CN101406521A - Use of Magnolia grandiflora leaf volatile oil in pharmacy - Google Patents
Use of Magnolia grandiflora leaf volatile oil in pharmacy Download PDFInfo
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- CN101406521A CN101406521A CNA2007101756567A CN200710175656A CN101406521A CN 101406521 A CN101406521 A CN 101406521A CN A2007101756567 A CNA2007101756567 A CN A2007101756567A CN 200710175656 A CN200710175656 A CN 200710175656A CN 101406521 A CN101406521 A CN 101406521A
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- volatile oil
- magnolia
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- gradiflora
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Abstract
The invention relates to pharmaceutic application of southern magnolia leaf volatile oil. The southern magnolia leaf volatile oil can be obtained by extraction of southern magnolia leaves by the prior method for extracting and separating volatile oil. As proved by pharmacological research, the southern magnolia leaf volatile oil has good functions of antibacterium and bacteriostasis, has stronger abirritation, and can be used for preparing an antibacterial and analgesic medicine.
Description
Technical field
The present invention relates to the purposes of leaf of Magnolia gradiflora volatile oil, relate in particular to its application on antibiotic, the analgesic of preparation.
Background technology
YULAN is one of taxon important in Magnoliaceae (Magnoliaceae) plant, is a class fast-growing woods, special good species with economic forest, forests for water and soil conservation and the town and country landscape ecological forest, and development and exploitation prospect are arranged very much.The dry flower of Magnoliacea plant Flos Magnoliae (Magnolia biondii Pamp.), YULAN (Magnolia denudate desr.) or Flos Magnoliae (Magnolia sprengeri Pamp.) is the medicinal part of Chinese medicine Flos Magnoliae, is used for treating cold symptoms such as headche due to wind-cold, nasal obstruction clinically.Document (Zhao Liqin. Y biondii(Pamp)D.L.Fu. ter penoids and bioactivity research thereof progress. the time precious traditional Chinese medical science traditional Chinese medicines [J] .2005.16 (4): 298-230) record, be rich in ter penoids in the YULAN, be mainly monoterpene and sesquiterpene and containing oxygen derivative thereof.(Chen Xingrong such as Chen Xingrong, Deng. the evergreen magnolia chemical constitution study. Chinese crude drug [J] .2000,13 (3): 159-160) grade is carried out chemical constitution study to evergreen magnolia, therefrom separates and has differentiated three sesquiterpene lactones compounds, is respectively syringaresinol, costunolide and parthenolide.Document (Two newgermacranolides from Magnolia gradiflora.J.Asian Nat Prod Res.2001,3 (2): 95-102) reported isolating sesquiterpene lactones compounds from southern magnolia, comprising lactone compounds such as-Alpha-hydroxy-dihydro parthenolide, parthenolide, constuslactones.
Summary of the invention
To the research of YULAN leaf volatile ingredient, still few at present, especially its application in pharmacy, food additive, spice.
One of purpose of the present invention provides the application of YULAN leaf volatility active component in pharmacy, especially the application in antibiotic, analgesic.
The present invention is a raw material with the YULAN leaf volatile oil, it can be developed to suitable antibiotic, analgesia preparation as acceptable carrier or pharmaceutic adjuvant in active component and the pharmacy, as injection, hard capsule, soft capsule, drop pill, tablet, granule, powder, oral liquid, emulsion, liposome etc.
YULAN leaf volatile oil raw material of the present invention can use separately, also can mix with other raw material to use and make required dosage form.
Contain various plants spice in the leaf of Magnolia gradiflora, as phellandrene, camphene, selinene, the sub-alkene of β-newcomer etc., they all are widely used in perfume industry, cosmetics and the food, and the value in essence is important day by day.Therefore, leaf of Magnolia gradiflora removes and can be used for preparing antibiotic, analgesic China and foreign countries, also can be used in food additive, cosmetics, the spice.
Among the present invention, the method that leaf of Magnolia gradiflora volatile oil adopts steam distillation, solvent extraction method or supercritical extraction etc. commonly used to be suitable for suitability for industrialized production is prepared.The leaf of Magnolia gradiflora volatile oil that obtains is faint yellow, mainly contain germacrene-D (Gemacrene-D), the purple triolefin (Santolina triene) of wingceltis, caryophyllene (Caryophyllene), 3,7-dimethyl-1,3,7 triolefins (1,3,7-Octatriene-3,7-dimehtyl-), camphene (Camphene), pinene (Pinene), phellandrene (Phellandrene), D-limonene (D-Limonene), alpha-terpineol (α-terpineol), thujopsene (Thujopesene), selinene, α-farnesene (α-Farnesene), nerol etc., account for more than 90% of total oil, the oil content of leaf of Magnolia gradiflora is 0.25%-0.40%, and promptly every 100g crude drug contains volatile oil 0.35-0.5mL.
