CN110548055A - Fresh and fragrant celery leaf water extract powder, preparation, vasodilatation effect and application thereof - Google Patents
Fresh and fragrant celery leaf water extract powder, preparation, vasodilatation effect and application thereof Download PDFInfo
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- CN110548055A CN110548055A CN201810561625.3A CN201810561625A CN110548055A CN 110548055 A CN110548055 A CN 110548055A CN 201810561625 A CN201810561625 A CN 201810561625A CN 110548055 A CN110548055 A CN 110548055A
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- cinnamoyl
- quinic acid
- carboxy
- hydroxy
- apigenin
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- 239000000843 powder Substances 0.000 title claims abstract description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000000284 extract Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 235000010591 Appio Nutrition 0.000 title claims description 46
- 235000015849 Apium graveolens Dulce Group Nutrition 0.000 title claims description 44
- 230000024883 vasodilation Effects 0.000 title abstract description 8
- 206010047141 Vasodilatation Diseases 0.000 title abstract description 3
- 230000000694 effects Effects 0.000 title description 12
- 244000101724 Apium graveolens Dulce Group Species 0.000 title 1
- 241000208317 Petroselinum Species 0.000 claims abstract description 25
- 235000011197 perejil Nutrition 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000002253 acid Substances 0.000 claims abstract 2
- 150000007513 acids Chemical class 0.000 claims abstract 2
- -1 1, 3-butadiene-carbonyloxy Chemical group 0.000 claims description 66
- 240000007087 Apium graveolens Species 0.000 claims description 43
- 239000006286 aqueous extract Substances 0.000 claims description 30
- AAWZDTNXLSGCEK-LNVDRNJUSA-N (3r,5r)-1,3,4,5-tetrahydroxycyclohexane-1-carboxylic acid Chemical compound O[C@@H]1CC(O)(C(O)=O)C[C@@H](O)C1O AAWZDTNXLSGCEK-LNVDRNJUSA-N 0.000 claims description 28
- AAWZDTNXLSGCEK-UHFFFAOYSA-N Cordycepinsaeure Natural products OC1CC(O)(C(O)=O)CC(O)C1O AAWZDTNXLSGCEK-UHFFFAOYSA-N 0.000 claims description 27
- AAWZDTNXLSGCEK-ZHQZDSKASA-N Quinic acid Natural products O[C@H]1CC(O)(C(O)=O)C[C@H](O)C1O AAWZDTNXLSGCEK-ZHQZDSKASA-N 0.000 claims description 27
- KZNIFHPLKGYRTM-UHFFFAOYSA-N apigenin Chemical compound C1=CC(O)=CC=C1C1=CC(=O)C2=C(O)C=C(O)C=C2O1 KZNIFHPLKGYRTM-UHFFFAOYSA-N 0.000 claims description 18
- 229940117893 apigenin Drugs 0.000 claims description 18
- XADJWCRESPGUTB-UHFFFAOYSA-N apigenin Natural products C1=CC(O)=CC=C1C1=CC(=O)C2=CC(O)=C(O)C=C2O1 XADJWCRESPGUTB-UHFFFAOYSA-N 0.000 claims description 18
- 235000008714 apigenin Nutrition 0.000 claims description 18
- 238000002791 soaking Methods 0.000 claims description 12
- 238000001228 spectrum Methods 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 9
- 229930006000 Sucrose Natural products 0.000 claims description 8
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 8
- 239000005720 sucrose Substances 0.000 claims description 8
- 238000004949 mass spectrometry Methods 0.000 claims description 7
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000008399 tap water Substances 0.000 claims description 3
- 235000020679 tap water Nutrition 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229940124549 vasodilator Drugs 0.000 claims description 2
- 239000003071 vasodilator agent Substances 0.000 claims description 2
- 239000007983 Tris buffer Substances 0.000 claims 1
- 125000003668 acetyloxy group Chemical group [H]C([H])([H])C(=O)O[*] 0.000 claims 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims 1
- 125000004356 hydroxy functional group Chemical group O* 0.000 claims 1
- 125000004029 hydroxymethyl group Chemical group [H]OC([H])([H])* 0.000 claims 1
- 239000003814 drug Substances 0.000 abstract description 7
- 230000002040 relaxant effect Effects 0.000 abstract description 4
- 210000004204 blood vessel Anatomy 0.000 abstract description 3
- 235000000346 sugar Nutrition 0.000 abstract 1
- 150000008163 sugars Chemical class 0.000 abstract 1
- 238000001819 mass spectrum Methods 0.000 description 17
- 150000002500 ions Chemical class 0.000 description 16
