Synthesis method of radial core-shell filler

Abstract

The synthesis method of the radial core-shell filler comprises a preparation step of a solid core, a synthesis step of a radioactive shell layer and a C18 stationary phase bonding step, and is characterized in that the preparation step of the solid core, the synthesis step of the radioactive shell layer, the C18 stationary phase bonding step and the end-capping step are carried out in sequence. The filler has the beneficial effects that the specific surface area of the filler is increased, selective separation of different substances can be realized by changing the chemical composition and physical properties of the filler in the design of the shell layer, various separation mechanisms can be integrated, and the separation efficiency and selectivity are improved.

Description

Technical Field

[0001] This invention relates to the field of liquid chromatography packing materials, and in particular to a method for synthesizing a radial core-shell packing material. Background Technology

[0002] Liquid chromatography (LC) has wide applications in numerous fields such as chemical analysis, biopharmaceuticals, and environmental monitoring. Traditional LC packing materials have some limitations, such as insufficient separation efficiency and limited selectivity. Radial core-shell structured packing materials offer unique advantages; their special structure provides faster mass transfer rates and better separation performance, meeting the needs of modern complex sample analysis. However, current synthetic techniques still require improvement and refinement to achieve the synthesis of more efficient and stable radial core-shell LC packing materials.

[0003] Liquid chromatography (LC), as a powerful separation and analysis technique, occupies a vital position in many fields such as modern chemistry, biology, medicine, and environmental science. It can separate and quantify various components in complex mixtures, making it one of the key methods for studying and detecting the composition of substances.

[0004] In the pharmaceutical industry, liquid chromatography (LC) is used for drug purity testing, impurity analysis, and the study of drug metabolites. For example, in the development of new drugs, it is necessary to accurately analyze various impurities in the drug to ensure its safety and efficacy. LC can separate the active ingredients from trace impurities in a drug and accurately determine their content.

[0005] In the field of biochemistry, liquid chromatography can be used for the separation and purification of biological macromolecules such as proteins and nucleic acids. For example, high-performance liquid chromatography (HPLC) can separate complex protein mixtures based on differences in their molecular weight, charge, hydrophobic properties, etc., providing strong support for proteomics research.

[0006] In environmental monitoring: Liquid chromatography is used to detect pollutants in water, soil, and air, such as organic pesticides, polycyclic aromatic hydrocarbons, and phenolic compounds. It can detect trace amounts of pollutants in environmental samples with high sensitivity, providing data support for environmental protection and pollution control.

[0007] Traditional liquid chromatography packing materials, such as fully porous spherical packing materials, can achieve separation of mixtures to a certain extent, but they suffer from slow mass transfer rates. During separation, sample molecules diffuse slowly within the pores of the packing material, resulting in significant peak broadening. This limits separation efficiency and makes the separation of complex mixtures less than ideal. Especially when analyzing biomolecules or complex organic compound mixtures, satisfactory separation results are often required after a long analysis time.

[0008] Traditional packing materials have relatively limited surface properties, relying mainly on a few mechanisms such as hydrophobic interactions or ion exchange for separation. For analytes with unique structures or properties, traditional packing materials may not provide sufficient selectivity. For example, for structurally similar isomers or complex compounds with multiple functional groups, effective separation is difficult to achieve solely through the hydrophobic or ion exchange interactions of traditional packing materials.

[0009] Column pressure problem: As liquid chromatography (LC) advances towards higher efficiency and speed, smaller particle sizes are often required to improve separation efficiency. However, reducing the particle size of traditional packing materials leads to a sharp increase in column pressure. This not only places higher demands on the pressure resistance of LC instruments, but excessively high column pressure can also cause compaction and deformation of the packing material, further affecting separation performance and the lifespan of the packing material. Summary of the Invention

