a kind of sio 2 / Urushiol ester polymer microspheres, preparation method and its application in the separation of gastrodin and its derivatives

A technology of polymer microspheres and urushiol ester, applied in the field of high-performance liquid chromatography, can solve the problem of unsatisfactory separation effect of gastrodin and its derivatives, and achieve a rich pore structure, good separation effect, and uniform particle size distribution Effect

Active Publication Date: 2022-02-18
HUBEI UNIV FOR NATITIES
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0010] However, the above-mentioned existing technologies all have the problem that the separation effect of gastrodin and its derivatives is not ideal enough, so it is necessary to explore a more efficient method for separating gastrodin and its derivatives
[0011] There are no reports on the separation of gastrodin and 4-nitrophenylphenyl-β-D-glucopyranoside

Method used

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  • a kind of sio <sub>2</sub> / Urushiol ester polymer microspheres, preparation method and its application in the separation of gastrodin and its derivatives
  • a kind of sio <sub>2</sub> / Urushiol ester polymer microspheres, preparation method and its application in the separation of gastrodin and its derivatives
  • a kind of sio <sub>2</sub> / Urushiol ester polymer microspheres, preparation method and its application in the separation of gastrodin and its derivatives

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Experimental program
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Effect test

preparation Embodiment 1

[0057] 0.35g of urushiol methacrylate as a monomer, 0.75g of ethylene glycol dimethacrylate as a crosslinking agent and 3mg of azobisisobutyronitrile were thoroughly mixed, and evenly coated on the surface of 5.00g of silica gel. In this embodiment, azobisisobutyronitrile is used as an azo free radical initiator, and organic peroxide free radical initiators such as benzoyl peroxide can also be used in other embodiments. Then place 250mL of sodium lauryl sulfate in an aqueous solution with a mass fraction of 0.1% as a surfactant, carry out free radical polymerization at 90°C for 8h, then use absolute ethanol to carry out Soxhlet extraction of the product, and then vacuum-dry. SiO can be obtained 2 / Urushiol ester polymer microspheres.

[0058] The particle size distribution of microspheres was measured by laser particle size analyzer, and the specific surface area and pore structure of microspheres were measured by specific surface area and microporous mesoporous physical ads...

preparation Embodiment 2

[0060] 1.50g of urushiol methacrylate as a monomer, 3.35g of ethylene glycol dimethacrylate as a crosslinking agent and 15mg of azobisisobutyronitrile are fully mixed, evenly coated on the surface of 50.00g of silica gel, and then placed In 1000mL sodium lauryl sulfate as surfactant, the mass fraction of 1% aqueous solution was used for free radical polymerization at 75°C for 8 hours, then Soxhlet extraction was performed on the product with absolute ethanol, and then vacuum dried to obtain SiO 2 / Urushiol ester polymer microspheres.

[0061] The particle size distribution of microspheres was measured by laser particle size analyzer, and the specific surface area and pore structure of microspheres were measured by specific surface area and microporous mesoporous physical adsorption instrument. After detection and analysis, the microsphere particle size distribution is 5-10μm, the average pore size is 6.59nm, and the specific surface area is 295m 2 / g.

preparation Embodiment 3

[0063] 1.5g of urushiol methacrylate as a monomer, 6.5g of ethylene glycol dimethacrylate as a crosslinking agent and 100mg of benzoyl peroxide are fully mixed, evenly coated on the surface of 90.00g of silica gel, and then placed in The mass fraction of 1000mL sodium lauryl sulfate as surfactant is 3% aqueous solution, carry out free radical polymerization reaction at 85°C for 8h, then perform Soxhlet extraction on the product with absolute ethanol, and then vacuum dry to obtain SiO 2 / Urushiol ester polymer microspheres.

[0064] The particle size distribution of microspheres was measured by laser particle size analyzer, and the specific surface area and pore structure of microspheres were measured by specific surface area and microporous mesoporous physical adsorption instrument. After detection and analysis, the microsphere particle size distribution is 10-15μm, the average pore size is 7.23nm, and the specific surface area is 300.65m 2 / g.

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Abstract

The invention belongs to the technical field of high performance liquid chromatography, in particular to a SiO 2 / Urushiol ester polymer microspheres, preparation method and application thereof in the separation of gastrodin and its derivatives. The technical solution includes: using urushiol methacrylate as a monomer, fully mixing it with a crosslinking agent and a free radical initiator, and then coating it on the surface of silica gel; performing free radical polymerization to obtain SiO 2 / Urushiol ester polymer microspheres. SiO 2 / Urushiol ester polymer microspheres filled chromatographic column for HPLC separation of gastrodin and its derivatives. The separation degree of gastrodin and phenyl-β-D-glucopyranoside is above 9.55, the separation degree of gastrodin and 4-nitrophenyl-β-D-glucopyranoside is above 17.01, and the separation degree of p-phenyl The separation degree of ‑β‑D‑glucopyranoside and 4‑nitrophenyl‑β‑D‑glucopyranoside is above 8.25, and the present invention has higher separation degree and selectivity for gastrodin and its derivatives .

Description

technical field [0001] The invention belongs to the technical field of high performance liquid chromatography, in particular to a SiO 2 / Urushiol ester polymer microspheres, preparation method and application thereof in the separation of gastrodin and its derivatives. Background technique [0002] The chemical structural formulas of gastrodin and its derivatives phenyl-β-D-glucopyranoside and 4-nitrophenyl-β-D-glucopyranoside are respectively: [0003] Gastrodin: Phenyl-β-D-glucopyranoside: 4-Nitrophenyl-β-D-glucopyranoside: [0004] Gastrodin is the main active ingredient of Gastrodia elata, a traditional Chinese medicinal material. It has the functions of sedative and hypnotic, anticonvulsant, analgesic, antiepileptic, and nerve cell protection. Clinically, it is mostly used as an adjuvant treatment for headache, dizziness, limb numbness, convulsions in children, convulsions, convulsions and high blood pressure, with remarkable effects. Phenyl-β-D-glucopyranoside...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 史伯安曾磊曹宇李国祥雷福厚
Owner HUBEI UNIV FOR NATITIES
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