A method for dissolving a dansyl chloride derivative solution and a reagent bottle assembly for preparation

In the preparation process of the densulphonyl chloride derivative solution, light shielding environment and gas replacement technology are used to combine the reduction effect of antioxidants to form the final solvent, which solves the problems of light, oxidation and temperature increase in the prior art, and significantly improves the sensitivity of bioamine detection.

CN112973482BActive Publication Date: 2025-06-24SHANGHAI OCEAN UNIV
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Patent Information

Application Number
CN202110379090.X
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2021-04-08
Publication Date
2025-06-24
Estimated Expiration
2041-04-08

AI Technical Summary

Technical Problem

During the preparation of existing denssulfonyl chloride derivative solutions, it is difficult to completely avoid light, oxidation and temperature increase, resulting in a decrease in the sensitivity of bioamine detection.

Method used

By placing the predetermined solvent in a light-shielding environment, and displacing the oxygen in the initial solvent with the predetermined gas, adding a predetermined antioxidant for reducing it, forming a final solvent for dissolving the dansulfonyl chloride derivative solution, ensuring light-proof, oxygen isolation and constant temperature.

Benefits of technology

It effectively improves the sensitivity of bioamine detection and ensures the stability and detection accuracy of dansulfonyl chloride.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention belongs to the field of food detection, and discloses a method for dissolving dansyl chloride derivatizing agent solution, which can simultaneously ensure light avoidance, oxygen isolation and constant temperature of dansyl chloride, greatly improving the sensitivity of biogenic amine detection. This method obtains the final solvent by performing gas displacement and reduction on a predetermined solvent, and dissolves the dansyl chloride derivatizing agent solution with the final solvent.
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Description

Technical Field

[0001] The present invention belongs to the field of food detection, and particularly relates to a method for dissolving dansyl chloride derivatizing agent solution. Background Art

[0002] In the process of determining biogenic amines in food, dansyl chloride derivatizing agent solution is necessary. It reacts with biogenic amines in food to generate substances that can be detected by an ultraviolet detector, so as to assist in the effective determination of biogenic amines.

[0003] When preparing dansyl chloride derivatizing agent solution, light avoidance and oxidation prevention should be considered simultaneously, so that dansyl chloride is not oxidized or photolyzed, which affects the effectiveness of dansyl chloride derivatizing agent solution. At the same time, the dansyl chloride derivatizing agent solution needs to be stably maintained at a certain low temperature to prevent the dansyl chloride derivatizing agent solution from being oxidized, thereby effectively maintaining the sensitivity of biogenic amine detection.

[0004] However, in the preparation process of dansyl chloride derivatizing agent solution so far, because it needs to be completed through multiple transfer operations, it is very difficult to completely avoid light, oxidation or temperature rise during this process, which seriously affects the sensitivity of biogenic amine detection. Summary of the Invention

[0005] Aiming at the deficiencies of the prior art, the present invention provides a method for dissolving dansyl chloride derivatizing agent solution. By implementing the method for dissolving dansyl chloride derivatizing agent solution through a reagent bottle assembly for preparing dansyl chloride derivatizing agent solution, the light avoidance, oxygen isolation and constant temperature of dansyl chloride are ensured simultaneously, greatly improving the sensitivity of biogenic amine detection.

[0006] To achieve the above object, the present invention provides the following technical solutions.

[0007] A method for dissolving dansyl chloride derivatizing agent solution, using acetone at a predetermined temperature as a predetermined solvent,

[0008] characterized by including the following steps.

[0009] Step S1: Place the predetermined solvent in a light-shielded environment to obtain an initial solvent.

[0010] Step S2: Replace the oxygen in the initial solvent with a predetermined gas to obtain an intermediate solvent.

[0011] Step S3: Add a predetermined antioxidant to the intermediate solvent for reduction to obtain a final solvent.

[0012] Step S4: Dissolve the dansyl chloride derivatizing agent solution with the final solvent.

[0013] Preferably, in step S2, more than 99.5% of the oxygen in the initial solvent is replaced by the predetermined gas.

[0014] Preferably, in step S2, the predetermined gas is nitrogen, and the replacement method is bubbling for 10 to 12.5 minutes.