[0010] The purpose of this invention is to solve the above-mentioned problems by designing a method for synthesizing radial core-shell packing materials. First, a solid core with uniform particle size is synthesized. Then, a radial shell is generated on the core, followed by multiple tail-sealing processes involving the bonding of C18 functional groups. The specific design scheme is as follows: A method for synthesizing a radial core-shell packing material includes a solid core preparation step, a radioactive shell synthesis step, and a C... 18 The fixed phase bonding step, the solid core preparation step, the radioactive shell synthesis step, and C 18 The fixed-phase bonding step and the sealing step are performed sequentially. The preparation steps of the solid core include a sol-gel mother liquor preparation step and a mixing step with tetraethyl orthosilicate (C2H5O)4Si. The synthesis steps of the radioactive core-shell include a reaction solution preparation step, a core-shell preparation step, and a cleaning and sintering step. The C 18 In the stationary phase bonding step, the silica gel surface is first hydroxylated, and then the C-terminated silica gel is bonded. 18 The stationary phase is bonded, and finally, the end is sealed.

[0011] The SOL mother liquor comprises C2H5OH, NH3H2O, and H2O, wherein the volume fractions of C2H5OH, NH3H2O, and H2O range as follows: 14-16 parts of C2H5OH, 1-2 parts of NH3H2O, and 4-5 parts of H2O.

[0012] In the mixing step, the following steps are performed sequentially: The SOL mother liquor and (C2H5O)4Si are mixed once. The volume ratio of SOL mother liquor to (C2H5O)4Si is 20-25 parts SOL mother liquor and 1-2 parts (C2H5O)4Si. Stirring is required during the mixing process and the stirring time is at least 2 hours. Continue to add SOL mother liquor and (C2H5O)4Si for secondary mixing. The volume ratio of SOL mother liquor to (C2H5O)4Si is: 140-150 parts of SOL mother liquor and 11-14 parts of (C2H5O)4Si. Stirring is required during the mixing process, and the stirring time is at least 2 hours. Continue adding SOL mother liquor and (C2H5O)4Si for three mixing cycles. The volume ratio of SOL mother liquor to (C2H5O)4Si should be 430-450 parts and 45-55 parts respectively. Stirring is required during the mixing process for at least 2 hours. If the amount of SOL mother liquor added after three mixing cycles is still insufficient, you can continue to add and stir according to the amount required. After three mixing cycles, stop stirring, allow to settle naturally, pour off the solution, and retain the settled particles at the bottom. After dissolving and dispersing the particles in deionized water, centrifuge them and then wash them. The washing process includes washing with deionized water and anhydrous ethanol multiple times. The cleaned particles are dried and crushed to obtain dry, neutral solid cores, which are SiO2 core particles.

[0013] The reaction solution preparation step includes preparing solution A and solution B, wherein solution A is a mixture of a solid core and H2O, and solution B is an aqueous solution of hexadecyltrimethylammonium bromide (CTAB) and carbamide (CH4N2O). The mass fractions of CTAB and CH4N2O range from 11 to 13 parts CHBrN to 3 to 4 parts CH4N2O. Solution B can be dissolved by heating.

[0014] In the core-shell preparation step, the solid core in solution A is ultrasonically dispersed to ensure complete and uniform ultrasonic dispersion. Then, solution A is poured into solution B and stirred for at least 15 minutes. The stirring speed is then reduced, and cyclohexane and isopropanol are added. Stirring continues for at least 5 minutes. Then, (C2H5O)4Si is added and magnetic stirring is performed for at least 30 minutes. The volume fraction ratio of each component is solution A: solution B: cyclohexane: isopropanol: (C2H5O)4Si = 120 parts: 240 parts: 260 parts: 10.8 parts: 8 parts. The mixture is placed in a hydrothermal reactor for reaction. The optimal reaction temperature is 120℃ and the optimal reaction time is 4 hours to obtain the core-shell solution.

