Built-in trace nuclear magnetic resonance sample tube
By designing an internal micro NMR sample tube, utilizing an outer tube and an inner rod structure, the problems of inconvenient operation and large reagent consumption of existing micro NMR sample tubes are solved, achieving reduced sample solution volume, increased concentration, and reduced cost, while obtaining high-quality NMR spectra.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-30
- Publication Date
- 2026-04-07
AI Technical Summary
Existing micro NMR sample tubes are similar in length to conventional sample tubes, which are inconvenient to operate and expensive. They cannot effectively reduce the volume of sample solution, resulting in large reagent consumption, high costs, and severe interference between solvent signals and water peak signals.
Design an internal micro-nuclear magnetic resonance sample tube, which adopts an outer tube and an inner rod structure. The inner rod is inserted into the outer tube to reduce the volume and raise the liquid level. A gap is formed between the inner wall of the outer tube and the outer wall of the inner rod to hold the sample solution. The bottom end of the inner rod fits in the center with the bottom of the outer tube. The inner diameter of the outer tube is 3.0 to 3.5 mm, the outer diameter of the inner rod is 1.0 to 2.0 mm, and the length is 6.0 to 8.0 cm.
It reduces the volume of sample solution required for NMR testing, increases sample concentration, obtains higher quality NMR spectra, reduces reagent consumption, lowers analysis costs, and facilitates sample addition.
Smart Images
Figure CN224086787U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model belongs to the technical field of organic sample nuclear magnetic resonance (NMR) analysis, especially relates to a built-in trace nuclear magnetic resonance sample tube. BACKGROUND
[0002] NMR spectrum analysis is an important organic compound structure analysis means, is widely used in chemistry, biology, medicine and other fields. The conventional NMR analysis uses the sample tube with the outer diameter of 5mm, needs to fill about 500uL sample solution when testing. For some trace compounds, such as NMR hydrogen spectrum detection can be carried out with less sample solution, then the concentration of sample solution can be improved accordingly, so as to reduce the interference of solvent signal and water peak signal, and higher quality NMR spectrum is obtained. In addition, the price of some deuterium reagent is higher, and it cannot be recycled, if micro sample tube that is more convenient for experimental operation is used for daily NMR detection, then the experimental cost can be effectively reduced. At present, some trace NMR sample tubes with thin inner diameter on the market are inconvenient to sample and sample recovery due to the proximity of their length and the length of the conventional NMR sample tube with the outer diameter of 5mm, and the price of such trace NMR sample tubes is higher, or special rotors need to be used. SUMMARY
[0003] In view of the above problems existing in the prior art, the purpose of the embodiments of the utility model is to provide a built-in trace nuclear magnetic resonance sample tube.
[0004] The technical scheme adopted by the embodiments of the utility model is a built-in trace nuclear magnetic resonance sample tube, which comprises an outer tube, an inner plug rod is inserted into the outer tube, there is a gap between the inner wall of the outer tube and the outer wall of the inner plug rod, the gap is used to contain sample solution, and the inner plug rod is used to be inserted into the outer tube to reduce the volume of the outer tube and raise the liquid level in the outer tube.
[0005] Further, the bottom of the inner cavity of the outer tube is configured as an arc shape matched with the bottom end of the inner plug rod, and the arc-shaped inner cavity bottom of the outer tube is used to guide the bottom end of the inner plug rod to the central position of the bottom end of the outer tube.
[0006] Further, the bottom end of the inner plug rod is configured as a convex shape, and the convex-shaped bottom end of the inner plug rod is used to cooperate with the arc-shaped inner cavity bottom of the outer tube to guide the bottom end of the inner plug rod to the central position of the bottom end of the outer tube.
[0007] Further, the inner plug rod is configured as a solid or hollow shape.
[0008] Further, the outer diameter of the outer tube is 3.0 to 3.5mm, the inner diameter is 1.5 to 2.5mm, and the length is 5.0 to 7.0cm.
[0009] Further, the outer diameter of the inner insertion rod is 1.0-2.0 mm, and the length is 6.0-8.0 cm.
