CN1314789C - Method for preparing pure oleum fructus brucease - Google Patents
Method for preparing pure oleum fructus brucease Download PDFInfo
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- CN1314789C CN1314789C CNB2003101083304A CN200310108330A CN1314789C CN 1314789 C CN1314789 C CN 1314789C CN B2003101083304 A CNB2003101083304 A CN B2003101083304A CN 200310108330 A CN200310108330 A CN 200310108330A CN 1314789 C CN1314789 C CN 1314789C
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Abstract
The present invention relates to a method for preparing pure brucea javanica oil, which comprises the preparation steps that proper quantity of brucea javanica fruits are pulverized into coarse powder which is extracted by petroleum ether, and the petroleum ether is recovered by extracting liquid to obtain coarse brucea javanica oil; the obtained coarse brucea javanica oil is heated and is added with dried active carbon of which the weight accounts for 1 to 15% of the volume of the coarse brucea javanica oil; after the coarse brucea javanica oil and the dried active carbon are sufficiently stirred, the mixture carries out pressure reduction and extraction to obtain yellow coarse oil, and dried kaoline of which the weight accounts for 2 to 10% of the volume of the yellow coarse oil is added into the yellow coarse oil; after the dried kaoline and the yellow coarse oil are sufficiently stirred, the mixture carries out pressure reduction and extraction to obtain the brucea javanica oil; the brucea javanica oil obtained in the last step carries out pressure reduction, and nitrogen is led into the brucea javanica oil for 0.5 to 2 hours at the temperature of 90 to 120DEGC to obtain the pure brucea javanica oil. The pure brucea javanica oil prepared by the method has the advantages of high purity and few impurities, and can be used as an ideal raw material for preparing brucea javanica oil emulsion injection.
Description
(1) technical field
The present invention relates to a kind of extraction process of oil soluble vegetable active, specifically is a kind of extraction preparation method who extracts the pure Oleum Fructus Bruceae of anticancer active constituent in the fruit of khosam.
(2) background technology
Kosam seeds, another name crow courage, Semen Sophorae Flavescentis, bitter is poisonous.Be the dry mature fruit of quassia kosam seeds [Brucea javanico (L) Merr], originate in the ground such as Guangdong, Hainan, Guangxi, Fujian of China, gather during fruit maturation autumn, and Ex-all impurity dries.Major function is heat-clearing, hot-tempered wet, desinsection, detoxifcation, corrosion chela wart.Ancient times, China among the peoplely was widely used for treating amebic dysentery.Since nineteen fifty, many scholars treat papilloma of external auditory meatus, laryngeal papillomatosis, cervical cancer etc. with Oleum Fructus Bruceae.Having report to use kosam seeds treatment cervical cancer in 1972 succeeds.Fundamental research and clinical application by many decades subsequently makes medical matters bound pair kosam seeds that further complete understanding arranged, kosam seeds is poisonous, its composition can be divided into water-soluble and fat-soluble two portions, and deleterious composition mainly is water miscible amaroid, several nontoxicitys of its fixed oil.(1) water-soluble components: be a series of tetracyclic triterpenoid.(2) fat-soluble composition: 85%---three oleic acid R-Glyceric acid 10%---oleic acid 5%---linolic acid, other saturated fatty acids, carbon alkanoic acid, diluted acid etc.Oleic acid wherein, linolic acid is considered to antineoplastic active ingredient.
Make the bruceolic oil emulsion intravenous injection with pure Oleum Fructus Bruceae, a large amount of clinical verifications finds that its anticancer spectrum is wide, is applicable to multiple malignant tumours such as lung cancer, metastatic brain tumor, liver cancer, gastroenteric tumor, gynecological tumor, mammary cancer, sarcoma, lymphoma.But, cause pure Oleum Fructus Bruceae extraction process to become most important, when especially preparing intravenous injection owing to also contain toxic component in the kosam seeds.
1994 the 6th volume fourth phases of Strait Pharmaceutical Journal have been reported " extraction of kosam seeds " (author Huang Xiuqing), make extraction agent with chemical pure sherwood oil, extract repeatedly united extraction liquid continuously, reclaim sherwood oil, heating is waved the solvent of leaving over that looses and is promptly got Oleum Fructus Bruceae, yield 14.4%.