- 238000003776 cleavage reaction Methods 0.000 description 8
- 230000037361 pathway Effects 0.000 description 8
- 230000007017 scission Effects 0.000 description 8
- OIPILFWXSMYKGL-UHFFFAOYSA-N acetylcholine Chemical compound CC(=O)OCC[N+](C)(C)C OIPILFWXSMYKGL-UHFFFAOYSA-N 0.000 description 7
- 229960004373 acetylcholine Drugs 0.000 description 7
- 206010047139 Vasoconstriction Diseases 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 230000025033 vasoconstriction Effects 0.000 description 6
- SFLSHLFXELFNJZ-QMMMGPOBSA-N (-)-norepinephrine Chemical compound NC[C@H](O)C1=CC=C(O)C(O)=C1 SFLSHLFXELFNJZ-QMMMGPOBSA-N 0.000 description 5
- 241000700159 Rattus Species 0.000 description 5
- 230000000875 corresponding effect Effects 0.000 description 5
- 229960002748 norepinephrine Drugs 0.000 description 5
- SFLSHLFXELFNJZ-UHFFFAOYSA-N norepinephrine Natural products NCC(O)C1=CC=C(O)C(O)=C1 SFLSHLFXELFNJZ-UHFFFAOYSA-N 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 210000002376 aorta thoracic Anatomy 0.000 description 3
- 238000009395 breeding Methods 0.000 description 3
- 230000001488 breeding effect Effects 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 210000004185 liver Anatomy 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 210000000115 thoracic cavity Anatomy 0.000 description 3
- 238000004704 ultra performance liquid chromatography Methods 0.000 description 3
- 235000013311 vegetables Nutrition 0.000 description 3
- 244000153885 Appio Species 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000007853 buffer solution Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000000132 electrospray ionisation Methods 0.000 description 2
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000007157 ring contraction reaction Methods 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 230000001225 therapeutic effect Effects 0.000 description 2
- 229940126680 traditional chinese medicines Drugs 0.000 description 2
- 239000011782 vitamin Substances 0.000 description 2
- 229940088594 vitamin Drugs 0.000 description 2
- 229930003231 vitamin Natural products 0.000 description 2
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- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 201000001320 Atherosclerosis Diseases 0.000 description 1
- 206010010774 Constipation Diseases 0.000 description 1
- 208000037093 Menstruation Disturbances Diseases 0.000 description 1
- 206010027339 Menstruation irregular Diseases 0.000 description 1
- 206010030113 Oedema Diseases 0.000 description 1
- 241000220154 Parnassia Species 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000008485 antagonism Effects 0.000 description 1
- NTDLXWMIWOECHG-YRCFQSNFSA-N apiin Chemical class O([C@@H]1O[C@@H]([C@H]([C@H](O)[C@H]1O[C@H]1[C@@H]([C@@](O)(CO)CO1)O)O)CO)C(C=1)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(O)C=C1 NTDLXWMIWOECHG-YRCFQSNFSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 230000001914 calming effect Effects 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 150000001793 charged compounds Chemical class 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
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- 230000000249 desinfective effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 208000002173 dizziness Diseases 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000001616 ion spectroscopy Methods 0.000 description 1
- 208000028867 ischemia Diseases 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000006199 nebulizer Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000003285 pharmacodynamic effect Effects 0.000 description 1
- 239000013641 positive control Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 230000000384 rearing effect Effects 0.000 description 1
- 230000010410 reperfusion Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 150000003445 sucroses Chemical class 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000012353 t test Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000002211 ultraviolet spectrum Methods 0.000 description 1
- 239000005526 vasoconstrictor agent Substances 0.000 description 1
