Method for removing organic solvent residual in raw medicine

An organic solvent and API technology, applied in the field of chemical engineering, can solve problems such as unsuitable industrial production, loss of tomato oleoresin, removal of APIs, etc., and achieve the effect of realizing recycling, avoiding secondary pollution and large processing capacity.

Inactive Publication Date: 2009-04-15
ZHEJIANG UNIV
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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 CN1545914A disclose a kind of method adopting supercritical carbon dioxide extraction to remove organic solvent in tomato oleoresin, can remove most of organic solvents in tomato oleoresin, but, because tomato oleoresin itself in supercritical carbon dioxide High solubility, resulting in a large amount of loss of tomato oleoresin, making its yield not high, not suitable for industrial production

Method used

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  • Method for removing organic solvent residual in raw medicine

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Experimental program
Comparison scheme
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 residual organic solvents from a bulk drug, which comprises the following steps: firstly, extracting the bulk drug for 0.5 to 2 hours statically and then extracting the bulk drug for 0.5 to 6 hours dynamically under the condition that the temperature is between 35 and 80 DEG C and the pressure is between 10 and 40 MPa, so as to obtain a bulk drug finished product of which the residual organic solvent accords with the limit standard in an extraction kettle; secondly, decompressing and separating carbon dioxide flowing out of the extraction kettle under the condition that the pressure is between 4 and 7 MPa and the temperature is between 25 and 45 DEG C, collecting depositions in a separating kettle, and reclaiming the bulk drug in the depositions for reuse in the extraction kettle. The carbon dioxide flowing out of the separating kettle is adsorbed and separated by using an adsorbent, and the obtained carbon dioxide is introduced to the extraction kettle for recycling. The residual organic solvent in the bulk drug finished product obtained by the method accords with the limit standard, the yield of the bulk drug is high, and the carbon dioxide can be recycled. The method has the advantages of simple process, stable operation, economy and high efficiency, and suitability 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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Patent Type & Authority Applications(China)
IPC IPC(8): B01D11/00
Inventor 苏宝根任其龙邢华斌杨亦文苏云
Owner ZHEJIANG UNIV
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