CN106187983B - A kind of mouth xanthones compounds and its preparation method and application - Google Patents
A kind of mouth xanthones compounds and its preparation method and application Download PDFInfo
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- CN106187983B CN106187983B CN201610536311.9A CN201610536311A CN106187983B CN 106187983 B CN106187983 B CN 106187983B CN 201610536311 A CN201610536311 A CN 201610536311A CN 106187983 B CN106187983 B CN 106187983B
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- C07—ORGANIC CHEMISTRY
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- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/78—Ring systems having three or more relevant rings
- C07D311/80—Dibenzopyrans; Hydrogenated dibenzopyrans
- C07D311/82—Xanthenes
- C07D311/84—Xanthenes with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached in position 9
- C07D311/86—Oxygen atoms, e.g. xanthones
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- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
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Abstract
The invention discloses a kind of mouth xanthones compounds（Ⅰ）And its preparation method and application, the mouth xanthones compounds are from black purple Swertia patens（Swertia atroviolacea）In it is isolated, its molecular formula is C17H16O5, it is named as：The methyl mouth mountain ketone of 6 (2 methylol) 1,7 dimethoxy 3, the entitled methyl xanthone of 6 (2 hydroxymethyl) 1,7 dimethoxy 3 of English, has following structural formula：（Ⅰ）The preparation method of the mouth xanthones compounds, be using black purple Swertia patens as raw material, extracted through medicinal extract, silica gel column chromatography, high pressure liquid chromatography it is isolated.The mouth xanthones compounds have preferable bacteriostasis through active testing.The compounds of this invention structure is novel, and has preferable antibacterial activity, can be as the lead compound prepared in standby antibacterials.The compound is used for cigarette tipping paper, can eliminate or reduce bacteria breed and the possibility of breeding in cigarette tipping paper.
Description
Technical field
The invention belongs to natural product chemistry technical field, and in particular to extraction obtains one kind first from black purple Swertia patens
Mouth xanthones compounds and its preparation method and application.
Background technology
Swertia（Swertia）It is a category under Gentianaceae, about 170 kinds of the whole world, China has more than 80 to plant, main distribution
In Yunnan, Sichuan and other places.In China, the platymiscium is used as medicine with a long history, medicinal to have 35 kinds, has clearing heat secreting bile, removing dampness and detoxicating etc.
Effect, it is usually used in treating the diseases such as acute Jaundice Jaundice, osteomyelitis.The chemical composition of the platymiscium is enriched, and mainly has a mouthful mountain
The compounds such as ketone, flavones, iridoid, triterpene and alkaloid.Black purple Swertia patens（Swertia atroviolacea）For river deer tooth
Lepidium herbaceos perennial, it is born in the m of height above sea level 3400~4575 patana, more tor tops or rock seam, is Yunnan Province
The peculiar kind in Diqingzangzu area.
Mouth mountain ketone also known as dibenzopyrans ketone, its derivative are widely present in nature, are the important of medicinal plant
One of active ingredient.Because mouth mountain ketones derivant is that have Fen Xing functional groups on three rings of linear array, mostly with rich
Rich bioactivity and medical value；Xanthone derivative has extensive physiology and pharmacological activity, has antitumor, guarantor
Shield heart blood vessel, the pharmacological actions such as blood glucose, anti-oxidant, antibacterial are reduced, but many pharmacological mechanisms are still in the research and probe stage,
So that its pharmacological activity and its being received much attention with the research of configuration relationship., can in order to study the structure-activity relationship of this kind of compound
More mouth xanthones compounds are further researched and developed, therefrom find effective lead compound and active group.This hair
Related report is not yet seen in bright isolated from black purple Swertia patens a kind of new mouth xanthones compounds, the compound
Road, it is worth mentioning at this point that the compound has significant antibacterial activity.
The content of the invention
The first object of the present invention is to provide a kind of new mouth xanthones compounds；Second purpose is to provide the mouth
The preparation method of xanthones compounds；3rd purpose is in the answering in antibacterials are prepared in the offer mouth xanthones compounds
With.