- 230000000304 vasodilatating effect Effects 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P9/00—Drugs for disorders of the cardiovascular system
- A61P9/08—Vasodilators for multiple indications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/13—Preparation or pretreatment of starting material involving cleaning, e.g. washing or peeling
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pharmacology & Pharmacy (AREA)
- Engineering & Computer Science (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Animal Behavior & Ethology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Alternative & Traditional Medicine (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- General Chemical & Material Sciences (AREA)
- Heart & Thoracic Surgery (AREA)
- Cardiology (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Organic Chemistry (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Epidemiology (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for preparing fresh parsley leaf water extract powder, discloses structures of 38 new components in the fresh parsley leaf water extract powder, namely structures of 2 new cane sugars, structures of 22 new quinic acids and structures of 14 new apiosides, and further discloses vasodilatation of the fresh parsley leaf water extract powder, so that the invention discloses application of the fresh parsley leaf water extract powder in preparation of a blood vessel relaxing medicine.
Description
Technical Field
The invention relates to a method for preparing powder from an aqueous extract of fresh parsley green, which relates to the reproducibility of a process for preparing the powder from the aqueous extract of the fresh parsley green, which is defined by a characteristic UPLC-mass spectrum total ion current spectrum and 38 peaks thereof, relates to components in the powder, which are defined by the characteristic UPLC-mass spectrum total ion current spectrum and 38 peaks thereof, relates to the structures of 2 new sucrose analogs corresponding to the 38 peaks, relates to the structures of 22 new quinic acid analogs, relates to the structures of 14 new apioside analogs, and further relates to the vasodilation effect of the aqueous extract powder of the fresh parsley green, so the invention relates to the application of the aqueous extract powder of the fresh parsley green in preparing vasodilation medicines. The invention belongs to the field of biological medicine.
Background
a large body of statistical data suggests that vasoconstriction is closely related to aging, atherosclerosis and ischemia reperfusion. Effective prevention of vasoconstriction has become a health concern worldwide. Although some vitamins and traditional Chinese medicines have vasodilating effect, the long-term taking of the vitamin and traditional Chinese medicines as preventive medicines still has uncertainty. The discovery of the medicine which can be used for preventing vasoconstriction without any toxic and side effect is an important direction for medicine research.
the folk always has a theory of cool nature and taste of the celery leaves, and the celery leaves are considered to have the effects of clearing heat and disinfecting, treating the exuberant liver fire and calming the liver and clearing heat. In folk, vegetable leaves are rich in cellulose, so that the theory of relaxing bowels and treating constipation is provided. In folks, celery leaves are also thought to have the effect of lowering blood pressure and also can treat dizziness, edema and irregular menstruation. Without rigorous pharmacodynamic studies, the basis of these statements is only experience. Furthermore, whether celery leaves in these parnassia are celery leaves or parsley leaves is not defined. Further, these statements are not directly related to vasodilation. In addition, the inventor proposes the liver protection effect of the fresh celery leaf nano juice. However, the fresh celery leaf nano juice is not only mildewed but also precipitated after being placed for 20 days. Mildew may cause disease and precipitation may alter chemical composition. These two fatal problems caused the inventors to abandon the subsequent development of the fresh celery leaf nano-juice.
