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Preparation method of copper-baicalin complex, cobalt-baicalin complex and nickel-baicalin complex

A technology for baicalin and complexes, which is applied in the field of preparation of copper-cobalt-nickel-baicalin complexes, can solve the problems of many by-products, unstable baicalin, long precipitation time and the like, achieves high yield and purity, and accelerates precipitation. The effect of speed and broad application prospects

Inactive Publication Date: 2019-07-12
WUHAN POLYTECHNIC UNIVERSITY
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Problems solved by technology

This type of synthetic method has the following problems: baicalin is unstable in alkaline solution, and its structure is prone to deterioration, resulting in more by-products in the product, and the binding effect with transition metal ions is poor, and the yield is low; Metal ions are prone to precipitate in alkaline solution, resulting in reduced product purity; in addition, when transition metal and baicalin are mixed, it is easy to form a precipitated suspension, which is not easy to precipitate, resulting in too long precipitation time, so that the yield of the complex product is relatively low. Low

Method used

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  • Preparation method of copper-baicalin complex, cobalt-baicalin complex and nickel-baicalin complex
  • Preparation method of copper-baicalin complex, cobalt-baicalin complex and nickel-baicalin complex

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preparation example Construction

[0020] like figure 1 Shown, the present invention provides the preparation method of copper-cobalt-nickel transition metal-baicalin complex, it comprises the following steps:

[0021] S1. Preparation of copper (cobalt, or nickel) ion precursor: take copper salt compound such as Cu (Ac) 2 , CuCl 2 、CuSO 4 , Cu(NO 3 ) 2 , or cobalt salt compounds such as Co (Ac) 2 、CoCl 2 、CoSO 4 , Co(NO 3 ) 2 , or nickel salt compounds such as Ni (Ac) 2 、NiCl 2 、NiSO 4 , Ni(NO 3 ) 2 Dissolve in 0.2-0.9% sodium alginate aqueous solution to prepare transition metal ion precursor solution.

[0022] S2. Preparation of triethylamine aqueous solution of baicalin: taking baicalin powder and dissolving it in 4-12% triethylamine aqueous solution to obtain a triethylamine-containing baicalin solution with a pH value of 7.1-8.2.

[0023] S3. Slowly add the transition metal ion precursor solution obtained in S1 into the triethylamine aqueous solution of baicalin obtained in S2 under magneti...

Embodiment 1

[0026] Take baicalin powder and dissolve it with 100mL of 4% triethylamine aqueous solution to make 6.7mmol of baicalin solution, the pH value of this solution is 7.1; 8.04mmol copper acetate solution (containing 0.2% sodium alginate), the precipitate was obtained; continue to stir at room temperature for 2 hours, then let stand for 60 minutes, then filter, wash with 3% triethylamine aqueous solution for several times, and then distilled water Wash 5 times, and finally wash several times with 95% ethanol, and dry under vacuum at 70°C to obtain the copper-baicalin complex precipitation product.

[0027] The content of trace copper in the product was measured by atomic absorption spectrometry, and the yield and purity were calculated; the yield of the product was determined to be 98.72%, and the purity was 99.25%.

Embodiment 2

[0029] Take baicalin powder and dissolve it with 100mL of 12% triethylamine aqueous solution to make 6.7mmol of baicalin solution. The pH value of this solution is 8.2; 10.72 mmol copper sulfate solution (containing 0.9% sodium alginate), the precipitate was obtained; continue to stir at room temperature for 3 h, then let stand for 30 min, filter, wash with 6% triethylamine aqueous solution for several times, and then wash with distilled water 5 times, and finally washed several times with 95% ethanol, and dried under vacuum at 50°C to obtain the copper-baicalin complex precipitation product.

[0030] The content of trace copper in the product was measured by atomic absorption spectrometry, and the yield and purity were calculated; the yield of the product was determined to be 99.03%, and the purity was 99.14%.

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Abstract

The invention provides a preparation method of a copper-baicalin complex, cobalt-baicalin complex and nickel-baicalin complex. The method comprises the following steps of dissolving a copper salt compound or a cobalt salt compound or a nickel salt compound in an aqueous solution of sodium alginate to prepare a transition metal ion precursor solution; dissolving baicalin in a 4-12% of triethylaminesolution to obtain a baicalin solution; under magnetic stirring, dropwise adding the transition metal ion precursor solution into the triethylamine aqueous solution containing baicalin for a coordination reaction to obtain a mixed precipitate solution; continuously stirring the mixed precipitate solution until the reaction is completed, and then carrying out standing for a period of time, carrying out suction filtration and drying a precipitate to obtain finished products of the copper-baicalin complex, cobalt-baicalin complex and nickel-baicalin complex separately. The reaction time is short, the process is simple, the products are easily obtained, the yield and the purity are high, properties are stable, the products are easy to preserve, and the method has a broad application prospectin medicine and animal breeding.

Description

technical field [0001] The invention relates to the field of preparation of transition metal complexes, in particular to a preparation method of a copper-cobalt-nickel-baicalin complex. Background technique [0002] Baicalin is a flavonoid-containing compound that exists in traditional Chinese medicine and has various pharmacological effects such as antibacterial, anti-inflammatory, antiviral, antihypertensive and diuretic, scavenging superoxide free radicals, and inhibiting lipase. In addition, some researchers have confirmed that baicalin has anti-inflammatory and anti-HIV-1 activities, and its anti-HIV-1 efficacy in vitro is more significant. Therefore, baicalin has become a popular research anti-AIDS drug. In recent years, some people often chelate some pharmacologically active metal ions (such as zinc, copper, cobalt, iron, aluminum, manganese, etc.) The purpose of pharmacological activity. [0003] The synthesis of existing transition metal-baicalin complexes usually...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/00
CPCC07H1/00C07H17/07
Inventor 程先忠王洋邱银生刘玉兰
Owner WUHAN POLYTECHNIC UNIVERSITY
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