[0010] Further, a plurality of first protrusions are arranged on the outer wall of the inner insertion rod, and the first protrusions are centrally symmetrically distributed with the inner insertion rod as the axis; when the inner insertion rod is inserted into the outer tube, the end of the first protrusion away from the inner insertion rod abuts against the inner wall of the outer tube, so that the inner insertion rod is in a centered position after being inserted into the outer tube.
[0011] Further, a plurality of second protrusions are arranged on the inner wall of the outer tube, and the second protrusions are centrally symmetrically distributed with the central axis of the outer tube as the axis; when the inner insertion rod is inserted into the outer tube, the end of the second protrusion away from the inner wall of the outer tube abuts against the outer wall of the inner insertion rod, so that the inner insertion rod is in a centered position after being inserted into the outer tube.
[0012] Compared with the prior art, the built-in micro nuclear magnetic resonance sample tube can reduce the volume of the sample solution required for NMR testing, improve the concentration of the micro sample, and help obtain a higher quality NMR spectrum. When used for conventional NMR detection, the amount of reagent can be effectively reduced, and the analysis cost can be reduced. And in the case of using the same volume of reagent, the inner diameter of the outer tube can be larger by using the inner insertion rod, and the sample can be conveniently added.
[0013] It should be understood that the foregoing general description and the following detailed description are only exemplary and explanatory, and are not intended to limit the present application.
[0014] The foregoing summary of various implementations or examples of the technology described in this application is not a comprehensive disclosure of the entire scope or all features of the disclosed technology. BRIEF DESCRIPTION OF DRAWINGS
[0015] In the drawings, which are not necessarily drawn to scale, like numerals can describe similar components in different views. Like numerals having different letter suffixes can represent different instances of similar components. The drawings illustrate generally, by way of example, various embodiments of the application and are not intended to limit the application. The same reference numerals in different drawings can identify the same or similar elements. Such embodiments of the application can be used in any combination, and exchange of elements between embodiments is contemplated.
[0016] Figure 1 It is an overall schematic view of the first protrusion constructed on the inner insertion rod of the embodiment of the application.
[0017] Figure 2 It is a cross-sectional schematic view of the first protrusion constructed on the inner insertion rod of the embodiment of the application.
[0018] Figure 3 This is an overall schematic diagram of the second protrusion constructed on the outer tube according to an embodiment of the present invention.
[0019] Figure 4 This is a cross-sectional schematic diagram of the second protrusion on the outer tube according to an embodiment of the present invention.
[0020] Figure 5 The hydrogen spectrum is the result of comparative test 1 of this utility model embodiment.
[0021] Figure 6 The hydrogen spectrum is shown in Comparative Test 2 of this utility model embodiment. Detailed Implementation
[0022] To make the objectives, technical solutions, and advantages of the embodiments of this utility model clearer, the technical solutions of the embodiments of this utility model will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this utility model. All other embodiments obtained by those skilled in the art based on the described embodiments of this utility model without creative effort are within the scope of protection of this utility model.
[0023] Unless otherwise defined, the technical or scientific terms used in this utility model shall have the ordinary meaning understood by one of ordinary skill in the art to which this utility model pertains. The terms "first," "second," and similar terms used in this utility model do not indicate any order, quantity, or importance, but are merely used to distinguish different components. Terms such as "comprising" or "including" mean that the element or object preceding the word encompasses the elements or objects listed following the word and their equivalents, without excluding other elements or objects. Terms such as "connected" or "linked" are not limited to physical or mechanical connections, but can include electrical connections, whether direct or indirect. Terms such as "upper," "lower," "left," and "right" are used only to indicate relative positional relationships; when the absolute position of the described object changes, the relative positional relationship may also change accordingly.
[0024] To keep the following description of the embodiments of this utility model clear and concise, detailed descriptions of known functions and known components are omitted.