The inventor researches the chemical components and the treatment effect of the fresh and fragrant celery leaf water extract powder for a long time. The inventors have recognized that it is not clear to the skilled artisan which chemical components are contained in the aqueous extract of celeriac, nor is it clear what the therapeutic effect of the aqueous extract of celeriac. In response to this situation, the inventors performed mass spectrometry on an aqueous extract of fresh parsley leaf. Analysis of 38 components in the aqueous extract of fresh celery leaves led the inventors to realise that the aqueous extract of fresh celery leaves prevents vasoconstriction. The structural analysis of 38 components in the water extract of the fresh celery leaves leads to the discovery of 38 new compounds, thereby embodying the intelligence and creativity of the invention. Compared with all celery related known inventions, the fresh fragrant celery leaf water extract powder reaches a brand new height. Based on these findings, the inventors have proposed the present invention.
Disclosure of Invention
The first content of the invention is a method for providing fresh celery leaf aqueous extract powder, which comprises the following steps:
(1) Washing 1000g of fresh celery leaves without silt on the surface with 3000mL of tap water for 2 times, then transferring to a sterile environment, washing with 3000mL of triple-distilled water for 3 times, and filtering water to obtain clean fresh celery leaves;
(2) soaking clean fresh celery leaves in triple-distilled water at 60-90 ℃ for 3 times, soaking in 3000mL of triple-distilled water for at least 30 minutes each time, and slowly stirring during soaking;
(3) After each soaking, the water extract flows out slowly and automatically, and the time for use is not less than 30 minutes;
(4) And concentrating the obtained 9000mL of water extract at 60-90 ℃ under reduced pressure to obtain 24g of fresh celery leaf water extract powder.
The second content of the invention is to provide the ultraviolet spectrum of the fresh celery leaf water extract powder.
The third content of the invention is to provide a mass spectrum total ion current spectrum of the fresh celery leaf water extract powder.
the fourth aspect of the invention is to provide the chemical structures of the 38 components corresponding to the peaks in the mass spectrum total ion flow spectrum of the fresh parsley leaf aqueous extract powder.
The fifth content of the invention is to describe the therapeutic effect of the fresh celery leaf water extract powder on vasoconstriction.
drawings
FIG. 1 UPLC chromatogram of fresh celery leaf water extract powder.
FIG. 2. UPLC-mass spectrum of total ion current of fresh parsley leaf extract powder.
FIG. 3 is a mass spectrum of 6-O- [ E-2, 6-dihydroxy-2, 5-di- (2, 4-hexadienoyloxy) -4- (1, 3-butadienoyloxy) cinnamoyl ] sucrose.
FIG. 4 shows the cleavage pathway of 6-O- [ E-2, 6-dihydroxy-2, 5-di- (2, 4-hexadienoyloxy) -4- (1, 3-butadienoyloxy) cinnamoyl ] sucrose.
FIG. 5 is a mass spectrum of 3-O- [ E-2-hydroxy-6-acetoxy-3, 5-bis (carboxybutadienylcarbonyloxy) -4- (carboxy-n-acryloyloxy) cinnamoyl ] quinic acid.
FIG. 6 shows the cleavage pathway of 3-O- [ E-2-hydroxy-6-acetoxy-3, 5-bis (carboxybutadienylcarbonyloxy) -4- (carboxy n-acryloyloxy) cinnamoyl ] quinic acid.
FIG. 7.mass spectrum of 3-hydroxy-4- (n-propylcarbonyloxy) apigenin.
FIG. 8.3-hydroxy-4- (n-propylcarbonyloxy) apigenin cleavage pathway.
Detailed Description
To further illustrate the invention, a series of examples are given below. These examples are purely illustrative and are intended to be a detailed description of the invention only and should not be taken as limiting the invention.
Example 1 preparation of an aqueous extract powder of fresh parsley leaf
1000g of fresh celery leaves without silt on the surface are washed with 3000mL of tap water for 2 times, and then transferred to a sterile environment and washed with 3000mL of triple-distilled water for 3 times. Filtering off water to obtain clean fresh celery leaves. Soaking clean fresh celery leaves in triple-distilled water at 60-90 ℃ for 3 times, soaking in 3000mL of triple-distilled water for at least 30 minutes each time, and slowly stirring during soaking. After each soaking, the water extract is allowed to slowly flow out by itself for no less than 30 minutes. About 9000mL of the slowly flowing aqueous extracts were combined and concentrated at 60 ℃ -90 ℃ under reduced pressure to obtain 24g of powder of the fresh parsley leaf aqueous extract.