2002 the 26th the 10th phases of volume of Heilungkiang medical science are pointed out with chloroform give solvent extraction Oleum Fructus Bruceae content higher in " Oleum Fructus Bruceae extracts preparation and clinical application " literary composition by Wang Qiuhong, Li Jincai, reclaim easily.But as extraction agent, price is more expensive not to be suitable for heavy dose of extraction with chloroform, and chloroform also may residual toxicity, and the author also recommends heavy dose of production to use sherwood oil.
The disadvantage of two pieces of extraction processes that document provides is to be slightly oil of simple Petroleum ether extraction, not refining, purification step.Because the general record of kosam seeds is poisonous plants, be present in water-soluble bitter taste part through clear and definite its toxic component of present research, several nontoxicitys of its fixed oil, therefore, the purity of kosam seeds is related to toxicity problem, must purify, especially will control the content of water-soluble components, require not contain any plant residue such as chlorophyll, deliquescent Mierocrystalline cellulose etc. simultaneously.
(3) summary of the invention:
The objective of the invention is in order to overcome the deficiency that existing Oleum Fructus Bruceae extraction process can not thoroughly be purified, on original technology, increase thick oily purification step, remove in the kosam seeds virose water-soluble composition fully and do not contain any plant residue such as chlorophyll, deliquescent Mierocrystalline cellulose, a kind of extraction preparation method of purity 100% Oleum Fructus Bruceae is provided, thereby provides a kind of preparation Java brucea fruit oil emulsion injection pure safely and effectively Oleum Fructus Bruceae raw material.
Invent the following technical scheme that adopts for this reason:
A kind of preparation method of pure Oleum Fructus Bruceae, preparation as follows: select an amount of fruit of khosam to be ground into meal, with described meal Petroleum ether extraction, extracting solution reclaims sherwood oil and gets slightly oil of kosam seeds, again the thick oil heating of gained kosam seeds back is added the gac of weight in the thick oil volume 0.01～0.15g/mL of kosam seeds drying, stirring fully, decompression extracting in back gets yellow thick oil, again that described yellow is thick oily with the kaolin of weight in the thick oil volume 0.02～0.10g/mL of yellow drying, stirring fully, decompression extracting in back gets Oleum Fructus Bruceae; To go up under 90～120 ℃ of conditions, reduce pressure logical nitrogen 0.5～2 hour of the Oleum Fructus Bruceae that obtains of step again, must pure Oleum Fructus Bruceae.
Specifically, the preparation method of pure Oleum Fructus Bruceae in the following order step carry out:
(1) pulverizes: select an amount of fruit of khosam to be ground into meal;
(2) petroleum ether extraction: by kosam seeds meal weight (kg): sherwood oil volume (L) soaks in encloses container and extracts than being 1: 6～9 to add sherwood oils, filters, and collects filtrate;
(3) thick oil preparation: distilation steps (2) gained filtrate, the heating recovery sherwood oil till dripless flows out, gets slightly oil of blackish green kosam seeds;
(4) refining: that the thick oil of the blackish green kosam seeds of step (3) gained is heated to 70 ℃～95 ℃, to add weight is counted the drying of 0.01～0.15g/mL with the thick oil volume of described kosam seeds gac again after the thick oil heating of gained kosam seeds, stirring fully, decompression extracting in back gets yellow thick oil, the yellow thick oil that obtains is heated to 70 ℃～95 ℃, the thick oil of described yellow is added weight again and count the kaolin of the drying of 0.02～0.10g/mL with the thick oil volume of yellow, stirring fully, decompression extracting in back gets Oleum Fructus Bruceae;
(5) purifying: will go up under 90～120 ℃ of conditions, reduce pressure logical nitrogen 0.5～2 hour of the Oleum Fructus Bruceae that obtains of step, must pure Oleum Fructus Bruceae.
Above-mentioned preparation method's purification step adds gac and kaolin and can adsorb some impurity more up hill and dale, takes away the moisture content in the thick oil simultaneously, the removing of moisture content, and guaranteeing does not thoroughly have the residual of water-soluble toxic substance in the oil.