The first object of the present invention is achieved in that described mouth xanthones compounds are separated from black purple Swertia patens
Obtain, its molecular formula is C17H16O5, there is following structural formula：
The compound is named as：6- (2- methylols) -1,7- dimethoxys -3- methyl-mouth mountain ketone, the entitled 6- of English
(2- hydroxymethyl) -1,7-dimethoxy-3-methyl- xanthone, it is light yellow gum thing.
The second object of the present invention is achieved in that the preparation method of the mouth xanthones compounds, is with black purple river deer
Tooth dish is raw material, is extracted through medicinal extract, silica gel column chromatography, high pressure liquid chromatography step, is specially：
A, medicinal extract extracts:Using black purple Swertia patens as raw material, black purple Swertia patens are crushed or are cut into segment, use organic solvent
The h of 24 h~72 is soaked, is extracted 3 ~ 5 times, merges extract solution, filtering, is concentrated under reduced pressure into medicinal extract；
B, silica gel column chromatography：Medicinal extract carries out silica gel column layer with 160~300 mesh silica gel dry column-packings of the weight than 2~4 times of amounts
Analysis；Gradient elution is carried out with chloroform-acetone solution, merges identical part, each several part eluent is collected and concentrates；
C, high pressure liquid chromatography isolates and purifies：The 7 of step B eluent:3 parts are further separated pure with high pressure liquid chromatography
Change and produce required mouth xanthones compounds.
The structure for the mouth xanthones compounds that method described above is prepared is to identify to come by the following method：
The compounds of this invention is light yellow gum thing；High resolution mass spectrum (HRESIMS) provides quasi-molecular ion peakm/z
323.0887 [M+Na]+(calculated value 323.0895).With reference to1H and13 C H NMR spectroscopies provide a molecular formula C17H16O5, insatiable hunger
It is 10 with degree.Ultraviolet spectra has absorption maximum at 335,254 and 210 nm, it was demonstrated that aromatic ring structure in compound be present；It is red
External spectrum data, which are also confirmed that in compound, has hydroxyl (3415 cm-1), carbonyl (1652 cm-1) and aromatic ring 1610,1524,
1465 cm-1) functional group.Compound1H and13C NMR data (table -1), which are shown in compound, 17 carbon and 16 hydrogen letters
Number, including the quaternary mouth mountain ketone skeletons of a 1,3,6,7- [Ind. Crop. Prod., 58, 125 (2014)](C-1
~ C-9, C-4a, C-8a ~ C10a；H-2, H-4, H-5 and H-8), a methylol (C-1 '；H2- 1 '), substitute on an aromatic ring
Methyl (C-2 ' and H3- 2 '), 2 methoxyl groups (δ H56.0 q and 56.3 q；3.81 s and 3.86 are s).Deposited in compound
In H2-1′ (δH4.64) and C-5 (δ C 119.4)、C-6 (δ C 143.4)、C-7 (δ C157.6), and H-5 (δ H
6.97) and C-1 ' (δ C58.9) HMBC is related (Fig. 3), it can be verified that methylol is substituted in the C-6 positions of compound.According to H3-
2′ (δH2.39) and C-2 (δ C 112.4)、C-3 (δ C 147.4)、C-4 (δ C108.9) HMBC is related, it can be verified that should
Methyl is substituted in the C-3 positions of compound.Two methoxy substitutions can be by two methoxyl group hydrogen (δ in C-1 and C-7H 3.81 and
3.86) respectively with C-1 (δ C160.4) and C-7 (δ C157.6) HMBC correlations are confirmed.Typical matter in compound
Subsignal [δ H7.08 d (2.2), 6.85 d (2.2), 6.97 s, 7.34 s] also support that mouth mountain ketone B rings of the invention are
6,7- bis- substitute, and C rings are that 1,3- bis- substitutes.So far the structure of the compounds of this invention is determined, Compound nomenclature is 6- (2- hydroxyls
Methyl) -1,7- dimethoxys -3- methyl-mouth mountain ketone.
