CN102351868A - Extraction method of morphine from opium - Google Patents
Extraction method of morphine from opium Download PDFInfo
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- CN102351868A CN102351868A CN2011102271998A CN201110227199A CN102351868A CN 102351868 A CN102351868 A CN 102351868A CN 2011102271998 A CN2011102271998 A CN 2011102271998A CN 201110227199 A CN201110227199 A CN 201110227199A CN 102351868 A CN102351868 A CN 102351868A
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Abstract
The invention provides an extraction method of morphine from opium. In the extraction method, the opium is taken as a main raw material, and the extraction method comprises the steps of heating and extracting aqueous solution, concentrating, performing paraffin solid-liquid extraction, removing impurities and the like so as to obtain morphine extract solution. By adopting the method, the impurities can be effectively removed, the yield is high, the preparation process is simple, the repeatability is high, the operability is good, the production cost is low, the energy consumption is low, and the industrialization is easy.
Description
Technical field
The invention belongs to field of pharmaceutical preparations, the process for extracting of morphine in particularly a kind of opium.
Background technology
Opium is opium again, is commonly called as opium, comes from the creamcups capsule.Opium is different because of the place of production, black in color or brown; Ammonia flavor or outmoded urine flavor are arranged, bitter, smell is strong.Raw opium can be made into refining opium through hotting plate and fermenting, and is brown or golden yellow.Distribute fragrant and sweet smell when sucking.Opium is as medicinal at first, in medicine, still has application at present, as powdered opium, opium sheet, platycodon powder compound, Tuo Shi loose, Ah tangerine's sheet etc., be mainly used in antibechic, antidiarrheal etc.
Morphine is topmost vegeto-alkali in the opium (the about 10-15% of content), and it is a kind of psychiatric department medicine, is opioid receptor agonist, and the molecular chemistry formula is C
17H
19NO
3, molecular weight is 285.34, structural formula is following:
Its hydrochloride commonly used or vitriol, medicine is main with oral forms.Morphine has analgesic activity, but short-term is used for the invalid acute intense pain of other anodynes, like three step analgesias of the having an intense pain of operation, wound, burn, patients with advanced cancer; To normotensive myocardial infarction patient, the effect of calm and lightening heart load is arranged, can alleviate frightened mood, also can be used for the preceding administration of cardiac asthma and anesthesia and operation.
Existing document to be adopted successively with solvent extraction, add the dissociate step of morphine and organic solvent extraction of alkali extracts the method for morphine from opium.For example Mehltretter CL etc. (U.S. Pat 2715627) has studied use chloroform, sulfuric acid, water, Virahol, isopropylcarbinol or propyl carbinol and from opium, has extracted morphine; Use acidifying solution, water-miscible organic solvent or 1 to the morphine in the extracting solution after dissociating out with alkaline solution; 2-ethylene dichloride, chloroform or chloroform and the removal of impurities of alcoholic acid mixture extraction, the bullion that obtains contains 62% morphine.John Matchett etc. has studied and has been dissolved in dilute acid soln to opium, with the free morphine of sodium hydroxide, uses benzene extraction more then, behind the evaporate to dryness, uses the solution acidifying, with the free morphine of ammoniacal liquor, extracts with benzene-Virahol at last.(Device for continuous liquid-liquid extraction:Adaptation for the determination of morphine [J]. Ind Eng Chem Anal Ed; 1941; 13 (4); 264-265.) because these class methods have been used the method for liquid-liquid extraction, therefore have organic phase with the organic solution that aqueous phase separation is loaded down with trivial details, use have toxicity, consumption of organic solvent greatly, problems such as organic solvent residual and recovery.
Summary of the invention
The object of the invention is to overcome prior art and from opium, extracts the morphine complicated steps, uses toxic organic solvent, and the problem that extract yield is not high provides that a kind of preparation method is simple, the method for from opium, extracting morphine of high yield.
The object of the invention is achieved through following technical scheme.
The present invention is a kind of method of from opium, extracting morphine, comprises following concrete steps.
(1) opium 40-100 ℃ of heating in aqueous solution is multiple extraction, with extracting liquid filtering, merging;
(2) extracting solution that step (1) is obtained concentrates;
(3) liquid concentrator that step (2) is obtained adds the solid paraffin of fusing, stirs, and adds a cover and leaves standstill, and discards the upper strata solid paraffin, obtains the morphine solution of purifying.
