) | 2022-08-09 |
| CN114870924B true CN114870924B (en) | 2023-05-26 |
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| Application Number | Title | Priority Date | Filing Date |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2018036258A (en) * | 2016-08-30 | 2018-03-08 | 三浦工業株式会社 | Method for preparing analytical sample of residual pesticide |
| CN210458222U (en) * | 2019-08-22 | 2020-05-05 | 奥然科技生物(深圳)有限责任公司 | Trace amount DNA extraction capsule |
| CN111603385A (en) * | 2020-06-15 | 2020-09-01 | 王建平 | Liquid-dropping type capsule capable of being separately stored and mixed for use |
| CN213327596U (en) * | 2020-05-07 | 2021-06-01 | 立森印迹诊断技术（无锡）有限公司 | Collection container and kit |
| CN216207777U (en) * | 2021-10-09 | 2022-04-05 | 上海康黎诊断技术有限公司 | Sputum sample collecting tube |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030013205A1 (en) * | 2001-07-06 | 2003-01-16 | Franz Konrad | Separating device |
| JP5661740B2 (en) * | 2010-03-15 | 2015-01-28 | 鷹仁 松村 | Vacuum blood collection tube, blood collection unit, and inspection method identification device |
| US11193930B2 (en) * | 2016-08-02 | 2021-12-07 | DPX Technologies, LLC | Automated protein precipitation and/or dispersive solid phase extraction using filter tips |
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2022
- 2022-04-29 CN CN202210472981.4A patent/CN114870924B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2018036258A (en) * | 2016-08-30 | 2018-03-08 | 三浦工業株式会社 | Method for preparing analytical sample of residual pesticide |
| CN210458222U (en) * | 2019-08-22 | 2020-05-05 | 奥然科技生物(深圳)有限责任公司 | Trace amount DNA extraction capsule |
| CN213327596U (en) * | 2020-05-07 | 2021-06-01 | 立森印迹诊断技术（无锡）有限公司 | Collection container and kit |
| CN111603385A (en) * | 2020-06-15 | 2020-09-01 | 王建平 | Liquid-dropping type capsule capable of being separately stored and mixed for use |
| CN216207777U (en) * | 2021-10-09 | 2022-04-05 | 上海康黎诊断技术有限公司 | Sputum sample collecting tube |
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