Method for removing organic solvent residue from bulk drug

A technology of organic solvents and raw materials, applied in the field of chemical engineering, can solve problems such as unsuitability for industrial production, loss of tomato oleoresin, removal of raw materials, etc., and achieve the effect of recycling, avoiding secondary pollution, and large processing capacity

Inactive Publication Date: 2016-02-24
SHANDONG GUANGTONGBAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are very few studies and reports on the application of supercritical fluid technology to remove organic solvents in finished products or semi-finished products (food and pharmaceuticals). So far, there are no relevant patents and public reports on using this technology to remove organic solvent residues in raw materials.
[0006] Chinese patent application CN1523064A and CN1545

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  • Method for removing organic solvent residue from bulk drug

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Daunorubicin hydrochloride 1.2g (residual amount of methanol 3.17wt%, residual amount of chloroform 0.95wt%) is packed in the extraction kettle, then filled with CO 2 , the temperature was set at 50°C, the pressure was maintained at 35MPa, and static extraction was performed for 0.5 hours. Maintain the same temperature and pressure, keep the SCCO 2The flow rate is 6g / hr for dynamic extraction, and the extraction time is 4 hours. After the extraction is completed, collect the sample in the kettle to obtain the daunorubicin hydrochloride finished product, the residual amount of methanol is 669ppm, and the residual amount of chloroform is 31ppm.

[0029] SCCO out of the extraction kettle 2 Enter the decompression separation kettle, set the pressure of the separation kettle to 6MPa, and the temperature to 30°C, collect the precipitate in the separation kettle, concentrate and dry to obtain the recovered raw material drug, and transfer it to the extraction kettle for mecha...

Embodiment 2

[0033] Daunorubicin hydrochloride 1.2g (residual amount of methanol 3.17wt%, residual amount of chloroform 0.95wt%) is packed in the extraction kettle, then filled with CO 2 , the temperature was set at 40°C, the pressure was maintained at 20MPa, and the static extraction was carried out for 0.5 hours. Maintain the same temperature and pressure, keep the SCCO 2 The flow rate is 6g / hr for dynamic extraction, and the extraction time is 4 hours. After the extraction was completed, the sample in the kettle was collected to obtain the daunorubicin hydrochloride finished product, wherein the residual amount of methanol was 1124ppm, and the residual amount of chloroform was 52ppm.

[0034] SCCO out of the extraction kettle 2 Enter the decompression separation kettle, set the pressure of the separation kettle to 6MPa, and the temperature to 30°C, collect the precipitate in the separation kettle, concentrate and dry to obtain the recovered raw material drug, and transfer it to the ex...

Embodiment 3

[0038] Daunorubicin hydrochloride 1.2g (residual amount of methanol 3.17wt%, residual amount of chloroform 0.95wt%) is packed in the extraction kettle, then filled with CO 2 , the temperature was set at 40°C, the pressure was maintained at 20MPa, and the static extraction was carried out for 0.5 hours. Maintain the same temperature and pressure, keep the SCCO 2 The flow rate is 12g / hr for dynamic extraction, and the extraction time is 3 hours. After the extraction was completed, the sample in the kettle was collected to obtain the daunorubicin hydrochloride finished product, wherein the residual amount of methanol was 1040 ppm, and the residual amount of chloroform was 47 ppm.

[0039] SCCO out of the extraction kettle 2 Enter the decompression separation kettle, set the pressure of the separation kettle to 7MPa, and the temperature to 40°C, collect the precipitate in the separation kettle, concentrate and dry to obtain the recovered raw material drug, and transfer it to the...

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Abstract

The invention discloses a method for removing organic solvent residue from a bulk drug. The method includes: under a temperature of 35-80DEG C and a pressure of 10-40MPa, firstly performing static extraction for 0.5-2h, and then conducting dynamic extraction for 0.5-6h so as to obtain a bulk drug finished product with the organic solvent residue meeting the limit standard in an extraction kettle; carrying out pressure reduction separation on the carbon dioxide flowing out of the extraction kettle at a pressure of 4-7MPa and a temperature of 25-45DEG C, collecting the precipitate in a separation kettle, recovering the bulk drug, and loading the bulk drug into the extraction kettle for application. An adsorbent is employed to conduct adsorption separation on the carbon dioxide flowing out of the separation kettle, and the obtained carbon dioxide is introduced into the extraction kettle for cycle use. The bulk drug finished product obtained by the method has the organic solvent residue meeting the limit standard, the bulk drug yield is high, and the carbon dioxide can be recycled. The method provided by the invention has the advantages of simple process, stable operation, economical efficiency and high efficiency, and is suitable for industrial application.

Description

technical field [0001] The invention relates to a method for removing residual organic solvents in raw materials, in particular to a supercritical carbon dioxide (SCCO 2 ) extraction combined with decompression separation to remove residual organic solvents in raw materials, which belongs to the technical field of chemical engineering. Background technique [0002] The toxicity or carcinogenicity of residual organic solvents in drugs has attracted increasing attention, and domestic and foreign pharmaceutical management departments have requested to strengthen the restrictions on the residual amount of toxic solvents in drugs, and passed the International Conference on Harmonization (ICH) in 1997. Guiding Principles. Therefore, in order to ensure the quality and drug safety of pharmaceutical products, it is very important to strengthen the control of solvent residues in raw materials. [0003] Raw materials refer to the pharmaceutical raw materials used for the preparation ...

Claims

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Application Information

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IPC IPC(8): B01D11/02
CPCB01D11/0203B01D2011/007B01D2221/10B01D2251/00B01D2259/122
Inventor 曹永民陈玉奎
Owner SHANDONG GUANGTONGBAO PHARMA
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