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Method for preparing single crystal or amorphous substance of medicine or medicine intermediatemedicinemedicine with adjustable particle size

An amorphous and intermediate technology, applied in the direction of single crystal growth, single crystal growth, chemical instruments and methods, etc., can solve the problems of poor controllability of crystal nucleation and growth, easy generation of polycrystals or twins, etc. Solve the effect that the formation of single crystal is not easy to control

Pending Publication Date: 2019-12-24
INST OF CHEM CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above methods generally have problems such as poor controllability of crystal nucleation and growth, and prone to polycrystals or twins.

Method used

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  • Method for preparing single crystal or amorphous substance of medicine or medicine intermediatemedicinemedicine with adjustable particle size
  • Method for preparing single crystal or amorphous substance of medicine or medicine intermediatemedicinemedicine with adjustable particle size
  • Method for preparing single crystal or amorphous substance of medicine or medicine intermediatemedicinemedicine with adjustable particle size

Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach

[0154] According to an embodiment of the present invention, the method for cultivating a single crystal further includes the following steps:

[0155] (b1) transferring the single crystal of the drug or drug intermediate prepared above to the mother liquor of the drug or drug intermediate for cultivation;

[0156] (b2) Collecting the single crystal in step (b1).

[0157] According to an embodiment of the present invention, the transfer is any method known to those skilled in the art that can remove a single crystal, including but not limited to optical microscope transfer, scanning electron microscope transfer, dual-beam electron microscope transfer , Transmission electron microscope transfer in one or a combination of several.

[0158] According to an embodiment of the present invention, the mother liquor is a mother liquor system known by those skilled in the art and compatible with the single crystal phase to be cultivated, for example, it can be a saturated solution syste...

Embodiment 1

[0162] Prepare a 10-hydroxycamptothecin solution with a concentration of 5 μM in dimethyl sulfoxide, take 5 parts of 5 mL of the solution into a beaker with a graduated cylinder, and place it in liquid nitrogen at -196 ° C until it is completely frozen, and then Slowly heat up at 8°C / min and place them in temperature-controlled cold traps at -50°C, -45°C, -40°C, -35°C, and -25°C for aging for 40 minutes, and then freeze-dry the sample to completely sublimate the solid dimethylformamide 10-Hydroxycamptothecin single crystal nanoparticles can be obtained, and the average particle size is continuously adjustable from 10nm to 1000nm. The test results are shown in Figure 4 ,from Figure 4 It can be seen from the figure that the average particle diameters of the prepared 10-hydroxycamptothecin single crystal nanoparticles are 10.7nm, 130nm, 420nm, 650nm, 1190nm, respectively. Finally, 1000 mL of 0.1 mg / mL Tween-80 solution was used to collect the 10-hydroxycamptothecin single crys...

Embodiment 2

[0165] Use 95wt% chloroform-5wt% methanol mixed solvent to prepare a 10-hydroxycamptothecin solution with a concentration of 5mM, take 100μL of the solution with a syringe, spread it on a silicon wafer, and place it in -196°C liquid nitrogen to cool down completely Freeze, then slowly heat up at 5°C / min and place them in temperature-controlled cold traps at -100°C, -96°C, -88°C, -85°C, and -79°C for 45 minutes, then freeze-dry the sample and sublime completely solid solvent, 10-hydroxycamptothecin single crystal nanoparticles can be obtained, and the average particle sizes are 12nm, 105nm, 440nm, 680nm, 1200nm respectively. Finally, 1000 mL of 0.1 mg / mL Span-80 solution was used to collect the obtained single crystal nanoparticles to form a stable suspension.

[0166] In addition, spread 50 μL of the above-mentioned 5 mM 10-hydroxycamptothecin solution on the silicon wafer cooled to -150 °C, and then raise the temperature to -100 °C, -88 °C, -79 °C at a heating rate of 25 °C / m...

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Abstract

The invention provides a method for preparing a single crystal or amorphous substance of a medicine or a medicine intermediate with adjustable particle size. According to the method, the supply and aggregation rate of medicine or medicine intermediate molecules is controlled by freezing and curing a medicine or medicine intermediate solution, so that the medicine or medicine intermediate single crystal or amorphous substance with adjustable particle size is prepared. Controllable preparation of the single crystal or amorphous substance of the medicine or the medicine intermediate is achieved in a mode of freezing the medicine or the medicine intermediate solution for the first time; by controlling the freezing and curing process of the solution, the supply rate and aggregation rate of themedicine or medicine intermediate are regulated and controlled, so that whether the medicine or medicine intermediate can be nucleated and crystallized and the crystal growth condition thereof are regulated and controlled, and the single crystal or amorphous substance of the medicine or medicine intermediate is efficiently prepared. Meanwhile, the particle size of the medicine or the medicine intermediate single crystal or amorphous substance is regulated and controlled by controlling the curing temperature.

Description

[0001] This application claims the priority of the prior application of the patent application number 2018112806394 submitted to the State Intellectual Property Office of China on October 30, 2018, and the title of the invention is "a method for preparing and cultivating a single crystal of a drug or drug intermediate". The entirety of the prior application is incorporated by reference into the present application. technical field [0002] The invention relates to the technical field of preparation of single crystals or amorphous substances, in particular to a method for preparing single crystals or amorphous substances of drugs or drug intermediates with adjustable particle size. Background technique [0003] Drugs, whether they are natural drugs (such as plant drugs, antibiotics, biochemical drugs, etc.), synthetic drugs or genetically engineered drugs, are chemically composed of chemical elements such as C, H, O, N, S, etc. Taste. However, drugs are not just general chem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B7/08C30B29/54
CPCC30B7/08C30B29/54B01F33/836B01D9/04B01D9/0063B01D2009/0086
Inventor 王健君周昕薛涵吕健勇
Owner INST OF CHEM CHINESE ACAD OF SCI
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