Example 2 determination of chromatography and Mass Spectrometry ion Spectroscopy of fresh celery leaf aqueous extract powder
2-1 preparation of sample solution (10mg/mL)
26.7mg of the water extract powder of fresh and fragrant celery leaves was weighed out and dissolved in 2.67mL of ultrapure water. The resulting solution was sonicated for 1 minute and then centrifuged at 13000r/min for 10 minutes. The supernatant was taken, filtered through a 0.22 μm filter and placed in a sample vial for chromatographic and mass spectrometric determination.
2-2. chromatographic conditions
Chromatographic column Waters, AcquityA HSS T3 column (2.1 × 100mm i.d.,1.8 μm);
The sample injection volume is 2 mu L;
PDA detector 210-400 nm;
Mobile phase water (0.1% formic acid), acetonitrile;
the mobile phase washed the column according to the gradient of table 1.
TABLE 1 mobile phase gradiometer
2-3 measuring chromatogram
UPLC chromatogram of the fresh celery leaf aqueous extract powder was determined and recorded according to the above chromatographic determination conditions (see the attached figure 1 of the specification).
2-4. conditions for measuring ion flow spectrum and mass spectrum
Electrospray ionization mode, Positive (PI) and Negative (NI) modes;
the collision energy of the inclined trap is 20-60V;
Cone current 40V;
The temperature of the ion source is 100 ℃;
The capillary voltage is 30 kV;
Spraying pressure is 6.5 bar;
the m/z range is 100-1500.
2-5, recording ion flow spectrum and mass spectrum
ion flow spectrum and mass spectrum of the fresh celery leaf water extract powder are measured and recorded according to the above conditions (see the attached figures 2 and 3-38 of the specification).
Example 3 assignment of the Structure of 38 Components in an aqueous extract powder of fresh parsley leaf
the UPLC chromatogram of example 2 was coupled to a mass spectrum and the UPLC-mass spectrum of the fresh parsley leaf aqueous extract powder was determined. Mass spectrometry conditions are two modes of electrospray ionization Positive Ion (PI) and Negative Ion (NI). The slant trap collision energy (ramp trap collision energy) is 20-60V. The cone voltage (cone voltage) was 40V. The ion source temperature was 100 ℃. The capillary voltage was 30 kV. The pressure of the nebulizer (nebulizerpressure) was 6.5 bar. The mass/charge ratio (m/z range) is 100-1500. 34 independent peaks separated within 14 minutes. According to the mass spectrometry fragmentation law, the peaks (numbered sequentially from left to right for the peaks of the total ion current spectrum) are assigned to the corresponding components of table 2.
TABLE 2 component names corresponding to peaks of the Total ion flux map
Example 4 chemical Structure, Mass Spectrometry and lysis Process of 34 Components in fresh celery leaf aqueous extract powder
The molecular ions and the fragment ions were correlated with each other on the basis of the mass spectrum corresponding to each peak in the total ion current measured in analytical example 2. Thus, the process is completed. The inventors established the cleavage pathway of the 38 components in table 2 of example 3 under the mass spectrometric conditions. After the confirmation of these cleavage pathways, it is in turn the basis for the discovery of the invention that 38 components in the water extract powder of fresh celery leaves have undisputed novelty and inventiveness. As representative examples, FIG. 3 shows a mass spectrum of 6-O- [ E-2, 6-dihydroxy-2, 5-bis- (2, 4-hexadienoyloxy) -4- (1, 3-butadienoyloxy) cinnamoyl ] sucrose, FIG. 4 shows a cleavage pathway of 6-O- [ E-2, 6-dihydroxy-2, 5-bis- (2, 4-hexadienoyloxy) -4- (1, 3-butadienoyloxy) cinnamoyl ] sucrose, FIG. 5 shows a mass spectrum of 3-O- [ E-2-hydroxy-6-acetyloxy-3, 5-bis (carboxybutadienoyloxy) -4- (carboxy n-acryloyloxy) cinnamoyl ] quinic acid, FIG. 6 shows 3-O- [ E-2-hydroxy-6-acetyloxy-3, the cleavage pathway of 5-bis (carboxybutadienecarbonyloxy) -4- (carboxy n-acryloyloxy) cinnamoyl ] quinic acid, FIG. 7 is 3-hydroxy
mass spectrum of-4- (n-propylcarbonyloxy) apigenin, and figure 8 is a cleavage pathway of 3-hydroxy-4- (n-propylcarbonyloxy) apigenin.
