CN102526163A - Method for extracting Olibanum and Myrrha in Fengtongling medicament - Google Patents
Method for extracting Olibanum and Myrrha in Fengtongling medicament Download PDFInfo
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- CN102526163A CN102526163A CN2011104592601A CN201110459260A CN102526163A CN 102526163 A CN102526163 A CN 102526163A CN 2011104592601 A CN2011104592601 A CN 2011104592601A CN 201110459260 A CN201110459260 A CN 201110459260A CN 102526163 A CN102526163 A CN 102526163A
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Abstract
The invention relates to a method for extracting Olibanum and Myrrha in Fengtongling medicament, which replaces the methods for extracting Olibanum and Myrrha in Fengtongling medicament in the prior art. The invention is characterized in that methylene chloride is used as an extraction solvent during the extraction process; the consumption of methylene chloride is 0.1 to 2 times the total weight of Olibanum and Myrrha; the extraction method is one available in solvent extraction methods of traditional Chinese medicines and comprises the steps of mixing, ultrasonic treatment and refluxing; during the preparation process of Fengtongling medicament, the procedure of extracting Olibanum and Myrrha with methylene chloride is performed after first-time extraction with methyl salicylate or after second-time or third-time extraction with methyl salicylate; and the application of methylene chloride as extraction solvent of Olibanum and Myrrha in Fengtongling medicament can improve safety of production and application of Fengtongling medicament.
Description
Technical field
The present invention relates to the method for distilling of a kind of Olibanum and Myrrha, be used for substituting the method for distilling of existing wind clever production technology Olibanum of pain and Myrrha.
Background technology
The 9th in Chinese traditional patent formulation preparation records wind pain spirit (WS
3-B-1709-94) target level of product quality, its prescription element is Olibanum, Myrrha, Sanguis Draxonis, thymol, Borneolum Syntheticum, Camphora, Mentholum, Oleum Ocimi Gratissimi, methyl salicylate.Function cures mainly and is promoting blood circulation to remove blood stasis, and reducing swelling and alleviating pain is used for the bruise pain, rheumatic arthralgia, and chilblain is red and swollen.Wherein Olibanum is the resin that Burseraceae Boswellia carterii Boswellia carterii Birdw. and congener Boswellia bhaw-dajiana Birdw. bark ooze out.Warm in nature, acrid in the mouth is bitter, main component for free α-boswellic acid, β-boswellic acid, combine boswellic acid and ferulic acid and amaroid, volatilization wet goods.Myrrha is for olive subject plant Herba Violae tree Commiphora myrrha Engl. or breathe out the dry resin that Herba Violae is set Commiphora molmol Engl..Property is put down, bitter in the mouth, and main component is resin, natural gum and volatile oil, the two all has promoting blood circulation and stopping pain, the effect of detumescence and promoting granulation.In the existing production technology of wind pain spirit, following technology (abbreviation original production process) is taked in the extraction of Olibanum and Myrrha: get Olibanum, Myrrha is ground into fine powder, get that not have medicated powder to add methyl salicylate an amount of; Stir after 1 hour; Hold over night adds the Olibanum fine powder again, stirs 3 hours in 38 ℃; Filter filtrate for later use.Medicinal residues add chloroform, stir 0.5 hour, filter, and filtrating (the chloroform extraction thing of claiming Olibanum, Myrrha) is subsequent use.Medicinal residues add methyl salicylate again and extract secondaries in 38 ℃ in right amount, stir 3 hours for the first time, stir 2 hours for the second time, filter, merges above-mentioned each filtrate, subsequent use.
Wherein use chloroform as one of extracts active ingredients solvent, and chloroform is claimed chloroform, for three hydrogen atoms in the methane molecule are replaced the chemical compound that generates, molecular formula CHCl by chlorine
3, be harmful liquid, can be by skin absorbs, it also is deleterious sucking its steam, chloroform mainly acts on the central nervous system, has anesthetic action, and the heart, liver, kidney are had infringement.Its acute toxicity influence: suck or absorb and cause acute poisoning through skin; There are headache, dizziness at initial stage, feel sick, vomiting, excited, skin is damp and hot and the MMi symptom; Present abalienation, hypopnea, areflexia, stupor etc. later on; Respiratory paralysis, ventricular fibrillation take place in weight person, simultaneously can be with liver, renal damage.During accidental poisoning, stomach has burn feeling, accompanies and feels sick, vomits, suffers from abdominal pain, suffers from diarrhoea, and occurs later on anaesthetizing symptom again, can cause dermatitis, eczema, even skin burn.The influence of its chronic toxicity: mainly cause liver injury, and symptoms such as dyspepsia, weak, headache, insomnia are arranged, minority has renal damage and has a liking for the chloroform addiction.Under illumination; Chloroform can also be oxidized to hydrogen chloride and the phosgene that severe toxicity is arranged by airborne oxygen; Therefore use chloroform in this production technology as extraction solvent; May also possibly there be safety hidden danger aspect the clinical use simultaneously to production operation personnel's the actual bodily harm that causes in process of producing product.