[0015] In the cleaning and sintering steps, the core-shell solution is first centrifuged, then cleaned with anhydrous ethanol, and subsequently dried and calcined to obtain silica gel. The optimal centrifugation speed is 3000 rpm, the centrifugation time is no less than 5 min, the number of times anhydrous ethanol is used for cleaning is multiple times, the optimal drying temperature is 60℃, the drying time is no less than 3 h, the optimal calcination temperature is 550℃, the optimal calcination time is 4 h, and the optimal heating rate is 1℃ / min.

[0016] During the hydroxylation process of silica gel, the hydrochloric acid aqueous solution is stirred at room temperature for at least 10 minutes, then silica gel is added and mixed, and then refluxed in an oil bath. The optimal temperature is 150℃ and the optimal time is 7 hours to obtain hydroxylated silica gel particles. These particles are then cooled, centrifuged, washed, and dried in sequence. During the washing process of the hydroxylated silica gel particles, they are first washed with deionized water until neutral, and then washed multiple times with methanol. The hydrochloric acid acidification is 10% hydrochloric acid, with 1 g of core-shell corresponding to 15-25 mL of hydrochloric acid.

[0017] The C 18 Following the stationary phase bonding step, hydroxylated silica gel particles were ultrasonically dispersed in anhydrous toluene. A mixed solution of octadecyldimethylchlorosilane and anhydrous toluene was then added, followed by reflux under a nitrogen atmosphere. The optimal nitrogen atmosphere temperature was 110°C, and the reflux reaction time was no less than 8 hours, yielding bonded silica gel particles. Finally, the bonded silica gel particles were sequentially washed and dried. During the washing process, the particles were washed multiple times with isopropanol, methanol, and ethanol, respectively. The optimal bonding method was as follows: 3 g of SiO2 particles were ultrasonically dispersed in 100 mL of anhydrous toluene, and a mixed solution of 3 mL of C18 and 5 mL of toluene was added. The reaction was carried out at 112°C for 12 hours under nitrogen protection. After cooling, the particles were washed sequentially with isopropanol, methanol, and ethanol, and then dried at 60°C for 6 hours.

[0018] During the sealing process, bonded silica particles are incorporated into anhydrous toluene, and trimethylchlorosilane is added. The mixture is then refluxed under a nitrogen atmosphere, with the optimal nitrogen atmosphere temperature being 110°C and the reflux reaction time being no less than 4 hours. Finally, the mixture is washed multiple times with toluene, methanol, and ethanol, and then dried to obtain a single-sealed C14. 18 filler.

[0019] The first sealing is C 18 The filler was refluxed with trimethylchlorosilane again under a nitrogen atmosphere to obtain C20 with secondary tailing. 18 The packing material is repeatedly sealed, and then cleaned and dried to obtain a radial core-shell packing material.

[0020] The radial core-shell packing material has a solid core diameter of 1-3 μm, a surface shell thickness of 100-500 nm, a surface pore size of 8-30 nm, a carbon content of 2-10%, and a column efficiency greater than 60,000 N / m.

[0021] The method for synthesizing radial core-shell packing material obtained by the above-described technical solution of the present invention has the following advantages: The specific surface area of ​​the packing material is increased, and the selective separation of different substances can be achieved by changing the chemical composition and physical properties of the shell layer. Multiple separation mechanisms can be combined to improve separation efficiency and selectivity. Attached Figure Description

[0022] Figure 1 This is a schematic diagram illustrating the principle of hydroxylation of the silicone surface described in this invention; Figure 2 It is the C described in this invention. 18 A schematic diagram illustrating the principle of fixed-phase bonding; Figure 3 This is a schematic diagram illustrating the principle of the sealing step described in this invention; Figure 4 This is an evaluation diagram of the radial core-shell packing material after being packed into a column according to the present invention; Figure 5 This is an evaluation data graph after the radial core-shell packing material of the present invention has been loaded into a column; Figure 6 This is a particle size distribution diagram of the 2µm solid core described in this invention; Figure 7 This is a BET detection image of the radial core-shell structure described in this invention; Figure 8 This is a TEM image of the radial core-shell structure described in this invention; Figure 9 The radial core-shell packing material C described in this invention 18 Infrared chromatogram of the bonded sample; Figure 10 The radial core-shell packing material C described in this invention 18 Graph of elemental analysis of bonded bonds; Detailed Implementation

[0023] The present invention will now be described in detail with reference to the accompanying drawings.