The scheme that above-mentioned steam distillation extracts volatile oil mainly is to separate volatile oil by oil water separator, the steps include: to calculate by weight, get leaf of Magnolia gradiflora 1-20 part, add water 5-200 part, be dipped to earlier, vapor distillation 3-8 hour, temperature is controlled at 85-105 ℃, temperature can be provided with height when initial, after waiting to seethe with excitement, suitably turns down temperature, to keep water is little boiling, carry out oil-water separation, obtain moisture leaf of Magnolia gradiflora volatile oil, moisture volatile oil is with extracted with diethyl ether, extracted with diethyl ether partly adds anhydrous sodium sulfate drying (more than 24 hours), filter, remove water, boil off ether, can obtain leaf of Magnolia gradiflora volatile oil.
Above-mentioned solvent extraction method, the steps include: to get leaf of Magnolia gradiflora 1-20 part, add organic solvent-normal hexane or cyclohexane extraction 6-120 weight portion, carry out reflux, extract,, temperature is controlled at 50-70 ℃, backflow 2-3 hour, when treating that the backflow temperature is reduced to room temperature, emit backflow, reclaim organic solvent, can obtain the volatile oil crude product; In crude product, add dehydrated alcohol 0.01-0.1 weight portion, with the volatile oil crude product from minute mixing, place in-20 ℃ of refrigerators, more than the 24h, muddy liquid is removed by filter, continue to place and repeat this step in the refrigerator, till the liquid clarification, the alcoholic solution that will contain volatile oil concentrates, and can obtain leaf of Magnolia gradiflora volatile oil.
Above-mentioned described supercritical extraction the steps include: to get leaf of Magnolia gradiflora, is ground into the flour that particle diameter is 0.5-1mm, and the pressure of extraction axe is 10-30Mpa, and temperature is 20-50 ℃, carries out supercritical CO
2Extraction, the extraction time is 30-90 minute, from extracting the CO that axe comes out
2Enter piece-rate system, the flash trapping stage temperature is 35-50 ℃, and pressure is 15-25Mpa; The secondary separation temperature is 20-30 ℃, and pressure is 4-8Mpa, obtains leaf of Magnolia gradiflora volatile oil, CO
2Flow velocity is 10-20L/h, the CO that separates
2Recycling with refrigeration system pressurization back after filtration again.
Essence for a better understanding of the present invention below illustrates the present invention's application the antibiotic and analgesic in preparation from the antibacterial and analgesic experiment of leaf of Magnolia gradiflora volatile oil.
One, external bacteriostatic experiment
1, strain Klebsiella oxytoca, Salmonella enteritidis, shigella dysenteriae, escherichia coli, staphylococcus epidermidis, staphylococcus aureus.
2, culture medium M-H broth bouillon adds 0.3% agar, makes semisolid culturemedium.
3, the mensuration of MIC adopt micro-agar dilution measure MIC (Xu Shuyun. pharmacological experiment methodology [M]. Beijing: People's Health Publisher .1985,1066-1070).2% southern magnolia oil solution (emulsion) is done 1: the 2-128 doubling dilution, get 20 μ l and add in the culture hole, add each bacterium liquid (about 10 more respectively with the bouillon agar dilution
7/ ml) 200 μ l, mixing is cultivated 24h in 37 ℃, and repeated experiments 1 time the results are shown in Table 1.
The minimum inhibitory concentration experiment of table 1 leaf of Magnolia gradiflora volatile oil
Annotate: the no bacterial growth of "-" expression, "+" expression has bacterial growth.
External bacteriostatic experiment shows, after 2% leaf of Magnolia gradiflora volatile oil is done 1/4 times of dilution, Klebsiella oxytoca, Salmonella enteritidis, shigella dysenteriae, escherichia coli, staphylococcus epidermidis, staphylococcus aureus all there is significant bacteriostasis, after doing 1/8 times of dilution, shigella dysenteriae, staphylococcus epidermidis are still had remarkable antibacterial action, and stronger than 1% berberine.The minimum inhibitory concentration that leaf of Magnolia gradiflora volatile oil is described is that 2% southern magnolia solution is done 1/4 times of dilution, i.e. the solution of 0.5% concentration (V/V).
Two, antibacterial experiment in the body
1. inoculated bacteria is in the 10ml nutrient broth before the experiment, and hatching 24h is bacterium stock solution, continue to make desired concn with 5% high activity dried yeast, with preliminary experiment be select make mouse death rate reach the bacterium liquid of 80%-100% (colibacillary dilution factor is 10
-1, the dilution factor of staphylococcus aureus is 10
-2) as infection dosage, the mice random packet, 10 every group, male and female half and half, each is organized mouse peritoneal and injects each bacterium liquid 0.5ml infection; Give the leaf of Magnolia gradiflora volatile oil liquid (volatile oil concentration is 2% (V/V)) of various dose, lumbar injection 0.03ml/kg and 0.015ml/kg, irritate stomach 0.1ml/kg and 0.05ml/kg, the blank group is given normal saline, matched group lumbar injection 40U/kg gentamycin, administration second day, statistics was respectively organized dead mouse quantity in the 7th day, the results are shown in Table 2.