The described kosam seeds meal of above-mentioned step (2) soaks even more preferably in encloses container, and extraction time is 6～12 hours.The comparatively preferred kaolinic add-on of above-mentioned step (4) is for to count 0.05～0.08g/mL by the thick oil volume of described yellow, and the add-on of gac is counted 0.03～0.05g/mL by the thick oil volume of kosam seeds.
Above-mentioned preferably by kosam seeds meal weight (kg): sherwood oil volume (L) adds sherwood oil than the amount that is 1: 8.
Further, the preferred version of above-mentioned step (5) purifying is: under 100～115 ℃ of conditions, reduce pressure logical nitrogen 0.5～1 hour of the Oleum Fructus Bruceae that step (4) is obtained, pure Oleum Fructus Bruceae.Can make the preparation method of big production more economical like this.
The preparation method of most preferred pure Oleum Fructus Bruceae, preparation as follows:
(1) pulverizes: select an amount of fruit of khosam to be ground into meal;
(2) petroleum ether extraction: by kosam seeds meal weight (kg): sherwood oil volume (L) soaked in encloses container 8～10 hours than being to add sherwood oil at 1: 8, filtered, and collected filtrate;
(3) thick oil preparation: distilation steps (2) gained filtrate, the heating recovery sherwood oil till dripless flows out, gets slightly oil of blackish green kosam seeds;
(4) refining: that the thick oil of the blackish green kosam seeds of step (3) gained is heated to 80 ℃～85 ℃, add the gac of counting 0.03～0.05g/mL drying by the thick oil volume of yellow again, stirring fully, decompression extracting in back gets yellow thick oil, the yellow thick oil that obtains is heated to 80 ℃～85 ℃, adding is by the kaolin of the thick oil volume 0.05～0.08g/mL of yellow drying, and stirring fully, decompression extracting in back gets Oleum Fructus Bruceae;
(5) purifying: will go up the Oleum Fructus Bruceae that obtains of the step logical nitrogen of 700mmHg decompression 1 hour under 115 ℃ of conditions again, pure Oleum Fructus Bruceae.
Further, making pure Oleum Fructus Bruceae bottles filling under the nitrogen condition.
The inventive method technology is simple, and is with low cost, is easy to heavy dose of production, and the pure Oleum Fructus Bruceae relative density that makes is 0.890～0.920 (20 ℃).Do not contain alkaloid, flavonoid and other non-fatty acid components after testing
(4) embodiment
The invention will be further described below in conjunction with specific embodiment:
Embodiment 1
Raw material: fruit of khosam; 60 ℃～90 ℃ AR of sherwood oil
Gac is (medicinal; 160 ℃ of baking 1h)
Kaolin (pharmaceutical grade; 160 ℃ of baking 1h)
(1) pulverize: select for use maturation, exsiccant fruit of khosam to wipe out stalk impurity, be ground into meal (20 mesh sieve), take by weighing meal 25Kg,
(2) petroleum ether extraction: add sherwood oil 200L, in encloses container, soak 9 hours (per hour fully stirring 2 times), filter, collect filtrate, add sherwood oil 150L in the kosam seeds residue, encloses container soaked 9 hours, (per hour fully stirring 2 times) collects filtrate, and it is stand-by to merge twice filtrate;
(3) thick oil preparation: distilation steps (2) gained filtrate, the heating recovery sherwood oil till dripless flows out, gets the thick oily 10L of blackish green kosam seeds;
(4) refining: that the thick oil of the blackish green kosam seeds of step (3) gained is heated to 82 ± 1 ℃, the gac 0.4Kg that adds drying again, stirring fully, decompression extracting in back gets yellow thick oily 8.8L, the thick oil that obtains is heated to 82 ± 1 ℃, add exsiccant kaolin 0.57Kg, stirring fully, decompression extracting in back gets Oleum Fructus Bruceae 7.48L;
(5) purifying: will go up the Oleum Fructus Bruceae that obtains of the step logical nitrogen of 700mmHg decompression 1 hour under 115 ℃ of conditions again, pure Oleum Fructus Bruceae volume 7.1L, the 6.5Kg that weighs, total recovery 26% makes pure Oleum Fructus Bruceae and bottles filling under the nitrogen condition.