The aqueous solution that process for extracting step of the present invention (1) adopts is pure water or alcohol solution or acidic aqueous solution, and is preferred but be not limited in aqueous ethanolic solution, isopropanol water solution or the dilute hydrochloric acid solution any one.
The alcohol solution concentration that process for extracting step of the present invention (1) adopts is 40%-60%.
Opium and aqueous solution weightmeasurement ratio that process for extracting step of the present invention (1) adopts are 1:10-1:20.
The extraction time that process for extracting step of the present invention (1) adopts is 3 times, each 30～60 minutes extraction times.
The concentrating means that process for extracting step of the present invention (2) adopts is conventional concentrating means, and is preferred but be not limited to decompression or atmospheric distillation.
Morphine content is 1-3% in the said liquid concentrator of process for extracting step of the present invention (2).
The solid paraffin consumption that process for extracting step of the present invention (3) adopts is 1-2 a times of opium weight.
The invention provides the process for extracting of morphine in a kind of preferred opium, extraction step is:
(1) opium and aqueous solution weightmeasurement ratio are 1:20; Adopt following any one condition: 75 ℃ of 60% aqueous ethanolic solutions extract or 80 ℃ of 60% isopropanol water solutions extract or aqueous hydrochloric acid or 100 ℃ of extractions of pure water of pH 4; Extract 3 times, each extraction time is 60 minutes.
(2) extracting solution that step (1) is obtained concentrates;
(3) liquid concentrator that step (2) is obtained adds the solid paraffin of fusing, stirs, and adds a cover and leaves standstill, and discards the upper strata solid paraffin, obtains the morphine solution of purifying.
The consumption of opium described in the present invention does not have concrete restriction, is advisable with the amount that is fit to laboratory to suitability for industrialized production.
The concentration of alcohol solution described in the present invention is meant the volume(tric)fraction that contains alcohol in the 100 volume alcohol solutions.
Opium described in the present invention and aqueous solution weightmeasurement ratio are meant the ratio of opium weight amount unit (gram) and aqueous solution volume amount unit (milliliter).
Described in the present invention in the liquid concentrator morphine content be meant the weight of morphine in the 100 volume liquid concentrators.
The extracting solution that adopts Chinese Pharmacopoeia CP2010 tinctura opii analysis on Content method that the inventive method is obtained identifies and assay that specific analytical method is:
Measuring method: getting with the octadecylsilane chemically bonded silica is one of the solid phase pillar of weighting agent; Use methanol-water (3:1) 15ml and water 5ml flushing successively; Ammonia soln (water intaking is an amount of, and dripping ammonia solution to pH value is 9) with pH ≈ 9 washes to effluent pH ≈ 9, and is for use.One bottle of these article of getting shake up, and precision is measured 5ml, put in the ground Erlenmeyer flask; 90 ℃ of water-bath evaporated under reduced pressure, the accurate 5% acetum 50ml that adds of residue, close plug, supersound process made the morphine dissolving in 15 minutes; Take out, put to room temperature, filter, precision is measured subsequent filtrate 0.5ml; Put on the solid-phase extraction column, drip ammonia solution and make the pH value of solution in the post be about 9 (upward get in addition with the subsequent filtrate of volume before the appearance and debug in advance) in right amount, shake up to confirm to drip the amount of ammonia solution; After treating that solvent drips to the greatest extent, water 20ml flushing with the 5% acetum wash-out that contains 10% methyl alcohol, is collected elutriant to scale with the 5ml measuring bottle; Shake up, the accurate elutriant 10 μ l that draw inject liquid chromatograph, the record color atlas., promptly get with calculated by peak area by external standard method.
Fig. 2 is that the HPLC of morphine reference substance analyzes collection of illustrative plates, and Fig. 3 analyzes collection of illustrative plates for the HPLC of the extracting solution that the inventive method obtains, and identical through both RTs under identical chromatographic conditions of contrast, it is morphine that the inventive method of can reaching a conclusion is extracted the material that obtains.