Infrared, the ultraviolet and mass spectrometric data of compound：UV (methanol),λ max (log ε) 210 (4.02)、254
(3.57), 335 (3.42), IR (pressing potassium bromide troche)ν max 3415、3079、2932、1652、1610、1524、1465、
1357、1268、1162、1078、864 cm-1；、ESI-MS (positive ion mode)m/z 323 [M+Na]+; HR-ESI-MS
(positive ion mode)m/z [M + Na]+323.0887 (calculated value 323.0895, C17H16NaO5)。
The compound of table -1.1H NMR and13C NMR data (solvent C5D5N)
| No. | d C | d H (m, J, Hz) | No. | d C | d H (m, J, Hz) |
| 1 | 160.4 s | 4a | 154.6 s | ||
| 2 | 112.4 d | 7.08 d (2.2) | 8a | 114.8 s | |
| 3 | 147.4 s | 9a | 110.4 s | ||
| 4 | 108.9 d | 6.85 d (2.2) | 10a | 148.9 s | |
| 5 | 119.4 d | 6.97 s | 1′ | 58.9 t | 4.64 s |
| 6 | 143.4 s | 2′ | 24.3 q | 2.39 s | |
| 7 | 157.6 s | 1-OMe | 56.0 q | 3.81 s | |
| 8 | 111.9 d | 7.34 s | 7-OMe | 56.3 q | 3.86 s |
| 9 | 176.9 s |
The third object of the present invention is achieved in that described mouth xanthones compounds answering in antibacterials are prepared
With.
Application of the described mouth xanthones compounds in antimicrobial packaging is prepared.
The compounds of this invention is separated from black purple Swertia patens first, passes through nuclear magnetic resonance and measuring method of mass spectrum
It is defined as a mouthful xanthones compounds, and characterizes its concrete structure.Antimicrobial Screening is carried out to the compound, it is to golden yellow
Color staphylococcus, Escherichia coli, angstrom uncommon bacterium, hay bacillus, proteus etc. have significant activity,.The compound is through safety
Property evaluation, show it is nontoxic to animal, it is safe to use.
The compound is applied in cigarette tipping paper, is compared with control, and the tipping paper detection for adding this compound is thin
Bacterium sum, coliform, staphylococcus aureus, Pseudomonas aeruginosa, hemolytic streptococcus, total number of fungi substantially reduce；To large intestine
Bacillus (ATCC25922), the bacteriostasis rate of staphylococcus aureus (ATCC6538) entirely reach more than 88.3%, can reduce or
Elimination cigarette tipping paper and bacteria breed and the possibility of breeding in storage process, in addition, in smoking property of cigarette, transmittance process
In, the antibacterial action also can play inhibitory action to the contaminated microorganism of tipping paper on Cigarette.
Compared with prior art, the present invention has advantage following prominent：(1) raw materials of compound of the invention is easy to get, and extracts
Method is simple, can be easily separated to obtain；Molecular structure is also simple, easily realizes artificial synthesized.(2) employ conventional column chromatography and
The preparation method that high performance liquid chromatography combines, compound preparation manipulation flow is simple, and the compounds of this invention purity obtained is high,
Follow-up industrialized production is easily realized.(3) the compounds of this invention is nontoxic to animal, safe to use, shows good antibacterial
Activity, more than 88.3% is entirely reached to the bacteriostasis rate of Escherichia coli, staphylococcus aureus etc.；Applied to cigarette tipping paper, energy
It is enough that inhibitory action is played to the contaminated microorganism of cigarette tipping paper.Cigarette tipping paper directly exists with oral contact, the compound
Use in cigarette tipping paper can avoid cigarette suck, microbial contamination in transmittance process, effectively increase cigarette
Health and security.