[0024] A method for synthesizing a radial core-shell packing material includes a solid core preparation step, a radioactive shell synthesis step, and a C... 18 The fixed phase bonding step, the solid core preparation step, the radioactive shell synthesis step, and C 18 The fixed-phase bonding step and the sealing step are performed sequentially. The preparation steps of the solid core include a sol-gel mother liquor preparation step and a mixing step with tetraethyl orthosilicate (C2H5O)4Si. The synthesis steps of the radioactive core-shell include a reaction solution preparation step, a core-shell preparation step, and a cleaning and sintering step. The C 18 In the stationary phase bonding step, the silica gel surface is first hydroxylated, and then the C-terminated silica gel is bonded. 18 The stationary phase is bonded, and finally, the end is sealed.

[0025] The SOL mother liquor comprises C2H5OH, NH3H2O, and H2O, wherein the volume fractions of C2H5OH, NH3H2O, and H2O range as follows: 14-16 parts of C2H5OH, 1-2 parts of NH3H2O, and 4-5 parts of H2O.

[0026] In the mixing step, the following steps are performed sequentially: The SOL mother liquor and (C2H5O)4Si are mixed once. The volume ratio of SOL mother liquor to (C2H5O)4Si is 20-25 parts SOL mother liquor and 1-2 parts (C2H5O)4Si. Stirring is required during the mixing process and the stirring time is at least 2 hours. Continue to add SOL mother liquor and (C2H5O)4Si for secondary mixing. The volume ratio of SOL mother liquor to (C2H5O)4Si is: 140-150 parts of SOL mother liquor and 11-14 parts of (C2H5O)4Si. Stirring is required during the mixing process, and the stirring time is at least 2 hours. Continue adding SOL mother liquor and (C2H5O)4Si for three mixing cycles. The volume ratio of SOL mother liquor to (C2H5O)4Si should be 430-450 parts and 45-55 parts respectively. Stirring is required during the mixing process for at least 2 hours. If the amount of SOL mother liquor added after three mixing cycles is still insufficient, you can continue to add and stir according to the amount required. After three mixing cycles, stop stirring, allow to settle naturally, pour off the solution, and retain the settled particles at the bottom. After dissolving and dispersing the particles in deionized water, centrifuge them and then wash them. The washing process includes washing with deionized water and anhydrous ethanol multiple times. The cleaned particles are dried and crushed to obtain dry, neutral solid cores, which are SiO2 core particles.

[0027] The reaction solution preparation step includes preparing solution A and solution B, wherein solution A is a mixture of a solid core and H2O, and solution B is an aqueous solution of hexadecyltrimethylammonium bromide (CTAB) and carbamide (CH4N2O). The mass fractions of CTAB and CH4N2O range from 11 to 13 parts CHBrN to 3 to 4 parts CH4N2O. Solution B can be dissolved by heating.

[0028] In the core-shell preparation step, the solid core in solution A is ultrasonically dispersed to ensure complete and uniform ultrasonic dispersion. Then, solution A is poured into solution B and stirred for at least 15 minutes. The stirring speed is then reduced, and cyclohexane and isopropanol are added. Stirring continues for at least 5 minutes. Then, (C2H5O)4Si is added and magnetic stirring is performed for at least 30 minutes. The volume fraction ratio of each component is solution A: solution B: cyclohexane: isopropanol: (C2H5O)4Si = 120 parts: 240 parts: 260 parts: 10.8 parts: 8 parts. The mixture is placed in a hydrothermal reactor for reaction. The optimal reaction temperature is 120℃ and the optimal reaction time is 4 hours to obtain the core-shell solution.