[0025] See Figures 1 to 4 This utility model provides an internal micro-nuclear magnetic resonance sample tube, including an outer tube 1, an inner insert rod 2 inserted into the outer tube 1, and a gap between the inner wall of the outer tube 1 and the outer wall of the inner insert rod 2. The gap is used to hold a sample solution, and the inner insert rod 2 is used to be inserted into the outer tube 1 to reduce the volume of the outer tube 1 and increase the liquid level inside the outer tube 1.
[0026] The built-in micro NMR sample tube proposed in this technical solution reduces the volume of sample solution required for NMR testing, increases the concentration of trace samples, and helps obtain higher quality NMR spectra. Using it for routine NMR detection can effectively reduce reagent consumption and lower analytical costs. Furthermore, using the inner insert rod allows for the use of an outer tube with a larger inner diameter, facilitating sample addition, while maintaining the same volume of reagent. Before testing the NMR sample, add approximately 2 cm of sample solution to the outer tube 1, then insert the inner insert rod 2 to raise the liquid level to approximately 4 cm, the height required for NMR spectra testing. The assembled sample tube is then placed in a standard 5 mm outer diameter NMR tube, and detection can be performed using conventional methods.
[0027] In some embodiments, the bottom of the inner cavity of the outer tube 1 is constructed in an arc shape to cooperate with the bottom end of the inner rod 2, and the arc-shaped bottom of the inner cavity of the outer tube 1 is used to guide the bottom end of the inner rod 2 to the center position of the bottom end of the outer tube 1.
[0028] In some embodiments, the bottom end of the inner insert rod 2 is constructed to be protruding, and the protruding bottom end of the inner insert rod 2 is used to cooperate with the bottom of the arc-shaped inner cavity of the outer tube 1 to guide the bottom end of the inner insert rod 2 to the center position of the bottom end of the outer tube 1.
[0029] The arc-shaped inner cavity bottom of the outer tube 1 and the protruding bottom end of the inner rod 2 cooperate with each other to effectively guide the bottom end of the inner rod 2 to the center position of the bottom end of the outer tube 1.
[0030] In some embodiments, the insert rod 2 is constructed to be solid or hollow.
[0031] In some embodiments, the outer tube 1 has an outer diameter of 3.0 to 3.5 mm, an inner diameter of 1.5 to 2.5 mm, and a length of 5.0 to 7.0 cm.
[0032] In some embodiments, the outer diameter of the insert rod 2 is 1.0 to 2.0 mm and the length is 6.0 to 8.0 cm.
[0033] Referring to 1 to 2, in some embodiments, a plurality of first protrusions 3 are provided on the outer wall of the inner insert rod 2. The first protrusions 3 are centrally symmetrically distributed about the inner insert rod 2. When the inner insert rod 2 is inserted into the outer tube 1, the ends of the first protrusions 3 away from the inner insert rod 2 abut against the inner wall of the outer tube 1 so that the inner insert rod 2 is in a central position after being inserted into the outer tube 1.
[0034] Referring to 3 to 4, in some embodiments, a plurality of second protrusions 4 are provided on the inner wall of the outer tube 1. The second protrusions 4 are centrally symmetrically distributed with the central axis of the outer tube 1 as the axis. When the inner rod 2 is inserted into the outer tube 1, the end of the second protrusion 4 away from the inner wall of the outer tube 1 abuts against the outer wall of the inner rod 2 so that the inner rod 2 is in a central position after being inserted into the outer tube 1.
[0035] The function of either the first protrusion 3 or the second protrusion 4 is to ensure that the inner rod 2 is centered after being inserted into the outer tube 1.
[0036] When the inner diameter of the outer tube 1 is 2 mm and the outer diameter of the inner insert 2 is 1.5 mm, only about 50 μL of sample solution is needed to fill the tube to the required height for NMR testing. This is 90% less than the 500 μL required for a conventional 5 mm outer diameter NMR tube, thus reducing reagent consumption and significantly lowering analytical costs. Using the built-in micro-volume NMR sample tube proposed in this technical solution for testing micro-samples can reduce reagent usage, increase solution concentration by 10 times, and obtain higher quality spectra.