Embodiment 2
Raw material: exsiccant fruit of khosam; 60 ℃～90 ℃ AR of sherwood oil
Gac is (medicinal; 160 ℃ of baking 1h)
Kaolin (pharmaceutical grade; 160 ℃ of baking 1h)
(3) pulverize: select for use maturation, exsiccant fruit of khosam to wipe out stalk impurity, be ground into meal (20 mesh sieve), claim to such an extent that meal is 25Kg with pulverizer,
(4) petroleum ether extraction: add sherwood oil 200L, in encloses container, soak 8 hours (per hour fully stirring 2 times), filter, collect filtrate, add sherwood oil 150L in the kosam seeds residue, encloses container soaked 8 hours, (per hour fully stirring 2 times) collects filtrate, and it is stand-by to merge twice filtrate;
(3) thick oil preparation: distilation steps (2) gained filtrate, the heating recovery sherwood oil till dripless flows out, gets the thick oily 9.6L of blackish green kosam seeds;
(4) refining: that the thick oil of the blackish green kosam seeds of step (3) gained is heated to 85 ℃, the gac 0.29Kg that adds drying again, stirring fully, decompression extracting in back gets yellow thick oily 8.2L, the thick oil that obtains is heated to 80 ℃, add exsiccant kaolin 0.66Kg, stirring fully, decompression extracting in back gets Oleum Fructus Bruceae 6.8L;
(5) purifying: will go up the Oleum Fructus Bruceae that obtains of the step logical nitrogen of 700mmHg decompression 1 hour under 115 ℃ of conditions again, pure Oleum Fructus Bruceae volume 6.12L, weigh 5.6Kg.Total recovery 22.4%
Embodiment 3
Raw material: dry, even fruit of khosam; 60 ℃～90 ℃ of sherwood oils
Gac is (medicinal; 160 ℃ of baking 1h)
Kaolin (pharmaceutical grade; 160 ℃ of baking 1h)
(1) pulverize: select for use maturation, exsiccant fruit of khosam to wipe out stalk impurity, be ground into meal (20 mesh sieve), take by weighing meal 25Kg with pulverizer,
(2) oily ether extraction: add sherwood oil 200L, in encloses container, soak 10 hours (per hour fully stirring 2 times), filter, collect filtrate, add sherwood oil 150L in the kosam seeds residue, encloses container soaked 10 hours, (per hour fully stirring 2 times) collects filtrate, and it is stand-by to merge twice filtrate;
(3) thick oil preparation: distilation steps (2) gained filtrate, the heating recovery sherwood oil till dripless flows out, gets the thick oily 10L of blackish green kosam seeds;
(4) refining: that the thick oil of the blackish green kosam seeds of step (3) gained is heated to 80 ℃, the gac 0.50Kg that adds drying again, stirring fully, decompression extracting in back gets yellow thick oily 8.5L, the thick oil that obtains is heated to 85 ℃, add exsiccant kaolin 0.425Kg, stirring fully, decompression extracting in back gets Oleum Fructus Bruceae 7.06L;
(5) purifying: will go up the Oleum Fructus Bruceae that obtains of the step logical nitrogen of 700mmHg decompression 1 hour under 115 ℃ of conditions again, pure Oleum Fructus Bruceae volume 6.7L, weigh 6.14Kg.Total recovery 24.5% makes pure Oleum Fructus Bruceae and bottles filling under the nitrogen condition.
Embodiment 4
Raw material: fruit of khosam (dry, even); 60 ℃～90 ℃ AR of sherwood oil
Gac is (medicinal; 160 ℃ of baking 1h) kaolin (pharmaceutical grade; 160 ℃ of baking 1h)
Select an amount of fruit of khosam to be ground into meal, take by weighing meal 20Kg, with described meal Petroleum ether extraction, extracting solution reclaims sherwood oil and gets the thick oily 8L of kosam seeds, again the thick oil heating of gained kosam seeds back is added the 0.64Kg gac, stir the decompression extracting of abundant back and get yellow thick oily 6.8L, add the kaolin 0.36Kg of drying again, the decompression extracting gets Oleum Fructus Bruceae 4.8L after the stirring fully; To go up under 150 ℃ of conditions, reduce pressure logical nitrogen 0.5 hour of the Oleum Fructus Bruceae that obtains of step again, must pure Oleum Fructus Bruceae 4.42L, weigh 4Kg, total recovery is 20%.
