GMA-carboxymethyl-beta-cyclodextrin monomer, monolithic column and chiral drug separation method
A technology of chiral drugs and cyclodextrin, which is applied in the field of monolithic column and chiral drug separation, GMA-carboxymethyl-β-cyclodextrin monomer, can solve the problems of limited selectivity, achieve simple preparation method, Wide range of chiral drug separation spectrum, short cycle effect
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Embodiment 1
[0041] Embodiment 1 A kind of GMA-carboxymethyl-β-cyclodextrin monomer (GMA-CM-β-CD)
[0042] The GMA-carboxymethyl-β-cyclodextrin monomer is prepared from the following components:
[0043]
[0044] The preparation method comprises the following steps:
[0045] Preparation of carboxymethyl-β-cyclodextrin (CM-β-CD): Add 1g of β-cyclodextrin into a 50mL beaker, keep stirring in a water bath at 50°C, and add 1% NaOH solution dropwise; Slowly add 1% chloroacetic acid into the solution, stir the milky white suspension until it becomes clear; continue to stir for 4 hours under the condition of 60°C water bath, adjust the pH of the solution to 7 with dilute hydrochloric acid; then add ethanol to the solution until the precipitate disappears, static place; filter under reduced pressure to leave the precipitate, and place it in a constant temperature drying oven (60°C) to dry to obtain CM-β-CD. The reaction process is as follows: figure 1 shown;
[0046] Place 0.06 g of CM-β-CD,...
Embodiment 2
[0047] Example 2 Preparation method of a carboxymethyl-β-cyclodextrin organosilicon hybrid monolithic column
[0048] Described preparation method comprises the steps:
[0049] 1) Capillary activation: use sodium hydroxide (1.0M, 2h), water (10min), hydrochloric acid (1.0M, 1h), water (20min), acetone (10min) to perfuse the capillary in sequence, and dry with nitrogen gas flow;
[0050] 2) Prepare a homogeneous hydrolyzate: under ice bath conditions, continuously stir the solution containing acetic acid (0.01M, 1.0mL), polyethylene glycol (PEG, 10000mW, 108mg), methyl orthosilicate (TMOS, 375μL) and propyl A mixture of trimethoxysilane (γ-MAPS, 85 μL) was obtained for 2 hours to obtain a homogeneous hydrolyzate;
[0051] 3) Preparation of GMA-carboxymethyl-β-cyclodextrin monomer:
[0052] Place 0.06 g of CM-β-CD, 22 mg of glycidyl methacrylate (GMA), 6 mg of 8-diazabicycloundec-7-ene (DBU), and 120 μL of anhydrous DMSO into a reaction vessel, and wash with The rubber stopper ...
Embodiment 3
[0055] Embodiment 3 A kind of separation method of chiral drug
[0056] Chromatographic column: carboxymethyl-β-cyclodextrin organosilicon hybrid monolithic column;
[0057] Mobile phase: organic phase Acetonitrile (ACN): aqueous phase Tris-H 3 PO 4 (20mM)=20:80; ultrasonically degassed, and filtered with a filter membrane with a pore size of 0.22 μm;
[0058] pH: 5.5;
[0059] Detection wavelength: 220nm;
[0060] Column temperature: 45°C;
[0061] Separation voltage: 15kV.
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