Brief description of the drawings
Fig. 1 is the carbon-13 nmr spectra of mouth xanthones compounds compound of the present invention；
Fig. 2 is the proton nmr spectra of mouth xanthones compounds compound of the present invention；
Fig. 3 is that the main HMBC of mouth xanthones compounds compound of the present invention is related.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples, but not in any way to the present invention
It is any limitation as, based on present invention teach that any conversion or improvement made, each fall within protection scope of the present invention.
Unless otherwise indicated, the percentage employed in the present invention is mass percent.
Mouth xanthones compounds of the present invention, it is isolated from black purple Swertia patens, its molecular formula is C17H16O5,
It is named as：6- (2- methylols) -1,7- dimethoxys -3- methyl-mouth mountain ketone, the entitled 6- (2-hydroxymethyl) of English -
1,7-dimethoxy-3-methyl-xanthone, there is following structural formula：
The preparation method of mouth xanthones compounds of the present invention, it is using black purple Swertia patens as raw material, extracted through medicinal extract,
Silica gel column chromatography, high pressure liquid chromatography step, it is specially：
A, medicinal extract extracts:Using black purple Swertia patens as raw material, black purple Swertia patens are crushed or are cut into segment, use organic solvent
The h of 24 h~72 is soaked, is extracted 3 ~ 5 times, merges extract solution, filtering, is concentrated under reduced pressure into medicinal extract；
B, silica gel column chromatography：Medicinal extract carries out silica gel column layer with 160~300 mesh silica gel dry column-packings of the weight than 2~4 times of amounts
Analysis；Gradient elution is carried out with chloroform-acetone solution, merges identical part, each several part eluent is collected and concentrates；
C, high pressure liquid chromatography isolates and purifies：The 7 of step B eluent:3 parts are further separated pure with high pressure liquid chromatography
Change and produce required mouth xanthones compounds.
The organic solvent of the step A is 80%~100% methanol or ethanol, 60%~90% acetone.
The weight ratio of the step A organic solvent and black purple Swertia patens is 2~4:1；
The pure methanol or pure second that medicinal extract is measured before through silica gel column chromatography rough segmentation with weight than 1.5~3 times in the step B
After alcohol or pure acetone dissolving, with 80~100 mesh silica gel mixed samples of the weight than 0.8~1.2 times.
The volume proportion of chloroform-acetone solution is 1 in the step B:0、20:1、9:1、8:2、7:3、6:4、1:1 and 1:
2。
It is using the mm of 21.2 mm × 250 5 that the step C mesohigh liquid chromatogram, which isolates and purifies,μM C18Chromatogram
Post, flow velocity are 20 mL/min, and mobile phase is 50% methanol, and UV-detector Detection wavelength is 335 nm, each sample introduction 200μ
L, 22.6 min chromatographic peak is collected, is evaporated after repeatedly adding up.
Compound after the step C mesohigh liquid chromatogram isolates and purifies is dissolved with pure methanol again, then with pure methanol
For mobile phase, separated with gel filtration chromatography, further to isolate and purify.
The application of the present invention is application of the mouth xanthones compounds in antibacterials are prepared.
Application of the described mouth xanthones compounds in antimicrobial packaging is prepared.
Application of the described mouth xanthones compounds in antibacterial volume cigarette tipping paper is prepared.