[0015] Preferably, in step S3, the predetermined antioxidant is sodium borohydride, and 0.2 - 0.5 g of the predetermined antioxidant is added to each liter of the intermediate solvent.

[0016] Preferably, in step S3, the predetermined antioxidant reduces more than 90% of the oxygen in the intermediate solvent.

[0017] Preferably, in step S3, the reduction method is to bubble the intermediate solvent with the predetermined gas for 5 to 6 minutes, so as to accelerate the dissolution of the predetermined antioxidant in the intermediate solvent.

[0018] Preferably, the predetermined temperature range is 0°C to 10°C.

[0019] A reagent bottle assembly for preparing a dansyl chloride derivatizing agent solution, which is used to implement the method for dissolving a dansyl chloride derivatizing agent solution, and is characterized by including: an open outer bottle containing predetermined ice water; a preparation inner bottle containing a predetermined solvent, and a part of the preparation inner bottle is arranged in the predetermined ice water; and a bubbler, including a bubbling pressure vessel and a container valve, the bubbling pressure vessel contains a predetermined gas, wherein the bubbling pressure vessel is located at the bottom of the inner cavity of the preparation inner bottle, and the container valve is located outside the preparation inner bottle and the container valve is used to control the bubbling of the bubbling pressure vessel into the predetermined solvent.

[0020] Preferably, the height of the liquid level of the predetermined solvent relative to the bottom of the preparation inner bottle is within 2 / 3 of the height of the preparation inner bottle, and is used as the solvent height. The surface of the preparation inner bottle is provided with a detachable liquid level observation window, and the height range of the liquid level observation window relative to the bottom of the preparation inner bottle is 4 / 5 to 5 / 6 of the height of the preparation inner bottle.

[0021] Furthermore, the outer surface of the preparation inner bottle corresponding to the solvent height is fully pasted with a light-shielding film.

[0022] Compared with the prior art, the beneficial effects of the present invention are as follows.

[0023] 1. Since the method for dissolving a dansyl chloride derivatizing agent solution of the present invention obtains the final solvent by gas replacement and reduction of the predetermined solvent, and dissolves the dansyl chloride derivatizing agent solution with the final solvent, therefore, the present invention can simultaneously ensure the light shielding, oxygen isolation and constant temperature of dansyl chloride, greatly improving the sensitivity of biogenic amine detection.

[0024] 2. Since the predetermined gas of the present invention is nitrogen and the replacement method is bubbling for 10 to 12.5 minutes, therefore,

[0025] The present invention can greatly reduce the oxygen content in the initial solvent within a closed space and can isolate the contact between the initial solvent and oxygen in the environment, further improving the oxygen isolation effect.

[0026]

[0027] 3. Since the predetermined antioxidant of the present invention is sodium borohydride, 0.2 - 0.5 g of the predetermined antioxidant is added to each liter of the intermediate solvent, and the intermediate solvent is bubbled with the predetermined gas for 5 to 6 minutes, so that the predetermined antioxidant in the intermediate solvent is accelerated in dissolution. Therefore, the present invention can further reduce the residual oxygen in the intermediate solvent through the predetermined antioxidant accelerated in dissolution by bubbling, making the oxygen content in the final solvent further reduced.

[0028] 4. Since the reagent bottle assembly for preparing the dansyl chloride derivatizing agent solution of the present invention is used to implement the method for dissolving the dansyl chloride derivatizing agent solution, including an open outer bottle, a preparation inner bottle and a bubbler, the bubbler includes a bubbling pressure vessel and a container valve, the bubbling pressure vessel contains the predetermined gas, the bubbling pressure vessel is located at the bottom of the inner cavity of the preparation inner bottle, and the container valve is located outside the preparation inner bottle and the container valve is used to control the bubbling of the bubbling pressure vessel into the predetermined solvent, therefore, the reagent bottle assembly for preparing the dansyl chloride derivatizing agent solution of the present invention can effectively implement the method for dissolving the dansyl chloride derivatizing agent solution.