Summary of the invention
To the problem that exists in the clever production technology of present wind pain, the present invention substitutes chloroform as the extracts active ingredients solvent with dichloromethane, is applied to the extraction production of Olibanum and Myrrha in the spirit of wind pain.
The concrete operations step is:
Step 1: get Olibanum, Myrrha is ground into fine powder, get that not have medicated powder to add methyl salicylate an amount of, stir after 1 hour, hold over night adds the Olibanum fine powder again, stirs 3 hours (methyl salicylate extracts for the first time) in 38 ℃, filters filtrate for later use.
Step 2: the medicinal residues of getting step 1 add by weight the dichloromethane for 0.1～2 times of Olibanum and Myrrha gross weight; Extract (comprising the extracting mode that Chinese medicine solvent extraction methodes such as stirring, ultrasonic, backflow possibly exist) 10 minutes～1.5 hours; Filter filtrate for later use.
Step 3: the medicinal residues of getting step 2 add methyl salicylate again and extract secondaries in 38 ℃ in right amount, stir for the first time 3 hours (methyl salicylate extracts for the second time), stir for the second time 2 hours (methyl salicylate extracts for the third time), filter, merges above-mentioned each filtrate, subsequent use.
Wherein also can be after methyl salicylate extracts for the second time with the operation of dichloromethane extraction; Perhaps after methyl salicylate extracts for the third time; Its characteristics are to substitute the chloroform in the original production process with dichloromethane; Dichloromethane is that two hydrogen atoms are replaced the chemical compound that generates, molecular formula CH by chlorine in the methane molecule
2Cl
2The polarity and the chloroform of dichloromethane are close, and be close to the extraction performance of Chinese crude drug, and this chemical compound is that the methane chloride toxic is minimum, rat oral median lethal dose(LD 50) (LD
50) be 2524mg/Kg, and the LD of chloroform
50Be 1194mg/Kg.Use the extraction solvent of dichloromethane, can improve the safety of the clever production operation of wind pain, reduce patient's risk safe in utilization as Olibanum and Myrrha in the spirit of wind pain.
Description of drawings
Fig. 1: transdermal test in vitro absorption curve
The specific embodiment
Below further specify the present invention through embodiment, the Olibanum that the present invention relates to and the method for distilling of Myrrha specifically are applied in the production of wind pain spirit, specific embodiment also embodies with preparation through the prescription of wind pain spirit.
1, specific embodiment
Embodiment 1
Olibanum 25g Myrrha 25g Sanguis Draxonis 2g thymol 10g
Borneolum Syntheticum 30g Camphora 30g Mentholum 280g dichloromethane 27g
Essence 80ml Oleum Ocimi Gratissimi 40.1ml methyl salicylate is an amount of
More than ten simply, get Olibanum, Myrrha is ground into fine powder, get that not have medicated powder to add methyl salicylate an amount of, stir after 1 hour, hold over night adds the Olibanum fine powder again, stirs 3 hours in 38 ℃, filters filtrate for later use.Medicinal residues add methylene chloride, and stir 0.5 hour, filter filtrate for later use.Medicinal residues add methyl salicylate again and extract secondaries in 38 ℃ in right amount, stir 3 hours for the first time, stir 2 hours for the second time, filter, and merge above-mentioned each filtrating, add seven flavors such as Sanguis Draxonis, stir, and dissolving, filtration adds methyl salicylate to 1000g, promptly gets.
Embodiment 2
Olibanum 25g Myrrha 25g Sanguis Draxonis 2g thymol 10g
Borneolum Syntheticum 30g Camphora 30g Mentholum 280g dichloromethane 50g
Essence 80ml Oleum Ocimi Gratissimi 40.1ml methyl salicylate is an amount of
More than ten simply, get Olibanum, Myrrha is ground into fine powder, get that not have medicated powder to add methyl salicylate an amount of, stir after 1 hour, hold over night adds the Olibanum fine powder again, stirs 3 hours in 38 ℃, filters filtrate for later use.Medicinal residues add methylene chloride, and ultrasonic 0.5 hour, filter, filtrating (dichloromethane extract of claiming Olibanum, Myrrha) is subsequent use.Medicinal residues add methyl salicylate again and extract secondaries in 38 ℃ in right amount, stir 3 hours for the first time, stir 2 hours for the second time, filter, and merge above-mentioned each filtrating, add seven flavors such as Sanguis Draxonis, stir, and dissolving, filtration adds methyl salicylate to 1000g, promptly gets.