Black purple Swertia patens of the present invention are not limited by area and kind, the present invention can be realized, below with source
In the black purple Swertia patens raw tobacco material of Yunnan different sources, the present invention will be further described：
Embodiment 1
Tobacco sample derives from Lijiang, yunnan.Black purple Swertia patens are sampled into 2.0 kg crushing to extract 5 times with 95% methanol,
24 h of extraction every time, extract solution merge, and filtering, are concentrated under reduced pressure into medicinal extract, obtain the g of medicinal extract 105.What medicinal extract weight was measured than 2.0 times
Silica gel column chromatography is carried out, is used with the 120 g thick silica gel mixed sample of 100 mesh, 0.6 kg 160 mesh silica gel dress post after pure methanol dissolving
Volume proportion is 1:0、20:1、9:1、8:2、7:3、6:4、1:1、1:2 chloroform-acetone gradient elution, TLC monitorings merge identical
Part, obtain 8 parts, wherein volume proportion is 7:3 chloroform-acetone elution fraction is pacified prompt logical sequence 1,100 half and prepared efficiently
Liquid chromatogram separates, using 50% methanol as mobile phase, Zorbax SB-C18 (21.2 × 250 mm, 5 μm) to prepare post be solid
Determine phase, flow velocity is 20 ml/min, and UV-detector Detection wavelength is 335 nm, each μ L of sample introduction 200, collects 22.6 min's
Chromatographic peak, it is evaporated after repeatedly adding up；Products therefrom is dissolved with pure methanol again, then using pure methanol as mobile phase, uses Sephadex
LH-20 gel filtration chromatographies separate, and produce the noval chemical compound.
Embodiment 2
Black purple Swertia patens are sampled 3.5 kg choppings, with 95% second by black purple Swertia patens sample source in Shangri-La, Yunnan Province
Alcohol extracting 4 times, 48 h are extracted every time, extract solution merges, and filtering, is concentrated under reduced pressure into medicinal extract, obtains the g of medicinal extract 250.Medicinal extract weight
Than the thick silica gel mixed sample of 80 mesh after the pure methanol dissolving of 2.0 times of amounts with 250 g, 1.2 kg 200 mesh silica gel dress post carries out silica gel
Column chromatography, it is 1 with volume proportion:0、20:1、9:1、8:2、7:3、6:4、1:1、1:2 chloroform-acetone gradient elution, TLC prisons
Survey and merge identical part, obtain 8 parts, wherein volume proportion is 7:3 chloroform-acetone elution fraction pacifies prompt logical sequence 1100
Half preparative high-performance liquid chromatographic separates, using 50% methanol as mobile phase, Zorbax SB-C18 (21.2 × 250 mm, 5 μ
M) it is stationary phase to prepare post, and flow velocity is 20 ml/min, and UV-detector Detection wavelength is 335 nm, each μ L of sample introduction 200, is received
Collect 22.6 min chromatographic peak, be evaporated after repeatedly adding up；Products therefrom is dissolved with pure methanol again, then using pure methanol as flowing
Phase, separated with Sephadex LH-20 gel filtration chromatographies, produce the noval chemical compound.
Embodiment 3
Black purple Swertia patens are sampled 5 kg and crushed, used with 75% acetone super by black purple Swertia patens sample source in Yunnan Wei Xi
Sound extracts 3 times, extracts 72h every time, and extract solution merges, and filtering, is concentrated under reduced pressure into medicinal extract, obtains the g of medicinal extract 380.Medicinal extract weight ratio
After the pure methanol dissolving of 1.6 times of amounts silicagel column is carried out with the 400 g thick silica gel mixed sample of 90 mesh, 2.4 kg 180 mesh silica gel dress post
Chromatography, it is 1 with volume proportion:0、20:1、9:1、8:2、7:3、6:4、1:1、1:2 chloroform-acetone gradient elution, TLC monitorings
Merge identical part, obtain 8 parts, wherein volume proportion is 7:3 chloroform-acetone elution fraction pacifies prompt logical sequence 1,100 half
Preparative high-performance liquid chromatographic separates, using 50% methanol as mobile phase, Zorbax SB-C18 (21.2 × 250 mm, 5 μ
M) it is stationary phase to prepare post, and flow velocity is 20 ml/min, and UV-detector Detection wavelength is 335 nm, each μ L of sample introduction 200, is received
Collect 22.6 min chromatographic peak, be evaporated after repeatedly adding up；Products therefrom is dissolved with pure methanol again, then using pure methanol as flowing
Phase, separated with Sephadex LH-20 gel filtration chromatographies, produce the noval chemical compound.
Embodiment 4
Compound prepared by Example 1, is light yellow gum thing；
Assay method is：With nuclear magnetic resonance, structure is identified with reference to other spectroscopic techniques.