Embodiment 5～7
Raw material: fruit of khosam (dry, even); 60 ℃～90 ℃ AR gacs of sherwood oil are (medicinal; 160 ℃ of baking 1h) kaolin (pharmaceutical grade; 160 ℃ of baking 1h)
(1) pulverize: select an amount of fruit of khosam to be ground into meal,
(2) extraction: take by weighing meal 6Kg, add sherwood oil 50L and soak extraction after 8 hours, collect extracting solution, again the kosam seeds residue is extracted once more with the 30L sherwood oil, united extraction liquid reclaims sherwood oil and gets the thick oily 2.1L of kosam seeds, should be divided into 3 parts by thick oil, and get 0.7L for every part and carry out three kinds of processing condition according to the following steps and make with extra care purifying:
(3) refining: as to press temperature shown in the table 1 at the thick oil of every part of kosam seeds and add gac, stirring fully, decompression extracting in back gets yellow thick oil, the thick oil of yellow is heated to the kaolin that adds drying after the temperature as shown in table 1, stirring fully, decompression extracting in back gets Oleum Fructus Bruceae again;
(4) purifying: will go up the Oleum Fructus Bruceae that obtains of the step logical nitrogen that under condition as shown in table 1, reduce pressure again, must pure Oleum Fructus Bruceae, weigh, calculate total recovery
Testing data such as table 1 expression:
| Embodiment | 5 | 6 | 7 |
| The absorbent charcoal fine purification temperature | 60 | 80 | 100 |
| Activated carbon dosage kg | 0.105 | 0.001 | 0.001 |
| Must measure L behind the absorbent charcoal fine purification | 0.56 | 0.58 | 0.6 |
| Kaolin extraction temperature ℃ | 60 | 80 | 100 |
| Kaolin consumption kg | 0.056 | 0.012 | 0.024 |
| Refining back oil mass L | 0.45 | 0.48 | 0.51 |
| Cleansing temp ℃ | 90 | 120 | 105 |
| Logical nitrogen time h | 2 | 0.5 | 1.5 |
| Purely oilyly must measure L | 0.43 | 0.45 | 0.47 |
| Pure oil weigh (Kg) | 0.39 | 0.41 | 0.428 |
| Yield (weight %) | 19.5 | 20.5 | 21.4 |
Embodiment 8～13
Raw material: fruit of khosam (dry, even); 60 ℃～90 ℃ AR gacs of sherwood oil are (medicinal; 160 ℃ of baking 1h) kaolin (pharmaceutical grade; 160 ℃ of baking 1h) preparation process:
(1) pulverize: with the fruit of khosam decon, be ground into meal with pulverizer, take by weighing six parts of meal 2Kg, each part is one of embodiment 8～13, as follows preparation:
(2) petroleum ether extraction: each part adds sherwood oil at twice by table 2 a routine ratio, extracts after the immersion time as shown in table 2 in encloses container, filters, and collects filtrate;
(3) thick oil preparation: distilation steps (2) gained filtrate, the heating recovery sherwood oil till dripless flows out, gets slightly oil of blackish green kosam seeds;
(4) refining: as the thick oil of the blackish green kosam seeds of step (3) gained to be heated to the gac that adds drying after the temperature as shown in table 2 again by ratio, stirring fully, decompression extracting in back gets yellow thick oil, the yellow thick oil that obtains is heated to temperature as shown in table 2, press the kaolin that ratio adds drying, stirring fully, decompression extracting in back gets Oleum Fructus Bruceae;
(5) purifying: will go up the Oleum Fructus Bruceae that obtains of the step logical nitrogen that under condition as shown in table 2, reduce pressure, must pure Oleum Fructus Bruceae, bottle filling under the nitrogen condition.