[0029] In the cleaning and sintering steps, the core-shell solution is first centrifuged, then cleaned with anhydrous ethanol, and subsequently dried and calcined to obtain silica gel. The optimal centrifugation speed is 3000 rpm, the centrifugation time is no less than 5 min, the number of times anhydrous ethanol is used for cleaning is multiple times, the optimal drying temperature is 60℃, the drying time is no less than 3 h, the optimal calcination temperature is 550℃, the optimal calcination time is 4 h, and the optimal heating rate is 1℃ / min.

[0030] During the hydroxylation process of silica gel, the hydrochloric acid aqueous solution is stirred at room temperature for at least 10 minutes, then silica gel is added and mixed, and then refluxed in an oil bath. The optimal temperature is 150℃ and the optimal time is 7 hours to obtain hydroxylated silica gel particles. These particles are then cooled, centrifuged, washed, and dried in sequence. During the washing process of the hydroxylated silica gel particles, they are first washed with deionized water until neutral, and then washed multiple times with methanol. The hydrochloric acid acidification is 10% hydrochloric acid, with 1 g of core-shell corresponding to 15-25 mL of hydrochloric acid.

[0031] The C 18Following the stationary phase bonding step, hydroxylated silica gel particles were ultrasonically dispersed in anhydrous toluene. A mixed solution of octadecyldimethylchlorosilane and anhydrous toluene was then added, followed by reflux under a nitrogen atmosphere. The optimal nitrogen atmosphere temperature was 110°C, and the reflux reaction time was no less than 8 hours, yielding bonded silica gel particles. Finally, the bonded silica gel particles were sequentially washed and dried. During the washing process, the particles were washed multiple times with isopropanol, methanol, and ethanol, respectively. The optimal bonding method was as follows: 3 g of SiO2 particles were ultrasonically dispersed in 100 mL of anhydrous toluene, and a mixed solution of 3 mL of C18 and 5 mL of toluene was added. The reaction was carried out at 112°C for 12 hours under nitrogen protection. After cooling, the particles were washed sequentially with isopropanol, methanol, and ethanol, and then dried at 60°C for 6 hours.

[0032] During the sealing process, bonded silica particles are incorporated into anhydrous toluene, and trimethylchlorosilane is added. The mixture is then refluxed under a nitrogen atmosphere, with the optimal nitrogen atmosphere temperature being 110°C and the reflux reaction time being no less than 4 hours. Finally, the mixture is washed multiple times with toluene, methanol, and ethanol, and then dried to obtain a single-sealed C14. 18 filler.

[0033] The first sealing is C 18 The filler was refluxed with trimethylchlorosilane again under a nitrogen atmosphere to obtain C20 with secondary tailing. 18 The packing material is repeatedly sealed, and then cleaned and dried to obtain a radial core-shell packing material.

[0034] The radial core-shell packing material has a solid core diameter of 1-3 μm, a surface shell thickness of 100-500 nm, a surface pore size of 8-30 nm, a carbon content of 2-10%, and a column efficiency greater than 60,000 N / m.

[0035] Prepare the SOL stock solution (A): C2H5OH / NH3H2O / H2O = 15.03 / 1.485 / 4.455 (volume ratio). Pipette 21 mL of SOL into a 100 mL round-bottom flask and stir rapidly until homogeneous. Add 1.53 mL of (C2H5O)4Si and continue stirring for 2 hours. After 2 hours, transfer the reaction solution from the 100 mL round-bottom flask to a 500 mL volumetric flask using a glass funnel. Add 147 mL of SOL while stirring, followed by 12.25 mL of (C2H5O)4Si, and continue stirring for 2 hours. After 2 hours, transfer the reaction solution from the 500 mL round-bottom flask to a 1000 mL round-bottom flask and add 440 mL of SOL while stirring. Stir for 30 minutes, then add 49 mL of (C2H5O)4Si (stirring for 30 minutes helps the diluent mix thoroughly, resulting in more uniform particle growth). Continue stirring for 12 hours. After 12 hours, add 30 mL of (C2H5O)4Si and continue stirring for 2 hours. Stop stirring and allow the particles to settle naturally until compacted. Pour off the solution, keeping only the settled particles at the bottom. Dissolve and disperse the particles in deionized water, then centrifuge. Wash once with deionized water and twice with anhydrous ethanol. First, dry the particles in a 60°C oven, then gently crush them with a glass rod. Finally, dry them at 160°C for 5 hours until the final particles are neutral.

