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A method of extracting dibutyl phthalate from common buried rubber and applications of the dibutyl phthalate

A technology of dibutyl phthalate and ethyl acetate, which is applied in the application of anti-lung cancer drugs and the field of preparation of anti-lung cancer, can solve the problems of little research on small molecule pharmacodynamics and little research on small molecular compounds, and achieve practical High performance, stable properties, and low reagent consumption

Active Publication Date: 2016-06-22
TIANJIN YAOYU BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Because this substance is defined as a harmful chemical product by the public, and is limited to obtain through synthetic methods, there is little research on the small molecule compound that is naturally occurring in the molecule itself, and it is limited to the above-mentioned application, so many scholars study Its toxicological effects, such as reproductive toxicity research, neurotoxicity research, acute toxicity research, etc., but there are relatively few studies on the efficacy of this small molecule

Method used

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  • A method of extracting dibutyl phthalate from common buried rubber and applications of the dibutyl phthalate
  • A method of extracting dibutyl phthalate from common buried rubber and applications of the dibutyl phthalate
  • A method of extracting dibutyl phthalate from common buried rubber and applications of the dibutyl phthalate

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Experimental program
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Effect test

Embodiment 1

[0053] The present embodiment extracts the method for dibutyl phthalate monomer compound from triangular, comprises the following steps:

[0054] (1) Take the dried triangular ribs as the raw material, put them into a superfine pulverizer for superfine pulverization, and use 4°C water as the internal cooling liquid of the superfine pulverizer during the pulverization process, and the superfine pulverization time is 12 minutes to obtain superfine powder.

[0055] (2) Take 3Kg of the above-mentioned triangular superfine powder and extract it three times with ethyl acetate. For the first extraction: add 3kg of superfine powder to 24L ethyl acetate, extract for 70min, and after the extraction is completed, centrifuge at 25°C and 6000rpm for 30min to collect the residue. The second extraction: add the residue of the first extraction into 12L ethyl acetate, extract for 70min, and after the extraction is completed, centrifuge at 25°C and 6000rpm for 30min to collect the residue. The ...

Embodiment 2

[0062] Embodiment 2: the test of inhibiting the growth of human lung cancer A549 cells

[0063] Cell culture:

[0064] Human lung cancer A549 cells were cultured in F-12K (10% FBS+1% PS) medium at 5% CO2, 37°C, and saturated humidity, and the cells growing in logarithmic phase were selected as experimental cells. After counting the cells, dilute it with medium to obtain a certain concentration of cell suspension.

[0065] Cell growth monitoring:

[0066] Put the cell real-time monitor into a 5% CO2, 37°C saturated humidity incubator. Take an 8-well plate, add 150 μL of F-12K medium to each well, and put it into the real-time cell monitor for baseline. After the baseline, take out the eight-well plate and add 345 μL of diluted A549 cell suspension to each well to reach the number of cells in each well. About 2×104 cells, let stand for 3 minutes, and observe whether the cells are uniform under an inverted microscope. Add 5 μL of the diluted drug to each well to a final conce...

Embodiment 3

[0071] Embodiment 3: the test of suppressing the growth of human liver cancer Hep-G2 cells

[0072] Cell culture:

[0073] at 5% CO 2 , 37° C., under saturated humidity, cultured human lung cancer Hep-G2 cells with MEM (10% FBS, 1% PS) medium, and selected cells with good growth status as experimental cells. After counting the cells, dilute it with medium to obtain a certain concentration of cell suspension.

[0074] Cell growth monitoring:

[0075] Place the cell real-time monitor in 5% CO 2 , 37°C saturated humidity incubator. Take an 8-well plate, add 150 μL of MEM medium to each well, put it into a real-time cell monitor for baseline, take out the eight-well plate after the baseline, and add 345 μL of diluted Hep-G2 cell suspension to each well to reach the number of cells in each well. About 4×104 cells, let stand for 3 minutes, and observe whether the cells are uniform under an inverted microscope. Add 5 μL of the diluted drug to each well until the final concentra...

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Abstract

The invention provides a method for extracting dibutyl phthalate from triangular prisms, which comprises the following steps: take triangular prisms and add ethyl acetate to extract after superfine grinding, precipitate after centrifugation and add 95% ethanol for extraction, and centrifuge to extract dibutyl phthalate. Concentrate and dry the supernatant; add 80% methanol-water solution to sonicate to 15-50mg / ml, and 18 Reversed-phase silica gel chromatography column for liquid chromatography separation, using A pure water, B methanol binary mobile phase, the elution method is 20% methanol-water elution 5min, 40% methanol-water elution 7min, 80% methanol-water elution Water was eluted for 13 minutes, 100% methanol was eluted for 5 minutes, and the eluate was collected for 21-22 minutes according to the ultraviolet absorption spectrum, concentrated and vacuum freeze-dried to obtain dibutyl phthalate with a purity of more than 99%. The method has the advantages of stable separation method, high repeatability, large preparation amount, simple and time-saving operation.

Description

technical field [0001] The present invention relates to the technical field of traditional Chinese medicine extraction, in particular to a method for extracting dibutyl phthalate monomer compound from trigonum, and the application of the dibutyl phthalate in the preparation of anti-liver cancer and anti-lung cancer drugs . Background technique [0002] Dibutyl phthalate is a small molecular compound usually obtained by organic synthesis. It is a colorless, transparent or slightly yellow oily liquid, and its molecular formula is C 16 h 22 o 4 , the molecular weight is 278.35, and its skeleton is composed of a structure similar to a four-membered ring. The structural formula is as follows: [0003] [0004] Today's applications of dibutyl phthalate mainly include the following aspects: [0005] 1. Used as gas chromatography stationary liquid and solvent; [0006] 2. Used as a plasticizer, mainly used as a plasticizer for nitrocellulose, cellulose acetate, polyvinyl chl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/80C07C67/48C07C67/56A61K31/235A61P35/00
Inventor 张耀洲庞莉顾朋嫒杜思邈李聪聪姜睿
Owner TIANJIN YAOYU BIOLOGICAL TECH
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