Table 2:
| Embodiment | 8 | 9 | 10 | 11 | 12 | 13 |
| Sherwood oil consumption L | 12 | 18 | 15 | 15 | 16 | 16 |
| Soak time h | 6 | 12 | 9 | 9 | 8 | 8 |
| Thick oil mass L | 0.39 | 0.37 | 0.51 | 0.49 | 0.59 | 0.60 |
| Absorbent charcoal fine purification temperature ℃ | 95 | 70 | 82 | 88 | 82 | 76 |
| Activated carbon dosage kg | 0.004 | 0.06 | 0.026 | 0.015 | 0.024 | 0.048 |
| First refining back oil mass L | 0.34 | 0.32 | 0.44 | 0.45 | 0.52 | 0.55 |
| Kaolin extraction temperature ℃ | 95 | 70 | 82 | 88 | 82 | 76 |
| Kaolin consumption kg | 0.01 | 0.03 | 0.035 | 0.022 | 0.031 | 0.05 |
| Refining back oil mass L | 0.29 | 0.27 | 0.37 | 0.37 | 0.45 | 0.47 |
| Cleansing temp ℃ | 90 | 120 | 110 | 115 | 105 | 112 |
| Logical nitrogen time h | 2 | 0.5 | 1 | 1.2 | 1.2 | 1 |
| Pure oil mass L | 0.28 | 0.26 | 0.36 | 0.36 | 0.44 | 0.46 |
| Yield (weight %) | 12.5 | 12 | 16.5 | 16.5 | 20 | 21 |
The quality test of embodiment 14 pure Oleum Fructus Bruceaes
(1) assay of pure Oleum Fructus Bruceae:
A. triolein detection method: precision is measured this product 1g, puts in the 25ml measuring bottle, adds sherwood oil (60～90 ℃) and is diluted to scale, shakes up, as need testing solution.Other gets the triolein reference substance solution.According to tlc (solution that contains 4mg among the Chinese Pharmacopoeia 1ml, product solution in contrast.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia nineteen ninety-five version), draw need testing solution 1 μ l, reference substance solution 1 μ l, 2 μ l, the point of crossing is on same silica gel g thin-layer plate respectively, with sherwood oil (60～90 ℃)-vinyl acetic monomer (16: 1) is developping agent, launch, take out, dry, put and smoke to clear spot taking-up in the iodine vapor, in 105 ℃ of bakings 2～3 minutes, take out, on thin layer plate, cover the sheet glass of identical size, seal with adhesive plaster all around, scan according to tlc (an appendix VI of Chinese Pharmacopoeia nineteen ninety-five version B thin layer chromatography scanning), wavelength: λ S=400nm, λ R=650nm measures trial-product optical density integrated value and reference substance optical density integrated value, calculate, promptly.
B. the oleic acid detection method is measured according to vapor-phase chromatography (an appendix VI of Chinese Pharmacopoeia nineteen ninety-five version E)
Chromatographic condition and system suitability test are stationary phase with 5% phenyl, 95% methyl polysiloxane, and (25M * 0.25 μ m (crosslinked): column temperature is 250 ℃ to capillary column.Number of theoretical plate is pressed the oleic acid peak and is calculated, and should be not less than 2500, and the degree of doing all one can at oleic acid and internal standard substance peak should be greater than 2.
It is an amount of that correction factor mensuration is got positive palmitic acid, and accurate the title decides, and adds n-hexane dissolution and quantitatively be diluted to the solution that contains 6.2mg among every 1ml, as inner mark solution.Other gets the about 10mg of oleic acid reference substance, accurate claims surely, puts in the brown measuring bottle of 10ml, and the accurate inner mark solution 1ml that adds adds normal hexane and dissolves in right amount and be diluted to scale, shakes up.Measure 0.5 μ l and inject liquid chromatograph, the calculation correction factor.
The assay method precision takes by weighing this product 0.5g, puts during 10ml measures, and the accurate inner mark solution 1ml that adds adds normal hexane and is diluted to scale, shakes up.Measure 0.5 μ l and inject liquid chromatograph, measure, calculate, promptly.
(2) other project detects:
The c sherwood oil is got this product, with reference to Chinese Pharmacopoeia nineteen ninety-five version appendix VIII P Determination of Residual Organic Solvents assay method second method (headspace injection method) test, uses 5% phenyl methyl polysiloxane capillary column, and 45 ℃ of column temperatures contain sherwood oil and should cross 0.01%.