The present invention adopts above-mentioned Chinese Pharmacopoeia CP2010 tinctura opii analysis on Content method to measure morphine content, calculates the morphine yield according to following formula:
Yield=(morphine content that liquid concentrator volume * HPLC measures) * 100%/(theoretical content of the weight * morphine of opium)
The morphine content that HPLC measures in the above-mentioned formula is meant the weight of morphine in the unit volume.The theoretical content of morphine is the morphine content in the report that provides of opium raw material manufacturer, refers to the weight of morphine in the per unit weight opium.
The morphine solution that the present invention obtains can add proper supplementary material and solvent, can be mixed with the preparation that contains morphine, for example tinctura opii, paregoric and glycyrrhiza compound oral liquid etc.
Morphine of the present invention has anesthesia, analgesic effect to cns.
Morphine of the present invention can suppress the activity of brain respiratory centre and coughing centre, breathing is slowed down and produce suppression to cough effect.
Morphine of the present invention is for cardiovascular systems, and the therapeutic dose morphine does not have obvious effect to blood vessel and heart rate, and heavy dose of morphine can cause postural hypotension and bradyrhythmia.
Morphine of the present invention has excitation to gastrointestinal smooth muscle, the sphincter muscle of Digestive tract, and its tension force is improved, and therefore wriggle weakness has antidiarrheal and the effect that treats constipation.
The present invention compared with prior art has following advantage.
(1) the present invention adopts aqueous solutions such as water, dilute hydrochloric acid solution, aqueous ethanolic solution and isopropanol water solution to extract, and to extract concentration, the conditions such as temperature, extraction time and extraction time of extracting are optimized, and shorten extraction time, have improved extraction efficiency.
(2) the present invention adopts paraffin liquid-solid extraction technology, can effectively remove impurity, and not influence the yield of morphine; Because mixing stirring extraction after coagulation with extracting solution, melting wax become solid to float on the solution upper strata; Be easy to realize and the separating of morphine extracting solution that method is simple, and the paraffin safety non-toxic; With respect to using poisonous organic solvents such as benzene, chloroform in the prior art, the product that the inventive method obtains has very high quality and well security.
(3) product that obtains of the inventive method is the aqueous solution that contains morphine, therefore can directly add proper supplementary material and solvent, is mixed with the liquid preparation that contains morphine, for example tinctura opii, paregoric and glycyrrhiza compound oral liquid etc.
(4) preparation method of the present invention is simple, and repeatability is high and operability is good, and production cost is low, less energy consumption, and yield is high, is easy to industrialization.
Description of drawings
Fig. 1 is the process flow sheet that raw material extracts morphine with the opium for the present invention.
Fig. 2 is the HPLC collection of illustrative plates of morphine reference substance.
The HPLC collection of illustrative plates of the opium extracting solution that Fig. 3 obtains for the inventive method.
Embodiment
Below in conjunction with embodiment the inventive method is further described.
Embodiment 1Adopt aqueous ethanolic solution from opium, to extract morphine.
Comprise following process step successively:
(1) aqueous ethanolic solution of doubly measuring with opium weightmeasurement ratio 10-20 serves as to extract solvent, solvent strength 40%-60%; Heating and refluxing extraction 3 times; The each extraction 30-60 minute.
(2) No. three extracting solutions that (1) obtained concentrate, to morphine content be 1-3%.
(3) solid paraffin of the fusing of 1-2 times of opium weight of adding in the liquid concentrator that (2) obtain stirs, and adds a cover and leaves standstill, and discards the upper strata solid paraffin, obtains the morphine solution of purifying.Adopt the HPLC method to measure morphine content, calculate the morphine yield.
Concrete scheme and result see table 1.
Table 1 aqueous ethanolic solution extracts
| Sequence number | Solvent strength (%) | Solvent load (opium weightmeasurement ratio) | Temperature (℃) | Time (minute) | Yield |
| 1 | 40% | 10 times | 55℃ | 30min/ time | 86.62% |
| 2 | 40% | 15 times | 65℃ | 45min/ time | 91.10% |
| 3 | 40% | 20 times | 75℃ | 60min/ time | 92.14% |
| 4 | 50% | 10 times | 55℃ | 30min/ time | 84.42% |
| 5 | 50% | 15 times | 65℃ | 45min/ time | 91.60% |
| 6 | 50% | 20 times | 75℃ | 60min/ time | 92.82% |
| 7 | 60% | 10 times | 55℃ | 30min/ time | 88.87% |
| 8 | 60% | 15 times | 65℃ | 45min/ time | 92.03% |
| 9 | 60% | 20 times | 75℃ | 60min/ time | 93.69% |
The result shows, when ethanolic soln concentration is 60%, consumption is 20 times of opium weight, and 75 ℃ of extractions are extracted 3 times for 60min/ time, and yield is the highest.