[0036] Preparation of reaction solution: Solution A: 12g nuclear particles (H) + 240mL H2O Solution B: 12g CHBrN + 3.6g CH4N2O + 120mL H2O, dissolved by heating at 40℃.

[0037] Core-shell preparation: After the SiO2 core particles in reaction solution A are completely and uniformly dispersed by ultrasonication, A is poured into B and stirred for 15 min. The stirring speed is reduced, and then 360 mL of cyclohexane and 10.8 mL of isopropanol are added. Stirring is continued for 5 min, and then 8 mL of (C2H5O)4Si is added. The mixture is magnetically stirred for 30 min and then placed in a hydrothermal reactor. The reaction is carried out at 120 °C for 4 h.

[0038] Cleaning and calcination: Centrifuge at 3000 rpm for 5 min, wash 3 times with anhydrous ethanol, dry at 60℃ for 3 h, and finally calcine at 550℃ for 4 h (heating rate 1℃ / min).

[0039] Example 3C 18 Synthesis of bonded phases.

[0040] Silica surface hydroxylation: Add a certain proportion of hydrochloric acid aqueous solution to a round-bottom flask, stir at room temperature for 10 minutes, add a certain amount of silica gel, reflux in an oil bath at 150°C for 7 hours, after which place it in a water bath to cool, centrifuge, wash with deionized water until neutral, wash three times with methanol, and dry at 70°C overnight.

[0041] C 18 Fixed phase bonding: Surface-hydroxylated silica particles were ultrasonically dispersed in a certain amount of anhydrous toluene, and a mixed solution of octadecyl dimethylchlorosilane and anhydrous toluene was added. The mixture was refluxed at 110°C under a nitrogen atmosphere for 8 hours, washed three times each with isopropanol, methanol, and ethanol, and then dried.

[0042] Sealing steps: The bonded particles were dissolved in a certain amount of anhydrous toluene, and a certain amount of trimethylchlorosilane was added. The mixture was refluxed at 110°C under a nitrogen atmosphere for 4 hours. The particles were washed three times each with toluene, methanol, and ethanol, and then dried.

[0043] Second closing: The filler material after the first sealing was reacted again with trimethylchlorosilane to obtain C20 with a second sealing. 18 filler.

[0044] The radial core-shell packing material and column efficiency obtained in Examples 1-3 are as follows: Figure 4-10 As shown, radial core-shell packing materials exhibit a radially growing shell structure radiating outwards from the central core. This structure significantly increases the contact area between the packing material and sample molecules, while also providing more possibilities for designing various separation functions. By introducing different functional groups or functional materials into the shell, specific interactions with different types of analytes can be achieved, thereby improving selectivity. Moreover, the radial structure is beneficial for improving mass transfer rates and reducing peak broadening, showing great potential for improving separation efficiency. Currently, the synthesis technology of radial core-shell liquid chromatography packing materials is still in the stage of continuous development and improvement, and related research is of great significance for promoting the advancement of liquid chromatography technology.

[0045] The above technical solutions only embody the preferred technical solutions of the present invention. Any modifications that may be made by those skilled in the art to certain parts thereof embody the principles of the present invention and fall within the protection scope of the present invention.