[0037] Comparative Experiment 1:
[0038] The effects of using built-in micro-nuclear magnetic resonance sample tubes, with solid and hollow quartz inserters inserted respectively, to detect the hydrogen spectroscopy of phlorizin, a natural product of the same mass, were compared.
[0039] 1.5 mg of phlorizin was dissolved in 150 μL of deuterated methanol. 50 μL of this solution was pipetted into a built-in micro-NMR sample tube with an outer diameter of 3 mm, an inner diameter of 2 mm, and a length of 6 cm. A hollow quartz insert rod with an outer diameter of 1.5 mm, an inner diameter of 0.6 mm, and both ends sealed by firing was inserted into the tube, bringing the liquid level in the micro-NMR tube to approximately 4 cm. This was then placed in a conventional NMR tube with an outer diameter of 5 mm, and 32 measurements were accumulated using a Bruker AM-400 MHz NMR spectrometer. The obtained proton NMR spectrum is shown below. Figure 5 The upper curve in the middle.
[0040] Using a pipette, 50 μL of the remaining phlorizin deuterated methanol solution was added to an internal micro-NMR sample tube with an outer diameter of 3 mm, an inner diameter of 2 mm, and a length of 6 cm. A solid quartz insert rod with an outer diameter of 1.5 mm and a length of 7 cm was inserted into the tube, bringing the liquid level in the micro-NMR tube to approximately 4 cm. This tube was then placed in a conventional NMR tube with an outer diameter of 5 mm, and 32 measurements were accumulated using a Bruker AM-400MHz NMR spectrometer. The obtained proton NMR spectrum is shown below. Figure 5 The lower curve in the middle.
[0041] By comparison Figure 5The two proton spectra shown in the image reveal that using a solid or hollow insert rod has little effect on the proton spectrum.
[0042] Comparative Test 2:
[0043] A comparison of the performance of the built-in micro-NMR sample tube proposed in this technical solution and the conventional NMR sample tube with an outer diameter of 5 mm for detecting the same mass of phlorizin 1H NMR spectrum.
[0044] 1. Dissolve 1.5 mg of phlorizin in 60 μL of deuterated methanol. Pipette the solution entirely into a 3.0 mm outer diameter, 2.4 mm inner diameter, and 6 cm long soda-lime glass internal micro-NMR sample tube. Insert a 2.0 mm outer diameter, 1.6 mm inner diameter soda-lime glass insert rod sealed at both ends. Place the tube in a 5 mm outer diameter conventional NMR tube and perform 32 cycles using a Bruker AM-400 MHz NMR spectrometer. The obtained proton NMR spectrum is shown below. Figure 6 The image in the image is "1: GPG-3.0x2.4+2.0mm".
[0045] 2. Dissolve 1.5 mg of phlorizin in 110 μL of deuterated methanol, and pipette the entire solution into a 3.0 mm outer diameter, 2.4 mm inner diameter, and 6 cm long soda-lime glass internal micro-NMR sample tube. Insert a 1.5 mm outer diameter solid quartz glass insert rod into the tube, and place it in a 5 mm outer diameter conventional NMR tube. Perform 32 cycles using a Bruker AM-400 MHz NMR spectrometer. The obtained proton NMR spectrum is shown below. Figure 6 The image in question is "2: GPG-3.0x2.4+1.5mm".
[0046] 3. Dissolve 1.5 mg of phlorizin in 110 μL of deuterated methanol, and pipette the entire solution into a 3.0 mm outer diameter, 1.8 mm inner diameter, and 6 cm length soda-lime glass internal micro-NMR sample tube. Place the tube in a 5 mm outer diameter conventional NMR tube and perform 32 cycles using a Bruker AM-400 MHz NMR spectrometer. The obtained proton NMR spectrum is shown below. Figure 6 The image in the image is “4: GPG-3.0x1.8mm”.
[0047] 4. Dissolve 1.5 mg of phlorizin in 130 μL of deuterated methanol, and pipette the entire solution into a quartz glass built-in micro NMR sample tube with an outer diameter of 3.0 mm, an inner diameter of 2.0 mm, and a length of 6 cm. Place the tube in a standard NMR tube with an outer diameter of 5 mm, and perform 32 cycles using a Bruker AM-400 MHz NMR spectra. The obtained proton NMR spectrum is shown below. Figure 6 The image in the image is “4: GPG-3.0x2.0mm”.