High resolution mass spectrum (HRESIMS) provides quasi-molecular ion peakm/z 323.0887 [M+Na]+(calculated value
323.0895).With reference to1H and13 C H NMR spectroscopies provide a molecular formula C17H16O5, degree of unsaturation 10.Ultraviolet spectra 335,
There is absorption maximum at 254 and 210 nm, it was demonstrated that aromatic ring structure in compound be present；Ir data is also confirmed that in compound
Hydroxyl (3415 cm be present-1), carbonyl (1652 cm-1) and the cm of aromatic ring 1610,1524,1465-1) functional group.Compound1H
With13C NMR data (table -1), which are shown in compound, 17 carbon and 16 hydrogen signals, including a 1,3,6,7- tetra- substitutes
Mouth mountain ketone skeleton [Ind. Crop. Prod, 58,125 (2014)] (C-1 ~ C-9, C-4a, C-8a ~ C10a；H-2, H-
4, H-5 and H-8), a methylol (C-1 '；H2- 1 '), the nuclear substituted methyl of virtue (C-2 ' and a H3- 2 '), 2 first
Epoxide (δ H56.0 q and 56.3 q；3.81 s and 3.86 are s).H in compound be present2-1′ (δH4.64) and C-5 (δ C
119.4)、C-6 (δ C 143.4)、C-7 (δ C157.6), and H-5 (δ H6.97) and C-1 ' (δ C58.9) HMBC
Related (Fig. 3), it can be verified that methylol is substituted in the C-6 positions of compound.According to H3-2′ (δH2.39) and C-2 (δ C
112.4)、C-3 (δ C 147.4)、C-4 (δ C108.9) HMBC is related, it can be verified that the methyl is substituted in the C-3 of compound
Position.Two methoxy substitutions can be by two methoxyl group hydrogen (δ in C-1 and C-7H 3.81 and 3.86) respectively with C-1 (δ C
160.4) and C-7 (δ C157.6) HMBC correlations are confirmed.Typical proton signal in compound [δ H 7.08 d
(2.2), 6.85 d (2.2), 6.97 s, 7.34 s] also support the mouth mountain ketone B rings of the present invention to substitute for 6,7- bis-, C rings are 1,
3- bis- substitutes.So far the structure of the compounds of this invention is determined, Compound nomenclature is：6- (2- methylols) -1,7- dimethoxies
Base -3- methyl-mouth mountain ketone.
Embodiment 5
Any compound prepared by Example 2-3, is light yellow gum thing.Assay method is same as Example 4, confirms
Compound prepared by embodiment 2-3 is described mouth xanthones compounds --- 6- (2- methylols) -1,7- dimethoxy -3- first
Base-mouth mountain ketone.
Embodiment 6
Any mouthful of xanthones compounds prepared by Example 1-4 carry out antibacterial activity experiment, and test situation is as follows：
Antimicrobial test is carried out with agar diffusion method, and tested bacterium is equably coated in into plain agar culture medium (ox first
Meat extract, peptone, sodium chloride, serum, agar) flat board on, then (benzofuran C prime compound is with 10 by testing compound
ML DMSO dissolve, and are diluted with water into 50 μ g/mL solution) soaked tablet (mm of diameter 5) is placed on the culture medium to carry disease germs
On, it is put into insulating box, inhibition zone size is observed after being incubated the h of 24- 72 in 25 DEG C.As a result show：The compounds of this invention is to gold
Staphylococcus aureus, Escherichia coli, angstrom uncommon bacterium, hay bacillus, proteus etc. have very strong activity；Inhibiting rate exceedes
88.3%。
Embodiment 7
Safety evaluatio has been carried out to the compounds of this invention, tested by Micronuclei In The Mouse Bone Marrow, Ames is tested and TK genes
Mutating experiment, it was demonstrated that the compounds of this invention is nontoxic to animal, safe to use.
