Unlock instant, AI-driven research and patent intelligence for your innovation.
Silica gel liquid chromatography filler for alkaloid compounds and preparation method thereof
What is Al technical title?
Al technical title is built by PatSnap Al team. It summarizes the technical point description of the patent document.
A technology of alkaloids and liquid chromatography, which is applied in the field of silica gel liquid chromatography fillers for alkaloids and its preparation, can solve problems such as chromatographic peak shape tailing and column efficiency reduction, and achieve strong chemical stability and effective Separation, the effect of good chromatographic separation performance
Active Publication Date: 2020-02-07
YANTAI UNIV
View PDF6 Cites 0 Cited by
Summary
Abstract
Description
Claims
Application Information
AI Technical Summary
This helps you quickly interpret patents by identifying the three key elements:
Problems solved by technology
Method used
Benefits of technology
Problems solved by technology
The ionization characteristics of basic compounds make them interact with the residual acidic silanol groups on the surface of the silica matrix, resulting in chromatographic peak tailing and reduced column efficiency
Method used
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more
Image
Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
Click on the blue label to locate the original text in one second.
Reading with bidirectional positioning of images and text.
Smart Image
Examples
Experimental program
Comparison scheme
Effect test
Embodiment 1
[0022] A preparation method for silica gel liquid chromatography filler for alkaloid compounds, comprising the following five steps:
[0023] Alkaline solution activation: 2 g porous silica gel microspheres (commercial product, particle size 5 microns, pore size 10 nm) were placed in a strong alkaline aqueous solution, stirred at 25°C, centrifuged, washed with deionized water until neutral , Dry at 100°C for later use;
[0025] Single coating: Add the obtained activated silica gel to the obtained precursor mixed solution, mix and stir, wash and dry after 30 min, and obtain TiO 2 -ZrO 2 / SiO 2 -1;
[0026] Repeat: Repeat the coating reaction process of the above steps once to obtain TiO 2 -ZrO 2 / SiO 2 - 2 microspheres;
[0032] A preparation method for silica gel liquid chromatography filler for alkaloid compounds, comprising the following five steps:
[0033] Alkaline solution activation: put 3 g porous silica gel microspheres (particle size 5 microns, pore size 20 nm) in a strong alkaline aqueous solution, stir at 45°C, centrifuge, wash with deionized water until neutral, and dry at 80°C reserve;
[0034] Preparation of precursor mixed solution: Dissolve 2 g of titaniumnitrate and 1 g of zirconium nitrate in 30 mL of NH with pH=3 4 In AC-HCl buffer solution, stir vigorously until completely dissolved;
[0035] Single coating: add the obtained activated silica gel to the obtained precursor mixed solution, mix and stir, wash and dry after 2 hours, and obtain TiO 2 -ZrO 2 / SiO 2 -1;
[0036] Repeat: Repeat the coating reaction process of the above steps several times to obtain TiO 2 -ZrO 2 / SiO 2 - 5 microspheres;
[0037] Heat curing: for the prepared TiO 2 -ZrO 2 / SiO 2 -5 micros...
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More
PUM
Login to View More
Abstract
The invention relates to a silica gel liquid chromatography filler for an alkaloid compound and a preparation method of the filler. The preparation method comprises the following steps of putting porous silica gel microspheres into a strong alkaline aqueous solution to prepare activated silica gel; dissolving a water solubletitanium salt and zirconium salt mixture in an acidic buffer solution with the pH value of 1-6 to prepare a precursor mixed solution; carrying out mixing and stirring on the activated silica gel and the precursor mixed solution according to a certain ratio, so as to prepare TiO2-ZrO2 / SiO2-1; repeating the coating process to prepare TiO2-ZrO2 / SiO2-n microspheres; and carrying out heating treatment on the TiO2-ZrO2 / SiO2-n microspheres at a temperature of 300-600 DEG C for 3-12h to obtain the chromatography filler. The filler disclosed by the invention has abundant acting sites and relatively strong chemical stability; and the thickness of the TiO2-ZrO2 nano-layer andthe proportion of the two metal oxides in the composite nano-layer are adjusted by controlling the concentration of Ti<4+> and Zr <4+> in the solution, so that the filler has richer acting sites andis suitable for wider pH range.
Description
technical field [0001] The invention relates to the field of liquid chromatography, in particular to a silica gel liquid chromatography filler for alkaloid compounds and a preparation method thereof. Background technique [0002] At present, there are more than 12,000 types of alkaloid compounds, accounting for more than 50% of the natural products with important pharmacological activities, and have important development potential (Liang Xinmiao et al., Journal of Analysis and Testing, 2019). There are many types of such compounds and various structural types. Therefore, the separation and purification of such compounds has always been a key scientific problem to be solved urgently. [0003] In the separation and analysis of such compounds, reversed-phase liquid chromatography is the most widely used separation mode. The ionization characteristics of basic compounds make them interact with the residual acidic silanol groups on the surface of the silica matrix, resulting in ...
Claims
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More
Application Information
Patent Timeline
Application Date:The date an application was filed.
Publication Date:The date a patent or application was officially published.
First Publication Date:The earliest publication date of a patent with the same application number.
Issue Date:Publication date of the patent grant document.
PCT Entry Date:The Entry date of PCT National Phase.
Estimated Expiry Date:The statutory expiry date of a patent right according to the Patent Law, and it is the longest term of protection that the patent right can achieve without the termination of the patent right due to other reasons(Term extension factor has been taken into account ).
Invalid Date:Actual expiry date is based on effective date or publication date of legal transaction data of invalid patent.
Login to View More 
Login to View More