Embodiment 3
Olibanum 25g Myrrha 25g Sanguis Draxonis 2g thymol 10g
Borneolum Syntheticum 30g Camphora 30g Mentholum 280g dichloromethane 100g
Essence 80ml Oleum Ocimi Gratissimi 40.1ml methyl salicylate is an amount of
More than ten simply, get Olibanum, Myrrha is ground into fine powder, get that not have medicated powder to add methyl salicylate an amount of, stir after 1 hour, hold over night adds the Olibanum fine powder again, stirs 3 hours in 38 ℃, filters filtrate for later use.Medicinal residues add methylene chloride, and reflux 0.5 hour, filter filtrate for later use.Medicinal residues add methyl salicylate again and extract secondaries in 38 ℃ in right amount, stir 3 hours for the first time, stir 2 hours for the second time, filter, and merge above-mentioned each filtrating, add seven flavors such as Sanguis Draxonis, stir, and dissolving, filtration adds methyl salicylate to 1000g, promptly gets.2, the chloroform extraction thing comparative study of the dichloromethane extract of embodiment 1 Olibanum, Myrrha and Olibanum, Myrrha
The comparison that must measure admittedly
Get Olibanum 25g, Myrrha 25g prepares Olibanum, Myrrha dichloromethane extract by embodiment 1 method, and other gets Olibanum 25g; Myrrha 25g by the original production process method prepare Olibanum, Myrrha chloroform extraction liquid is put respectively in the evaporating dish of 40 ℃ of drying under reduced pressure to constant weights; Make solvent evaporates in 40 ℃ of drying under reduced pressure, and be dried to constant weight, calculate solid weight in the evaporating dish; Acetonideexample 1 method prepares Olibanum, the Myrrha dichloromethane extract must be measured admittedly and be 0.5412g; The original production process method prepares Olibanum, Myrrha chloroform extraction liquid must be measured admittedly and be 0.5304g, two kinds of extracting solution must measure basically identical admittedly, do not have significant difference.
The comparison of Caprylyl acetate content
Olibanum and Myrrha master contain volatile oil; These two kinds of volatile oil all can be dissolved in the organic solvents such as chloroform and dichloromethane; Wherein the main component of Olibanum volatile oil is a Caprylyl acetate; With gas chromatography embodiment 1 method being prepared Olibanum, Myrrha dichloromethane extract measures with the content for preparing Caprylyl acetate in Olibanum, the Myrrha chloroform extraction liquid by the original production process method; The total content that acetonideexample 1 method prepares Caprylyl acetate in Olibanum, the Myrrha dichloromethane extract is 78.7mg; The total content for preparing Caprylyl acetate in Olibanum, the Myrrha chloroform extraction liquid by the original production process method is 78.1mg, and the Caprylyl acetate content basically identical of two kinds of extracting solution is described.
3, the transdermal test in vitro of embodiment 1 absorbs
(accept the long-pending 16ml of being of cell body, the effective contact area of reception tank is 4.52cm to adopt improvement Franz device
2), fixture as absorption liquid, is got rat skin in vitro with 5% ethanol normal saline; Three-dimensional Corium Mus horny layer one side to the Franz device, is close to the spirit of wind pain in skin corium one side, constant temperature water bath to (37 ± 1) ℃; The electromagnetism constant speed stirs, and respectively at 1,3,4,7,9,12,24 hour taking-up 2ml acceptable solution from sample cell, adds 5% ethanol normal saline of equivalent simultaneously; The acceptable solution that takes out is analyzed eugenol content in gas chromatograph, calculate the accumulative total transit dose, sees table 1; With the accumulative total transit dose is vertical coordinate, and time T is an abscissa, draws the transdermal test in vitro absorption curve, sees Fig. 1.
Table 1 transdermal test in vitro accumulation transit dose
Transdermal test in vitro absorption test result shows that the wind pain spirit that embodiment 1 and original production process are produced all can pass through skin absorbs, the absorption curve basically identical, and reach value within a certain period of time.
4, the skin acute toxicity of embodiment 1 is observed
2 groups of 8 branches of rabbit; Wherein the well word is drawn as the damaged skin group with blade by four skin depilatory districts, and other four is the intact skin group, and clever 4.0ml/ only is applied to the depilation district with the wind pain; Observe by the sky in 14 days; The behavioral activity of two groups of rabbit, diet, fur gloss and body weight have no effect, and no rabbit is dead, any acute toxic reaction do not occur.