Embodiment 2Pure water extracts.
(1) adopt pure water to extract, consumption is 10-20 a times of opium weight, adopts 60-100 ℃ to extract 30-60min/ time 3 times.
(2) No. three extracting solutions that (1) obtained concentrate, to morphine content be 1-3%.
(3) solid paraffin of the fusing of 1-2 times of opium weight of adding in the liquid concentrator that (2) obtain stirs, and adds a cover and leaves standstill, and discards the upper strata solid paraffin, obtains the morphine solution of purifying.
Concrete scheme and result see table 2.Adopt the HPLC method to measure morphine content, calculate the morphine yield.
Table 2 pure water extracts
| Sequence number | Solvent load (opium weightmeasurement ratio) | Temperature (℃) | Time (minute) | Yield |
| 1 | 10 |
60℃ | 30min/ time | 86.03% |
| 2 | 15 |
80℃ | 45min/ time | 93.28% |
| 3 | 20 times | 100℃ | 60min/ time | 96.05% |
The result shows that the pure water consumption is 20 times of opium weight, 100 ℃ following 60min/ time, extract 3 times, the morphine extract yield is higher.
Embodiment 3Dilute hydrochloric acid solution (pH=4) extracts.
(1) employing pH is 4 dilute hydrochloric acid solution extraction, and consumption is 10-20 a times of opium weight, adopts 60-100 ℃ to extract 30min-60min/ time 3 times.
(2) No. three extracting solutions that (1) obtained concentrate, to morphine content be 1-3%.
(3) solid paraffin of the fusing of 1-2 times of opium weight of adding in the liquid concentrator that (2) obtain stirs, and adds a cover and leaves standstill, and discards the upper strata solid paraffin, obtains the morphine solution of purifying.
Concrete scheme and result see table 3.Adopt the HPLC method to measure morphine content, calculate the morphine yield.
Table 3 pH is 4 dilute hydrochloric acid solution extraction
| Sequence number | Solvent load (opium weightmeasurement ratio) | Temperature (℃) | Time (minute) | Yield |
| 1 | 10 |
60℃ | 30min/ time | 84.25% |
| 2 | 15 |
80℃ | 45min/ time | 92.03% |
| 3 | 20 times | 100℃ | 60min/ time | 95.80% |
The result shows, the consumption that as pH is 4 dilute hydrochloric acid solution is 20 times of opium weight, and 100 ℃ are extracted 3 times, and in the time of 60min/ time, yield is the highest.
Embodiment 4Isopropanol water solution extracts.
(1) doubly measures isopropanol water solution with opium weightmeasurement ratio 10-20 and extract strength of solution 40%-60%.Extract 30min-60min/ time 3 times; Extract temperature: 40 ℃-80 ℃.
(2) No. three extracting solutions that (1) obtained concentrate, to morphine content be 1-3%.
(3) solid paraffin of the fusing of 1-2 times of opium weight of adding in the liquid concentrator that (2) obtain stirs, and adds a cover and leaves standstill, and discards the upper strata solid paraffin, obtains the morphine solution of purifying.
Concrete scheme and result see table 4.Adopt the HPLC method to measure morphine content, calculate the morphine yield.