[0029] 5. Since the height of the liquid level of the predetermined solvent relative to the bottom of the preparation inner bottle is within 2 / 3 of the height of the preparation inner bottle, and the surface of the preparation inner bottle is provided with a detachable liquid level observation window, and the height range of the liquid level observation window relative to the bottom of the preparation inner bottle is 4 / 5 to 5 / 6 of the height of the preparation inner bottle, therefore, the present invention can not only observe the inside of the preparation inner bottle from the outside, but also add the predetermined antioxidant into the predetermined solvent by removing the liquid level observation window.

[0030] 6. Since the outer surface of the preparation inner bottle corresponding to the height of the solvent is fully pasted with a light-shielding film, therefore, the present invention effectively ensures the light-shielding effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 is a schematic diagram of the steps of the method for dissolving the dansyl chloride derivatizing agent solution according to an embodiment of the present invention.

[0032] Figure 2 is a schematic structural diagram of the reagent bottle assembly for preparing the dansyl chloride derivatizing agent solution according to an embodiment of the present invention.

[0033] In the figure: S100 is the method for dissolving dansyl chloride derivative solution; 100 is the reagent bottle assembly for preparing dansyl chloride derivative solution; 10 is the open outer bottle; A is the predetermined ice water; 20 is the inner bottle for preparation; B is the predetermined solvent; 21 is the inner bottle cap; 211 is the air outlet channel; 212 is the small channel sealing cap; 22 is the inner bottle body; 221 is the liquid level observation window; 23 is the light-shielding film; 30 is the bubbler; C is the connecting pipeline; 31 is the container valve; 32 is the bubbling pressure vessel. Detailed implementation mode

[0034] In order to make the technical means, creative features, achieved purposes and effects of the present invention easy to understand, the following embodiments will specifically elaborate on a method for dissolving dansyl chloride derivative solution and a reagent bottle assembly for preparation in combination with the accompanying drawings. It should be noted that the description of these embodiments is used to help understand the present invention, but does not constitute a limitation to the present invention.

[0035] As Figure 1 shown, in this embodiment, a method S100 for dissolving dansyl chloride derivative solution uses acetone at a predetermined temperature as the predetermined solvent. Specifically, the predetermined temperature range is from 0°C to 10°C.

[0036] The method S100 for dissolving dansyl chloride derivative solution includes the following steps.

[0037] Step S1: Place the predetermined solvent in a light-shielded environment to obtain the initial solvent.

[0038] Step S2: Replace the oxygen in the initial solvent with a predetermined gas to obtain the intermediate solvent.

[0039] Specifically, the predetermined gas is nitrogen, and the replacement method is bubbling for 10 to 12.5 minutes. Through bubbling, more than 99.5% of the oxygen in the initial solvent is replaced by the predetermined gas.

[0040] Step S3: Add a predetermined antioxidant to the intermediate solvent for reduction to obtain the final solvent.

[0041] Specifically, the predetermined antioxidant is sodium borohydride. The addition method is to add 0.2 - 0.5 g of the predetermined antioxidant per liter of the intermediate solvent. The predetermined antioxidant reduces more than 90% of the oxygen in the intermediate solvent, and the reduction process is assisted by bubbling the intermediate solvent with the predetermined gas for 5 to 6 minutes.

[0042] Step S4: Dissolve the dansyl chloride derivative solution with the final solvent.

[0043] As Figure 2As shown in the figure, this embodiment also provides a reagent bottle assembly 100 for preparing dansyl chloride derivative solution, which is used to implement the method S100 for dissolving dansyl chloride derivative solution, and includes an open outer bottle 10, a preparation inner bottle 20, and a bubbler 30.

[0044] The open outer bottle 10 is a container with an open upper part, and contains a predetermined ice water A inside. The temperature range of the predetermined ice water A is 0°C to 10°C.

[0045] The preparation inner bottle 20 is arranged inside the open outer bottle 10, and part of the preparation inner bottle 20 is arranged in the predetermined ice water A. The preparation inner bottle 20 contains a predetermined solvent B. Specifically, the predetermined solvent B is acetone at 0°C to 10°C.

[0046] The preparation inner bottle 20 includes an inner bottle cap 21, an inner bottle body 22, and a light-shielding film 23.

[0047] The inner bottle cap 21 is covered on the inner bottle body 22, and has an air outlet channel 211 communicating with the inner cavity of the inner bottle body 22 and a channel sealing small cover 212 for controlling the opening or closing of the air outlet channel 211 relative to the external environment.