5, the skin irritation of embodiment 1 is observed
2 groups of 6 branches of rabbit, wherein the well word is drawn as the damaged skin group with blade by 3 skin depilatory districts, and other 3 is the intact skin group, adopts the contrast of consubstantiality left and right sides self; QUMAO district, left side is coated with the clever 1ml of embodiment 1 wind pain, and the right side is coated with the clever 1ml of wind pain that original production process is produced, and administration is after 24 hours; Remove remnants with warm water and tried thing, and in 1h, 24h; 48h, 72h hour, record was smeared the position and is had or not situation such as erythema, edema.Two kinds of clever administration smear zones of wind pain of intact skin group have inadequate visible erythema at 1h as a result, all recover in 24 hours.The clever smear zone of embodiment 1 wind pain of damaged skin is at 1h, and 24h has inadequate visible erythema, recovers in 48 hours; The clever smear zone of wind pain that the original production process of damaged skin is produced is at 1h, 24h, inadequate visible erythema arranged in 48 hours, recovers gradually in 72 hours.
6, the skin hypersensitivity of embodiment 1 is observed
Albino guinea-pig back left side QUMAO is pressed the skin semar technique and is given embodiment 1 wind pain clever 0.2ml, continues 6 hours, and in administration after 24 hours; Excited administration on the 28th day with the method repeat administration on the 14th day, clever 0.2ml is applied in QUMAO district, guinea pig back right side with embodiment 1 wind pain; Flush away is tried thing after 6 hours, observes at once, then in 24h; 48h, 72h observes once more, and skin does not have allergic phenomena generations such as erythema as a result.It is thus clear that the spirit of embodiment 1 wind pain does not produce sensitization.
7, the clever crowd of the wind of embodiment 1 pain is on probation
The clever function of wind pain cures mainly and is promoting blood circulation to remove blood stasis, reducing swelling and alleviating pain.Be used for the bruise pain, rheumatic arthralgia, chilblain is red and swollen.
32 acute soft tissue injury patients use the wind pain spirit of embodiment 1, every day 4 times, use a week after, subjective symptoms is obviously improved, swelling obviously improves.40 chilblain patients use the wind pain spirit of embodiment 1, every day 4 times, use a week after, pruritus disappears with local red and swollen phenomenon, the wind of all embodiment 1 clever user does not bitterly in use produce sense of discomfort.Do not produce untoward reaction.
Model case:
Once * *, 38 years old, right sufficient soft tissue contusion, symptom is that right foot pain, swelling, tenderness are obvious; Local visible subcutaneous extvavasated blood speckle, right knee joint activity is slightly limited, gives the clever external of wind pain of embodiment 1, one or four times; Continuous 7 days, used for 1 week after, symptom is obviously improved; Swelling disappears, and activity does not have any discomfort freely between the operating period.
Claims (3)
1. the method for distilling of Olibanum and Myrrha is characterized in that described method for distilling is used for the spirit of wind pain and produces.
2. the method for distilling of a kind of Olibanum according to claim 1 and Myrrha is characterized in that using in the leaching process dichloromethane as extraction solvent.
3. according to the method for distilling of claim 1,2 described a kind of Olibanums and Myrrha, the use amount that it is characterized in that dichloromethane is Olibanum and Myrrha gross weight 0.1～2 times.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011104592601A CN102526163A (en) | 2011-12-27 | 2011-12-27 | Method for extracting Olibanum and Myrrha in Fengtongling medicament |
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| CN2011104592601A CN102526163A (en) | 2011-12-27 | 2011-12-27 | Method for extracting Olibanum and Myrrha in Fengtongling medicament |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104587388A (en) * | 2015-01-08 | 2015-05-06 | 季一艮 | Pharmaceutical composition for treating knee arthritis through external application and preparation method thereof |
Citations (3)
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| CN1096672A (en) * | 1993-06-22 | 1994-12-28 | 丛繁滋 | Warming and resuscitation inducing aerosol and preparation method thereof |
| WO2010087964A2 (en) * | 2009-01-28 | 2010-08-05 | Nanobio Corporation | Compositions for treatment and prevention of acne, methods of making the compositions, and methods of use thereof |
| WO2010100651A2 (en) * | 2009-03-04 | 2010-09-10 | Regenera Pharma Ltd. | Compositions of polymeric myrcene |
-
2011
- 2011-12-27 CN CN2011104592601A patent/CN102526163A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1096672A (en) * | 1993-06-22 | 1994-12-28 | 丛繁滋 | Warming and resuscitation inducing aerosol and preparation method thereof |
| WO2010087964A2 (en) * | 2009-01-28 | 2010-08-05 | Nanobio Corporation | Compositions for treatment and prevention of acne, methods of making the compositions, and methods of use thereof |
| WO2010100651A2 (en) * | 2009-03-04 | 2010-09-10 | Regenera Pharma Ltd. | Compositions of polymeric myrcene |
Non-Patent Citations (1)
| Title |
|---|
| 中华人民共和国卫生部: "《中华人民共和国卫生部药品标准•中药成方制剂》", 31 December 1994 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104587388A (en) * | 2015-01-08 | 2015-05-06 | 季一艮 | Pharmaceutical composition for treating knee arthritis through external application and preparation method thereof |
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Application publication date: 20120704 |