Preparation method and application of zinc-baicalin complex
A technology of baicalin and complexes, which is applied in the field of preparation of zinc-baicalin complexes, can solve the problems of many by-products, instability of baicalin, and low yield, so as to reduce the generation of by-products and increase the dissociation rate of hydroxyl groups , the effect of good product purity
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[0032] In view of this, the present invention proposes a preparation method of the zinc-baicalin complex, which has simple process, easy control, high yield and good product purity. combine figure 1 The schematic flow diagram of an embodiment of the preparation method of the proposed zinc-baicalin complex, the preparation method of the zinc-baicalin complex comprises the following steps:
[0033] Step S10, dissolving the zinc compound in the trimethylamine solution to obtain a zinc ion precursor solution with a pH of 7-8.5.
[0034] Wherein, the zinc compound is Zn(Ac) 2 , ZnCl 2 , ZnSO 4 , Zn(NO 3 ) 2 and ZnC 2 o 4 Any one of them; the mass concentration of the trimethylamine solution is 0.5-1.2%; the mass fraction of zinc in the zinc ion precursor solution is 10-26%.
[0035] In this embodiment, the trimethylamine solution is a solution formed by dissolving trimethylamine in water, and the percentage of the mass of trimethylamine in the solution to the total weight o...
Embodiment 1
[0058] Weigh 2.35g (10.72mmol) Zn(Ac) 2 2H 2 O in a 100ml small beaker, add 0.5% trimethylamine aqueous solution, stir and dissolve to obtain 10%, zinc ion precursor solution of pH7.5;
[0059] Put 3.0 g (6.7 mmol) of baicalin in a 250 ml three-neck flask, add trimethylamine aqueous solution (0.8% by mass fraction), stir and dissolve to form a brownish-yellow clear liquid, and obtain a baicalin solution with a pH of 7;
[0060] The baicalin solution was placed in an ice bath, and under stirring, the zinc ion precursor solution was slowly added dropwise at a speed of 1.0ml / min into the three-neck flask containing the baicalin solution through the addition funnel, and the zinc ions and the baicalin Precipitation occurred immediately after the complex reaction of the glycosides, and after the dropwise addition was completed, stirring was continued for 60 minutes in an ice bath to obtain a mixed solution;
[0061] After the mixed solution was left to stand in an ice bath for 3 h...
Embodiment 2
[0064] Weigh 1.624g (7.4mmol) Zn(Ac) 2 2H 2 O in a 50ml small beaker, add 1.2% trimethylamine aqueous solution, stir and dissolve to obtain 10.8%, pH8.5 zinc ion precursor;
[0065] Put 3.0g (6.7mmol) of baicalin in a 250ml three-necked flask, add trimethylamine aqueous solution (2.6% by mass fraction), stir and dissolve to form a brownish-yellow clear liquid, and obtain a baicalin solution with a pH of 9;
[0066] The baicalin solution is placed in an ice bath, and under stirring, the zinc ion precursor solution is slowly added dropwise at a speed of 2.5ml / min into the three-necked bottle of the baicalin solution through the addition funnel, and the zinc ions and the baicalin Precipitation occurred immediately after the complex reaction of the glycosides, and after the dropwise addition was completed, stirring was continued for 30 minutes in an ice bath to obtain a mixed solution;
[0067] After the mixture was left to stand in an ice bath for 6 hours, the precipitate was o...
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