[0048] The inner bottle body 22 contains a predetermined solvent B. The predetermined solvent B in the inner bottle body 22 is in a light-shielded environment, that is, the initial solvent. The height of the liquid level of the predetermined solvent B relative to the bottom of the preparation inner bottle 20 is within 2 / 3 of the height of the preparation inner bottle 20, and is used as the solvent height. Here, the bottom of the preparation inner bottle 20 refers to the bottom of the inner bottle body 22.

[0049] The surface of the preparation inner bottle 20 is provided with a detachable liquid level observation window 221, that is, the surface of the inner bottle body 22 is provided with a detachable liquid level observation window 221. The height range of the liquid level observation window 221 relative to the bottom of the preparation inner bottle is 4 / 5 to 5 / 6 of the height of the preparation inner bottle. The liquid level observation window 221 is made of a transparent material. Through the liquid level observation window 221, the inside of the preparation inner bottle 20 can be observed from the outside of the preparation inner bottle 20. In this embodiment, the liquid level observation window 221 is located outside the open outer bottle 10. The liquid level observation window 221 is detachably engaged with a corresponding through hole (not marked in the attached drawing) preset on the surface of the inner bottle body 22, and a sealing strip (not marked in the attached drawing) is provided at the edge of the corresponding through hole. When the liquid level observation window 221 is detachably engaged with the corresponding through hole, the sealing strip can seal the gap.

[0050] The light-shielding film 23 is fully attached to the outer surface of the preparation inner bottle 20, that is, the outer surface of the inner bottle body 22, and the full attachment height of the light-shielding film 23 corresponds to the solvent height. In this embodiment, the light-shielding film 23 is located inside the open outer bottle 10.

[0051] The bubbler 30 includes a bubbling pressure vessel 32 and a container valve 31.

[0052] The bubbling pressure vessel 32 contains a predetermined gas, namely nitrogen, and is located at the bottom of the inner cavity of the preparation inner bottle 20 and at the bottom of the inner bottle body 22. The bubbling pressure vessel 32 has a container mouth (not marked in the drawing) located in the predetermined solvent B.

[0053] The container valve 31 is located outside the preparation inner bottle 20. The container valve 31 is communicated with the container mouth through the connecting pipeline C, and the container valve 31 is used to control the bubbling of the bubbling pressure vessel 32 into the predetermined solvent B through the container mouth by controlling the opening or closing of the container mouth.

[0054] The process of the dansyl chloride derivatizing agent solution preparation reagent bottle assembly 100 in this embodiment implementing the dansyl chloride derivatizing agent solution dissolution method S100 is as follows.

[0055] First, the inner bottle body 22 pre-filled with acetone is capped by the inner bottle cap 21, and after the air outlet channel 211 is sealed by the channel sealing small cap 212, the inner bottle body 22 is placed in the predetermined ice water A in the open outer bottle 10.

[0056] Then, when the temperature range of the acetone in the light-shielded preparation inner bottle is 0°C - 10°C and becomes the initial solvent, the container valve 31 is operated to make the bubbling pressure vessel 32 bubble the initial solvent, and at the same time, the air outlet channel 211 is opened through the channel sealing small cap 212. When it reaches 10 to 12.5 minutes, more than 99.5% of the oxygen in the initial solvent is replaced, and the replaced oxygen and the residual oxygen in the inner cavity space of the preparation inner bottle 20 are discharged to the outside through the air outlet channel 211. At this time, the replaced initial solvent forms an intermediate solvent.

[0057] Next, the air outlet channel 211 is sealed again through the channel sealing small cap 212, and the liquid level observation window 221 is removed from the surface of the inner bottle body 22. Sodium borohydride, that is, a predetermined antioxidant, is added to the intermediate solvent at a rate of 0.2 - 0.5 g per liter of the predetermined solvent B. After the addition is completed, the liquid level observation window 221 is reinstalled, and the air outlet channel 211 is opened again through the channel sealing small cap 212. The container valve 31 is operated to make the bubbling pressure vessel 32 bubble the predetermined solvent B, so that the predetermined antioxidant in the intermediate solvent is dissolved more quickly. When it reaches 5 to 6 minutes, more than 90% of the residual oxygen in the intermediate solvent is reduced, and the reduced oxygen and the residual oxygen in the inner cavity space of the preparation inner bottle 20 are discharged to the outside through the air outlet channel 211. At this time, the reduced intermediate solvent forms a final solvent.