D moisture and volatile matter must not be crossed 1.0% (an appendix IX of Chinese Pharmacopoeia nineteen ninety-five version H first method)
E impurity must not be crossed 0.05% (an appendix IX of Chinese Pharmacopoeia nineteen ninety-five version N)
The f relative density should be 0.910～0.920 (an appendix IX of Chinese Pharmacopoeia nineteen ninety-five version N)
G ignition residue: must not cross 0.1% (an appendix IX of Chinese Pharmacopoeia nineteen ninety-five version J) and embodiment 1～13 prepared pure Oleum Fructus Bruceae be carried out quality test, result such as table 3 by the above-mentioned method of inspection:
Table 3:
| 2 | 0.916 | 0.025 | 0.12 | 0.04 | Less than 0.01% | 910 | 22.3 |
| 3 | 0.917 | 0.013 | 0.10 | 0.03 | Less than 0.01% | 930 | 21.0 |
| 4 | 0.915 | 0.020 | 0.12 | 0.03 | Less than 0.01% | 900 | 23.0 |
| 5 | 0.911 | 0.030 | 0.13 | 0.04 | Less than 0.01% | 927 | 21.2 |
| 6 | 0.913 | 0.013 | 0.10 | 0.03 | Less than 0.01% | 926 | 23.3 |
| 7 | 0.913 | 0.023 | 0.11 | 0.05 | Less than 0.01% | 930 | 23.2 |
| 8 | 0.915 | 0.031 | 0.18 | 0.04 | Less than 0.01% | 925 | 21.0 |
| 9 | 0.915 | 0.020 | 0.10 | 0.03 | Less than 0.01% | 932 | 23.6 |
| 10 | 0.914 | 0.027 | 0.17 | 0.05 | Less than 0.01% | 926 | 21.1 |
| 11 | 0.918 | 0.015 | 0.12 | 0.04 | Less than 0.01% | 930 | 23.5 |
| 12 | 0.916 | 0.020 | 0.10 | 0.03 | Less than 0.01% | 925 | 23.0 |
| 13 | 0.916 | 0.021 | 0.12 | 0.04 | Less than 0.01% | 927 | 23.0 |
Claims (9)
1. the preparation method of a pure Oleum Fructus Bruceae, comprise and be prepared as follows step: select an amount of fruit of khosam to be ground into meal, with described meal Petroleum ether extraction, extracting solution reclaims sherwood oil and gets slightly oil of kosam seeds, again the thick oil heating of gained kosam seeds back is added weight is counted the drying of 0.01～0.15g/mL with the thick oil volume of described kosam seeds gac, stirring fully, decompression extracting in back gets yellow thick oil, it is characterized in that the thicker oil of described yellow is added weight counts the kaolin of the drying of 0.02～0.10g/mL with the thick oil volume of described yellow, stirring fully, decompression extracting in back gets Oleum Fructus Bruceae; To go up under 90～120 ℃ of conditions, reduce pressure logical nitrogen 0.5～2 hour of the Oleum Fructus Bruceae that obtains of step again, must pure Oleum Fructus Bruceae.
2. the preparation method of pure Oleum Fructus Bruceae as claimed in claim 1 is characterized in that preparing as follows:
(1) pulverizes: select an amount of fruit of khosam to be ground into meal;
(2) petroleum ether extraction: by kosam seeds meal weight (kilogram): sherwood oil volume (liter) soaks in encloses container and extracts than being 1: 6～9 to add sherwood oils, filters, and collects filtrate;
(3) thick oil preparation: distilation steps (2) gained filtrate, the heating recovery sherwood oil till dripless flows out, gets slightly oil of blackish green kosam seeds;
(4) refining: that the thick oil of the blackish green kosam seeds of step (3) gained is heated to 70 ℃～95 ℃, add weight again and count the gac of the drying of 0.01～0.15g/mL with the thick oil volume of described kosam seeds, stirring fully, decompression extracting in back gets yellow thick oil, the yellow thick oil that obtains is heated to 70 ℃～95 ℃, add weight and count the kaolin of the drying of 0.02～0.10g/mL with the thick oil volume of yellow, stirring fully, decompression extracting in back gets Oleum Fructus Bruceae;
(5) purifying: will go up under 90～120 ℃ of conditions, reduce pressure logical nitrogen 0.5～2 hour of the Oleum Fructus Bruceae that obtains of step, must pure Oleum Fructus Bruceae.