This compound is added on cigarette tipping paper with 50 μ g/mL concentration；By the People's Republic of China (PRC)《It is disposable
Amenities sanitary standard》GB15979-2002 detection method, takes the volume cigarette tipping paper for adding the compounds of this invention, and 2.0
× 3.0 mm sizes are detection bacterium sum, coliform, staphylococcus aureus, Pseudomonas aeruginosa, hemolytic streptococcus, true
Bacterium sum.As a result show, the tipping paper total plate count for adding the compounds of this invention significantly reduces, and this compound is to several tests
Bacterium have obvious inhibiting effect, more than 88.3% is entirely reached to the bacteriostasis rate of Escherichia coli, staphylococcus aureus etc..
Claims (10)
1. a kind of mouthful xanthones compounds, it is characterised in that the mouth xanthones compounds are separated from black purple Swertia patens
Arrive, its molecular formula is C17H16O5, it is named as：6- (2- methylols) -1,7- dimethoxys -3- methyl-mouth mountain ketone, has following knots
Structure formula：
。
2. the preparation method of the mouth xanthones compounds described in a kind of claim 1, it is characterised in that using black purple Swertia patens as original
Material, is extracted, silica gel column chromatography, high pressure liquid chromatography step through medicinal extract, is specially：
A, medicinal extract extracts:Using black purple Swertia patens as raw material, black purple Swertia patens are crushed or are cut into segment, are soaked with organic solvent
24h ~ 72h, extract 3 ~ 5 times, merge extract solution, filtering, be concentrated under reduced pressure into medicinal extract；
B, silica gel column chromatography：Medicinal extract carries out silica gel column chromatography with 160 ~ 300 mesh silica gel dry column-packings of the weight than 2 ~ 4 times of amounts；With
Chloroform-acetone solution carries out gradient elution, merges identical part, collects each several part eluent and concentrates；
C, high pressure liquid chromatography isolates and purifies：The 7 of step B eluent:3 parts are further isolated and purified i.e. with high pressure liquid chromatography
Obtain required mouth xanthones compounds.
3. the preparation method of according to claim 2 mouthful of xanthones compounds, it is characterised in that the step A it is organic molten
Agent is 80% ~ 100% methanol or ethanol, 60% ~ 90% acetone.
4. the preparation method of according to claim 2 mouthful of xanthones compounds, it is characterised in that the step A organic solvent
Weight ratio with black purple Swertia patens is 2 ~ 4:1.
5. the preparation method of according to claim 2 mouthful of xanthones compounds, it is characterised in that medicinal extract exists in the step B
Before silica gel column chromatography rough segmentation, after pure methanol or straight alcohol or pure acetone dissolving of the weight than 1.5 ~ 3 times of amounts, with weight ratio
0.8 ~ 1.2 times of 80 ~ 100 mesh silica gel mixed samples.
6. the preparation method of according to claim 2 mouthful of xanthones compounds, it is characterised in that chloroform in the step B-
The volume proportion of acetone soln is 1:0、20:1、9:1、8:2、7:3、6:4、1:1 and 1:2.
7. the preparation method of according to claim 2 mouthful of xanthones compounds, it is characterised in that the step C mesohigh liquid
Phase chromatographic separation and purification is to use 21.2 mm × 250mm, 5μM C18Chromatographic column, flow velocity 20mL/min, mobile phase are 50%
Methanol, UV-detector Detection wavelength are 335nm, each sample introduction 200μL, 22.6min chromatographic peak is collected, steamed after repeatedly adding up
It is dry.
8. the preparation method of according to claim 2 mouthful of xanthones compounds, it is characterised in that the step C mesohigh liquid
Compound after phase chromatographic separation and purification is dissolved with pure methanol again, then using pure methanol as mobile phase, is separated with gel filtration chromatography,
Further to isolate and purify.
A kind of 9. application of the mouth xanthones compounds in antibacterials are prepared described in claim 1.
A kind of 10. application of the mouth xanthones compounds in antimicrobial packaging is prepared described in claim 1.
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