CN100446831C - Method for removing organic solvent from heavy-bodied liquid - Google Patents
Method for removing organic solvent from heavy-bodied liquid Download PDFInfo
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- CN100446831C CN100446831C CNB2006100616983A CN200610061698A CN100446831C CN 100446831 C CN100446831 C CN 100446831C CN B2006100616983 A CNB2006100616983 A CN B2006100616983A CN 200610061698 A CN200610061698 A CN 200610061698A CN 100446831 C CN100446831 C CN 100446831C
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- organic solvent
- thick liquid
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- described method
- ethanol
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Abstract
A process for removing organic solvent from viscous liquid includes such steps as loading said viscous liquid in particular container, and vacuumizing to remove organic solvent from it.
Description
Technical field
The present invention relates to a kind of method of removing organic solvent, exactly is the method for removing organic solvent from thick liquid.The present invention is applicable to pharmacy and chemical field, is specially adapted to pharmaceutical field.
Background technology
Generally adopt the rotary evaporation method for the method for removing organic solvent from thick liquid at present, the thick liquid that promptly will contain organic solvent earlier is rotated evaporation with Rotary Evaporators and removes organic solvent, is divided in the special container then.For example the method for in the United States Patent (USP) 5714512 ethanol that contains in the Tween 80 being taked is exactly first rotary evaporation, then the method for packing.
But the shortcoming of this method is that the packing precision is difficult to reach requirement because the viscosity of thick liquid is bigger, and the packing difficulty is bigger for the thick liquid of packing low dose, and required time is long in actual production.In case and the time lengthening of packing for the production of the injection in the pharmaceutical field, will greatly increase contaminated possibility, thereby cause product defective.
Summary of the invention
The object of the present invention is to provide a kind of method of from thick liquid, removing organic solvent conveniently feasible on producing.
Organic solvent is added in the thick liquid, evenly mixed, be divided in the cillin bottle, vacuumize then and remove organic solvent.
The advantage of this method has been greatly to reduce the difficulty of thick liquid packing, has improved the precision of packing.Because remove the effect that organic solvent has two aspects after the first packing, one side is the viscosity that the existence of organic solvent has reduced thick liquid, the 2nd, and the existence of organic solvent has increased the volume of packing.So greatly reduce the difficulty of thick liquid packing, improved the precision of packing.
Carry out vacuumizing after the packing and can use freeze dryer or vacuum drying chamber; Temperature when vacuumizing is at-10 ℃-30 ℃; Pumpdown time is 3-100 hour.The ethanol of extracting out can reclaim with the condenser system condensation liquefaction or with the form of gas.
The specific embodiment
Embodiment 1
500ml Tween 80 and 500ml absolute ethyl alcohol are mixed (volume ratio is 1: 1), be packed as the 1ml/ cillin bottle, totally 1000 bottles, do not jump a queue and put into freeze dryer and vacuumize;
The freeze dryer baffle temperature is remained 15 ℃; treat to begin to vacuumize after cold well temperature is reduced to below-50 ℃; shut down after 1 hour; discharge ethanol; treat then to begin again to vacuumize after cold well temperature is reduced to below-50 ℃; shut down once more after 17 hours and discharge ethanol, each takes a sample 5, treats then to begin to vacuumize 24 hours (ethanol residual quantity＜2% gets final product) again after cold well temperature is reduced to below-50 ℃.
Embodiment 2
500ml Tween 80 and 1000ml absolute ethyl alcohol are mixed (volume ratio is 1: 2), be packed as the 1.5ml/ cillin bottle, totally 1000 bottles, do not jump a queue and put into vacuum drying chamber and vacuumize;
Vacuum drying chamber is vacuumized 48 hours (ethanol residual quantity＜2% gets final product).
Embodiment 3
Scheme 1: Tween 80 (each 500ml of Tween 80 and the absolute ethyl alcohol) rotary evaporation that 1000ml is contained absolute ethyl alcohol is removed behind the ethanol (ethanol residual quantity＜2% gets final product) with industrial peristaltic pump packing, and the branch loading amount is the 0.5ml/ cillin bottle;
Scheme 2: the Tween 80 (each 500ml of Tween 80 and absolute ethyl alcohol) that 1000ml is contained absolute ethyl alcohol is first with industrial peristaltic pump packing, and the branch loading amount is 1.0ml, vacuumizes then to remove ethanol (ethanol residual quantity＜2% gets final product).
Table 1 scheme 1 and scheme 2 packing contrast
| Scheme 1 | Scheme 2 | |
| The used time of packing | 8.5 hour | 0.5 hour |
| Packing precision (X ± SD (n=20)) (all adopting gravimetric detemination) | 503mg±98mg | 502mg±20mg |
Annotate: what both measured all is the amount of finally removing the tween of ethanol.
As can be seen from the above table, used time of scheme 2 packing is few, and the precision height is fit to industrialized production.
Claims (6)
1. method of removing organic solvent from thick liquid is characterized in that may further comprise the steps:
Organic solvent is added in the thick liquid, evenly mixed, be divided in the cillin bottle, vacuumize then and remove organic solvent.
2. the described method of claim 1, the equipment that it is characterized in that vacuumizing usefulness is freeze dryer.
3. the described method of claim 1, the equipment that it is characterized in that vacuumizing usefulness is vacuum drying chamber.
4. the described method of claim 1, the temperature when it is characterized in that vacuumizing is limited to-10 ℃-30 ℃.
5. the described method of claim 1 is characterized in that the pumpdown time is 3-100 hour.
6. according to the described method of the arbitrary claim of claim 1 to 5, it is characterized in that the thick liquid Tween 80 that will contain organic solvent ethanol is divided in earlier in the cillin bottle, vacuumizes then and removes ethanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100616983A CN100446831C (en) | 2006-07-19 | 2006-07-19 | Method for removing organic solvent from heavy-bodied liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100616983A CN100446831C (en) | 2006-07-19 | 2006-07-19 | Method for removing organic solvent from heavy-bodied liquid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101028566A CN101028566A (en) | 2007-09-05 |
| CN100446831C true CN100446831C (en) | 2008-12-31 |
Family
ID=38714227
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100616983A Expired - Fee Related CN100446831C (en) | 2006-07-19 | 2006-07-19 | Method for removing organic solvent from heavy-bodied liquid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100446831C (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1242199A (en) * | 1998-07-17 | 2000-01-26 | 张家口市长城制药厂 | Process for producing powder injection of compound red sage root medicine |
-
2006
- 2006-07-19 CN CNB2006100616983A patent/CN100446831C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1242199A (en) * | 1998-07-17 | 2000-01-26 | 张家口市长城制药厂 | Process for producing powder injection of compound red sage root medicine |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101028566A (en) | 2007-09-05 |
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| PB01 | Publication | ||
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20081231 Termination date: 20190719 |
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| CF01 | Termination of patent right due to non-payment of annual fee |