Bacteriostatic experiment (n=10) in the body of table 2 leaf of Magnolia gradiflora volatile oil
2. acute toxicity testing is got the mice random packet, and lumbar injection and filling stomach give leaf of Magnolia gradiflora volatile oil respectively, as a result lumbar injection LD
50Be 0.75mL/kg, irritate stomach LD
50Be 4.86mL/kg.
Three, to the influence of mice analgesic activity
Make up a prescription: gained southern magnolia volatile oil is made into desired concn with 5% tween 80.
The healthy Kunming mouse of mice hot plate method, female, 18～22g, put into (55 ± 0.5) ℃ water-bath beaker in preceding 1 day in experiment, record is from putting into the time that metapedes occurs licking, i.e. pain threshold, get pain threshold and be 40 of the qualified mices of 5～30s, be divided into 4 groups at random, 10 every group.Fasting 16h before the experiment can't help water.Survey pain threshold before the administration again one time, as normal pain threshold.Positive controls lumbar injection aspirin 10mg/kg, 5% tween 80 solution of negative control group lumbar injection equal-volume (0.2mL/20g), drug study group administration volatile oil 0.15,0.3ml/kg, survey 15,30,60,90min pain threshold, relatively pain threshold size before and after the administration.The results are shown in Table 3.
The influence that table 3 leaf of Magnolia gradiflora volatile oil is reacted the mice threshold of pain (x ± s)
Compare with negative control group,
*P＜0.01,
*P＜0.05
Experimental result shows that southern magnolia volatile oil has significant analgesia role to mice, compares significant difference (P＜0.01) with negative control group.
The specific embodiment
Following embodiment is in order to further specifying the present invention, but do not limit the scope of the invention thus.
Embodiment 1
Get southern magnolia fresh leaf 500g, add 10 times of water gagings, vapor distillation 5 hours separates moisture volatile oil with oil water separator, and moisture volatile oil is used the anhydrous sodium sulfate dehydration dried overnight after repeatedly extracting on a small quantity with ether, and filtering and concentrating obtains southern magnolia volatile oil.Volatile oil becomes faint yellow transparence liquid, and peat-reek is arranged, and oil yield is 0.39% (ml/100g), promptly gets southern magnolia volatile oil 1.95mL.
Carry out GC-MS after the dissolving of volatile oil minimum of chloroform and analyze, the results are shown in Table 4.Chromatographic condition: quartz capillary column HP-5MS (30m * 0.25mm * 0.25 μ m), carrier gas is a helium, post flow 1ml/min is warming up to 260 ℃; Mass spectrum condition: EI ionization source, ionizing energy 70eV, 230 ℃ of ion source temperatures, sweep limits 30-500amu, sample size 1.0 μ L, split ratio 10: 1.
Table 4 leaf of Magnolia gradiflora volatile oil component analysis result (steam distillation)
Embodiment 2
Get leaf of Magnolia gradiflora 1000g, be ground into the coarse powder that particle diameter is about 0.5-1.0mm, put in the extraction axe, extraction axe pressure is 35Mpa, and temperature is 35 ℃; The flash trapping stage temperature is for being 40 ℃, and pressure is 15Mpa, and the secondary separation temperature is 20 ℃, and pressure is 6Mpa.Supercritical fluid static immersing raw material 1h, equipment stablize laggard action attitude extraction, collect product by receptor.Get leaf of Magnolia gradiflora volatile oil 4.2mL at last, volatile oil becomes light yellow transparent liquid, and peat-reek is arranged, and oil yield is 0.42% (ml/100g).
Volatile oil carries out the GC-MS analysis after adding the minimum of chloroform dissolving, and similar water steam distillation as a result is similar.
Claims (1)
1, the application of leaf of Magnolia gradiflora volatile oil in antibiotic, the analgesic of preparation.
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| CNA2007101756567A CN101406521A (en) | 2007-10-10 | 2007-10-10 | Use of Magnolia grandiflora leaf volatile oil in pharmacy |
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| CNA2007101756567A CN101406521A (en) | 2007-10-10 | 2007-10-10 | Use of Magnolia grandiflora leaf volatile oil in pharmacy |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113462475A (en) * | 2020-03-31 | 2021-10-01 | 广东省禾基生物科技有限公司 | Extraction method and application of yulan magnolia leaf cell water and yulan magnolia leaf essential oil |
-
2007
- 2007-10-10 CN CNA2007101756567A patent/CN101406521A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113462475A (en) * | 2020-03-31 | 2021-10-01 | 广东省禾基生物科技有限公司 | Extraction method and application of yulan magnolia leaf cell water and yulan magnolia leaf essential oil |
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Open date: 20090415 |