Claims

1. A method for synthesizing a radial core-shell packing material, comprising a solid core preparation step, a radioactive shell synthesis step, and a C... 18 The fixed phase bonding step is characterized by, The preparation steps of the solid core, the synthesis steps of the radioactive shell, and C 18 The stationary phase bonding step and the tailing step are performed sequentially. The solid core preparation step includes a SOL mother liquor preparation step and a mixing step with (C2H5O)4Si. The radioactive core-shell synthesis step includes a reaction solution preparation step, a core-shell preparation step, and a cleaning and sintering step. 18 In the bonding step, the silicone surface is first hydroxylated, and then the C-polymerization is completed. 18 The stationary phase is bonded, and finally, the end is sealed.

2. The method for synthesizing radial core-shell packing material according to claim 1, characterized in that, The SOL mother liquor includes C2H5OH, NH3H2O, and H2O.

3. The method for synthesizing radial core-shell packing material according to claim 1, characterized in that, In the mixing step, the following steps are performed sequentially: The SOL mother liquor was mixed with (C2H5O)4Si once; Continue adding SOL mother liquor and (C2H5O)4Si for secondary mixing; Continue adding SOL mother liquor and mixing (C2H5O)4Si three times; Allow the particles to settle naturally, then pour out the solution and retain the particles that have settled at the bottom. After dissolving and dispersing the particles in deionized water, centrifuge and then wash them. The cleaned particles are dried and crushed to obtain dry, neutral solid cores, which are SiO2 core particles.

4. The method for synthesizing radial core-shell packing material according to claim 1, characterized in that, The reaction solution preparation step includes preparing solution A and solution B, wherein solution A is a mixture of a solid core and H2O.

5. The method for synthesizing radial core-shell packing material according to claim 1, characterized in that, In the core-shell preparation step, after ultrasonically dispersing the solid core in solution A, solution A is poured into solution B and stirred. Then, cyclohexane and isopropanol are added and stirred continuously. Then, (C2H5O)4Si is added and magnetically stirred. The mixture is placed in a hydrothermal reactor for reaction. The optimal reaction temperature is 120℃ and the optimal reaction time is 4h to obtain the core-shell solution.

6. The method for synthesizing radial core-shell packing material according to claim 1, characterized in that, In the cleaning and sintering steps, the core-shell solution is first centrifuged, then cleaned with anhydrous ethanol, and then dried and calcined to obtain silica gel.

7. The method for synthesizing radial core-shell packing material according to claim 1, characterized in that, During the hydroxylation process of silica gel, hydrochloric acid aqueous solution is added to silica gel and mixed, followed by oil bath reflux to obtain hydroxylated silica gel particles, which are then cooled, centrifuged, washed, and dried in sequence.

8. The method for synthesizing radial core-shell packing material according to claim 1, characterized in that, The C 18 After the stationary phase bonding step, the hydroxylated silica gel particles are ultrasonically dispersed in anhydrous toluene, and then a mixed solution of octadecyl dimethylchlorosilane and anhydrous toluene is added. The mixture is then refluxed under a nitrogen atmosphere to obtain bonded silica gel particles. Finally, the bonded silica gel particles are washed and dried sequentially.

9. The method for synthesizing radial core-shell packing material according to claim 1, characterized in that, During the sealing process, bonded silica particles are incorporated into anhydrous toluene, and trimethylchlorosilane is added. The mixture is then refluxed under a nitrogen atmosphere, followed by washing and drying to obtain C10 with a single sealing step. 18 filler.

10. The method for synthesizing radial core-shell packing material according to claim 9, characterized in that, The first sealing is C 18 The filler was refluxed with trimethylchlorosilane again under a nitrogen atmosphere to obtain C20 with secondary tailing. 18 The packing material is repeatedly sealed, and then cleaned and dried to obtain a radial core-shell packing material.

11. The method for synthesizing radial core-shell packing material according to claim 10, characterized in that, The radial core-shell packing material has a solid core diameter of 1-3 μm, a surface shell thickness of 100-500 nm, a surface pore size of 8-30 nm, a carbon content of 2-10%, and a column efficiency greater than 60,000 N / m.

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