[0058] Finally, the dansyl chloride derivatizing agent solution is added to the predetermined solvent B through the air outlet channel 211, and then the air outlet channel 211 is sealed through the channel sealing small cap 212. At this time, the final solvent dissolves the dansyl chloride derivatizing agent solution.

[0059] The above embodiments are preferred examples of the present invention and are not intended to limit the protection scope of the present invention. Various modifications or variations that can be made by those of ordinary skill in the art without creative efforts within the scope of the appended claims still fall within the protection scope of this patent.

Claims

1. A method for dissolving dansyl chloride derivative solution, using acetone at a predetermined temperature as a predetermined solvent, It is characterized in that comprising the following steps: Step S1: Place the predetermined solvent in a light-shielded environment to obtain an initial solvent; Step S2: Replace the oxygen in the initial solvent with a predetermined gas to obtain an intermediate solvent; Step S3: Add a predetermined antioxidant to the intermediate solvent for reduction to obtain a final solvent; Step S4: Dissolve the dansyl chloride derivative solution with the final solvent, wherein the predetermined temperature range is 0°C to 10°C, and the predetermined gas is nitrogen.

2. The method for dissolving dansyl chloride derivative solution according to claim 1, wherein: Among them, In step S2, more than 99.5% of the oxygen in the initial solvent is replaced by the predetermined gas.

3. The method for dissolving dansyl chloride derivative solution according to claim 1, wherein: Among them, In step S2, the replacement method is bubbling for 10 to 12.5 minutes.

4. The method for dissolving dansyl chloride derivative solution according to claim 1, wherein: Among them, In step S3, the predetermined antioxidant is sodium borohydride, and 0.2 - 0.5 g of the predetermined antioxidant is added per liter of the intermediate solvent.

5. The method for dissolving dansyl chloride derivative solution according to claim 1, wherein: Among them, In step S3, more than 90% of the oxygen in the intermediate solvent is reduced by the predetermined antioxidant.

6. The method for dissolving dansyl chloride derivative solution according to claim 5, wherein: Among them, In step S3, the predetermined gas assists the reduction process by bubbling through the intermediate solvent for 5 to 6 minutes.

7. The method for dissolving dansyl chloride derivative solution according to claim 3, wherein: The method for dissolving dansyl chloride derivative solution is implemented by a reagent bottle assembly for preparing dansyl chloride derivative solution, and the reagent bottle assembly for preparing dansyl chloride derivative solution includes: An open outer bottle containing predetermined ice water; A preparation inner bottle containing the predetermined solvent, and a part of the preparation inner bottle is arranged in the predetermined ice water; and A bubbler, including a bubbling pressure vessel and a container valve, the bubbling pressure vessel contains the predetermined gas, wherein the bubbling pressure vessel is located at the bottom of the inner cavity of the preparation inner bottle, and the container valve is located outside the preparation inner bottle and the container valve is used to control the bubbling pressure vessel to bubble into the predetermined solvent.

8. The method for dissolving dansyl chloride derivative solution according to claim 7, wherein: Among them, The height of the liquid level of the predetermined solvent relative to the bottom of the preparation inner bottle is within 2 / 3 of the height of the preparation inner bottle and is used as the solvent height, The surface of the preparation inner bottle has a removably arranged liquid level observation window, and the height range of the liquid level observation window relative to the bottom of the preparation inner bottle is 4 / 5 to 5 / 6 of the height of the preparation inner bottle.

9. The method for dissolving dansyl chloride derivative solution according to claim 8, wherein: Among them, The outer surface of the preparation inner bottle corresponding to the solvent height is fully pasted with a light-shielding film.

Citation Information

Patent Citations

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    CN105842379A

  • Constant temperature anaerobic reactor

    CN203275260U

  • Reagent bottle assembly for preparing dansyl chloride derivative solution

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