Table 4 isopropanol water solution extracts
| Sequence number | Solvent strength (%) | Solvent load (opium weightmeasurement ratio) | Temperature (℃) | Time (minute) | Yield |
| 1 | 40% | 10 times | 40℃ | 30min/ time | 82.15% |
| 2 | 40% | 15 |
60℃ | 45min/ time | 93.02% |
| 3 | 40% | 20 |
80℃ | 60min/ time | 96.41% |
| 4 | 50% | 10 times | 40℃ | 30min/ time | 83.46% |
| 5 | 50% | 15 |
60℃ | 45min/ time | 94.20% |
| 6 | 50% | 20 |
80℃ | 60min/ time | 95.78% |
| 7 | 60% | 10 times | 40℃ | 30min/ time | 84.30% |
| 8 | 60% | 15 |
60℃ | 45min/ time | 92.36% |
| 9 | 60% | 20 |
80℃ | 60min/ time | 97.10% |
The result shows, when aqueous isopropanol concentration is 60%, consumption is 20 times of opium weight, and 80 ℃ of extractions are extracted 3 times for 60min/ time, and yield is the highest.
Claims (9)
1. the process for extracting of morphine in the opium is a raw material with the opium, it is characterized in that process for extracting comprises following steps:
(1) opium 40-100 ℃ of heating in aqueous solution is multiple extraction, with extracting liquid filtering, merging;
(2) extracting solution that step (1) is obtained concentrates;
(3) liquid concentrator that step (2) is obtained adds the solid paraffin of fusing, stirs, and leaves standstill, and discards the upper strata solid paraffin, obtains the morphine solution of purifying.
2. the process for extracting of morphine in the opium according to claim 1 is characterized in that the said aqueous solution of said step (1) is pure water or alcohol solution or acidic aqueous solution.
3. like the process for extracting of morphine in the said opium of claim 2, it is characterized in that said aqueous solution adopts any one in aqueous ethanolic solution, isopropanol water solution or the dilute hydrochloric acid solution.
4. like the process for extracting of morphine in the said opium of claim 2, it is characterized in that said alcohol solution concentration is 40%-60%.
5. like the process for extracting of morphine in each said opium of claim 1-4, it is characterized in that said opium of said step (1) and aqueous solution weightmeasurement ratio are 1:10-1:20.
6. like the process for extracting of morphine in the said opium of claim 5, it is characterized in that the said extraction time of said step (1) is 3 times, each 30～60 minutes extraction times.
7. the process for extracting of morphine in the opium according to claim 1 is characterized in that morphine content is 1-3% in the said liquid concentrator of said step (2).
8. the process for extracting of morphine in the opium according to claim 1 is characterized in that 1-2 that the said solid paraffin consumption of said step (3) is an opium weight doubly.
9. process for extracting of morphine in the opium according to claim 1; It is characterized in that said opium of said step (1) and aqueous solution weightmeasurement ratio are 1:20; Adopt following any one condition: 75 ℃ of 60% aqueous ethanolic solutions extract or 80 ℃ of 60% isopropanol water solutions extract or aqueous hydrochloric acid or 100 ℃ of extractions of pure water of pH 4; Extract 3 times, each extraction time is 60 minutes.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102749402A (en) * | 2012-08-07 | 2012-10-24 | 公安部禁毒情报技术中心 | Preparation method of morphine hydrochloride standard substance |
| WO2016053678A1 (en) | 2014-09-30 | 2016-04-07 | Noramco, Inc. | Method for extraction and concentration of alkaloids using dimethyl ether |
| CN110261194A (en) * | 2019-06-06 | 2019-09-20 | 深圳砺剑防卫技术有限公司 | A kind of preparation method and drugs detecting devices verification product of drugs detecting devices verification product |
| WO2023129112A3 (en) * | 2021-12-31 | 2023-10-05 | Toprak Mahsulleri̇ Ofi̇si̇ Genel Müdürlüğü | Process steps to help understanding the invention |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102749402A (en) * | 2012-08-07 | 2012-10-24 | 公安部禁毒情报技术中心 | Preparation method of morphine hydrochloride standard substance |
| WO2016053678A1 (en) | 2014-09-30 | 2016-04-07 | Noramco, Inc. | Method for extraction and concentration of alkaloids using dimethyl ether |
| CN110261194A (en) * | 2019-06-06 | 2019-09-20 | 深圳砺剑防卫技术有限公司 | A kind of preparation method and drugs detecting devices verification product of drugs detecting devices verification product |
| WO2023129112A3 (en) * | 2021-12-31 | 2023-10-05 | Toprak Mahsulleri̇ Ofi̇si̇ Genel Müdürlüğü | Process steps to help understanding the invention |
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Application publication date: 20120215 |