[0048] 5. Dissolve 1.5 mg of phlorizin in 600 μL of deuterated methanol, and add the entire solution to a standard NMR tube with an outer diameter of 5 mm using a pipette. Perform 32 pulses using a Bruker AM-400 MHz NMR spectra. The obtained proton NMR spectrum is shown below. Figure 6 The spectrum in the image is "5: GPG-5mm standard".
[0049] Comparison reveals that when the methanol solvent signal at 3.31 ppm is very close, the signal intensity of the natural product phlorizin in the proton spectrum measured using the built-in micro NMR sample tube proposed in this technical solution is significantly higher than that measured using a conventional NMR sample tube with a 5 mm outer diameter.
[0050] The above description is intended to be illustrative and not restrictive. Those skilled in the art can make variations, modifications, substitutions, and alterations to the above embodiments within the scope of this disclosure. Moreover, the above examples (or one or more of them) can be used in combination with each other, and these embodiments can be combined with each other in various combinations or arrangements.
Claims
1. An internal micro-nuclear magnetic resonance sample tube, comprising an outer tube (1), characterized in that, An inner insert rod (2) is inserted into the outer tube (1). There is a gap between the inner wall of the outer tube (1) and the outer wall of the inner insert rod (2). The gap is used to hold the sample solution. The inner insert rod (2) is used to be inserted into the outer tube (1) to reduce the volume of the outer tube (1) and raise the liquid level inside the outer tube (1).
2. The built-in micro-nuclear magnetic resonance sample tube according to claim 1, characterized in that, The bottom of the inner cavity of the outer tube (1) is constructed in an arc shape to match the bottom end of the inner rod (2). The arc-shaped bottom of the inner cavity of the outer tube (1) is used to guide the bottom end of the inner rod (2) to the center position of the bottom end of the outer tube (1).
3. The built-in micro-nuclear magnetic resonance sample tube according to claim 2, characterized in that, The bottom end of the inner rod (2) is convex and is used to cooperate with the bottom of the arc-shaped inner cavity of the outer tube (1) to guide the bottom end of the inner rod (2) to the center position of the bottom end of the outer tube (1).
4. The built-in micro-nuclear magnetic resonance sample tube according to claim 1, characterized in that, The insert rod (2) is constructed to be solid or hollow.
5. The built-in micro-nuclear magnetic resonance sample tube according to claim 1, characterized in that, The outer tube (1) has an outer diameter of 3.0 to 3.5 mm, an inner diameter of 1.5 to 2.5 mm, and a length of 5.0 to 7.0 cm.
6. The built-in micro-nuclear magnetic resonance sample tube according to claim 1, characterized in that, The inner insert (2) has an outer diameter of 1.0 to 2.0 mm and a length of 6.0 to 8.0 cm.
7. A built-in micro-nuclear magnetic resonance sample tube according to any one of claims 1 to 6, characterized in that, The outer wall of the inner rod (2) is provided with a plurality of first protrusions (3). The first protrusions (3) are centrally symmetrically distributed about the inner rod (2). When the inner rod (2) is inserted into the outer tube (1), the end of the first protrusion (3) away from the inner rod (2) abuts against the inner wall of the outer tube (1) so that the inner rod (2) is in the center position after being inserted into the outer tube (1).
8. A built-in micro-nuclear magnetic resonance sample tube according to any one of claims 1 to 6, characterized in that, The inner wall of the outer tube (1) is provided with a plurality of second protrusions (4). The second protrusions (4) are centrally symmetrically distributed with the central axis of the outer tube (1) as the axis. When the inner rod (2) is inserted into the outer tube (1), the end of the second protrusion (4) away from the inner wall of the outer tube (1) abuts against the outer wall of the inner rod (2) so that the inner rod (2) is in the center position after being inserted into the outer tube (1).