3. the preparation method of pure Oleum Fructus Bruceae as claimed in claim 2 is characterized in that the described kosam seeds meal of described step (2) soaks extraction time in encloses container be 6～12 hours.
4. the preparation method of pure Oleum Fructus Bruceae as claimed in claim 3 is characterized in that the kaolinic adding weight of described step (4) counts 0.05～0.08g/mL with the thick oil volume of described yellow.
5. the preparation method of pure Oleum Fructus Bruceae as claimed in claim 4 is characterized in that the adding weight of described step (4) gac is counted 0.03～0.05g/mL with the thick oil volume of described kosam seeds.
6. as the preparation method of the described pure Oleum Fructus Bruceae of one of claim 2～5, it is characterized in that described step (2) is by kosam seeds meal weight (kilogram): sherwood oil volume (liter) adds sherwood oil than the amount that is 1: 8.
7. the preparation method of pure Oleum Fructus Bruceae as claimed in claim 6 is characterized in that described step (5) purifying: will go up under 100～115 ℃ of conditions, reduce pressure logical nitrogen 0.5～1 hour of Oleum Fructus Bruceae that the step obtains, and must pure Oleum Fructus Bruceae.
8. the preparation method of pure Oleum Fructus Bruceae as claimed in claim 7 is characterized in that preparing as follows:
(1) pulverizes: select an amount of fruit of khosam to be ground into meal;
(2) petroleum ether extraction: by kosam seeds meal weight (kilogram): sherwood oil volume (liter) soaked in encloses container 8～10 hours than being to add sherwood oil at 1: 8, filtered, and collected filtrate;
(3) thick oil preparation: distilation steps (2) gained filtrate, the heating recovery sherwood oil till dripless flows out, gets slightly oil of blackish green kosam seeds;
(4) refining: that the thick oil of the blackish green kosam seeds of step (3) gained is heated to 80 ℃～85 ℃, add weight again and count the gac of the drying of 0.03～0.05g/mL with described thick oil volume, stirring fully, decompression extracting in back gets yellow thick oil, the yellow thick oil that obtains is heated to 80 ℃～85 ℃, add weight and count the kaolin of the drying of 0.05～0.08g/mL with the thick oil volume of yellow, stirring fully, decompression extracting in back gets Oleum Fructus Bruceae;
(5) purifying: will go up the Oleum Fructus Bruceae that obtains of step logical nitrogen of 700mmHg decompression 1 hour under 115 ℃ of conditions, pure Oleum Fructus Bruceae.
9. the preparation method of pure Oleum Fructus Bruceae as claimed in claim 7 is characterized in that describedly making pure Oleum Fructus Bruceae and bottling filling under the nitrogen condition.
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| CN1314789C true CN1314789C (en) | 2007-05-09 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100349582C (en) * | 2005-12-06 | 2007-11-21 | 广东大光药业有限公司 | Oil seed bruceae lyophilized powder for injection and its preparing method |
| CN101053579B (en) * | 2006-04-14 | 2010-09-08 | 首都医科大学附属北京友谊医院 | Application of brucea fruit oil nanometer emulsion in preparing gastrointestinal mucosa protective agent |
| CN101791282B (en) * | 2009-12-29 | 2013-09-25 | 广东药学院 | Beauty lotion and preparation method and application thereof |
| CN101804085B (en) * | 2010-05-06 | 2011-04-20 | 沈阳药大药业有限责任公司 | Brucea javanica oil and pharmaceutical composition containing the same and preparation method thereof |
| CN102772454B (en) * | 2012-05-31 | 2014-12-17 | 浙江中医药大学 | Brucea javanica oil dry emulsion capsule and preparation method thereof |
| CN105623841B (en) * | 2015-12-24 | 2016-12-07 | 华润三九（南昌）药业有限公司 | Oleum Fructus Bruceae extraction and purification process |
| CN112494525B (en) * | 2017-05-08 | 2022-06-03 | 沈阳药大雷允上药业有限责任公司 | Oleum fructus Bruceae, pharmaceutical composition containing oleum fructus Bruceae, and its preparation method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1070829A (en) * | 1992-09-26 | 1993-04-14 | 王志理 | Xilu eliminating wart medicine liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1070829A (en) * | 1992-09-26 | 1993-04-14 | 王志理 | Xilu eliminating wart medicine liquid |
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