Example 5 measurement of vasodilation Effect of fresh parsley leaf Water extract powder
Since noradrenaline is generally known as a vasoconstrictor and acetylcholine is generally known as a vasodilator, the antagonism of the noradrenaline-induced thoracic aortic ring contraction in rats by the fresh celery leaf extract powder is measured on a noradrenaline-induced thoracic aortic ring contraction model in rats. Acetylcholine is a positive control for the present invention.
Rats anesthetized with ether were sacrificed by cervical dislocation, the thoracic aorta was removed by opening the thoracic cavity and cut into a 2mm long loop. The prepared thoracic aorta ring of the rat is placed in a K-H buffer solution and aerated to keep the activity. Starting a physiological two-channel instrument (the running software is M3000), starting circulating water of the breeding tank, injecting K-H buffer solution into the breeding tank and introducing oxygen. The tension transducer is set and calibrated. The rat thoracic aorta was looped over a tension transducer, placed in a rearing trough and tension monitored. After the tonicity stabilized, 20. mu.L of noradrenaline aqueous solution was added to make its concentration in the incubator 20. mu.g/mL. Monitoring the tension, after the tension is stabilized, injecting an aqueous solution of the fresh celery leaf water extract powder (the concentration is 50 mu g/mL,100 mu g/mL,150 mu g/mL and 200 mu g/mL) or an acetylcholine aqueous solution (the concentration is 2 mu g/mL) into the breeding tank, and recording the tension after the tension is stabilized. And calculating the tension difference between the water solution of the fresh fragrant celery leaf water extract powder and the acetylcholine water solution before and after injection. The percentage of the difference value and the tension of the aqueous solution of the fresh parsley leaf water extract powder or the acetylcholine aqueous solution before injection is the relaxation rate. The results are shown in Table 3.
TABLE 3 vasodilation of the fresh parsley leaf aqueous extract powder
a) The concentration group ratio p of 120 mu g/mL,80 mu g/mL and 40 mu g/mL is less than 0.01, and the ratio p of acetylcholine is more than 0.05; b) the ratio p to the concentrations of 80 mug/mL and 40 mug/mL is less than 0.01; c) p <0.01 to a concentration of 40 μ g/mL; n is 3, and the experimental data statistics adopt t test.
The data in Table 3 illustrate that aqueous solutions of the fresh parsley leaf aqueous extract powder at concentrations of 40. mu.g/mL, 80. mu.g/mL, 120. mu.g/mL, and 160. mu.g/mL, concentration-dependently antagonize norepinephrine-induced vasoconstriction. The effect peaked at a concentration of 160. mu.g/mL and was not different from acetylcholine. Different from the blood vessel relaxing medicine applied clinically, the fresh and fragrant celery leaves are vegetables. As a vegetable which can be eaten at will, the fresh and fragrant celery leaf water extract powder has an unexpected technical effect of blood vessel relaxing effect.
Claims (6)
1. the fresh fragrant celery leaf water extract powder is characterized in that the powder is composed of 38 new compounds which are 2 kinds of sucrose, 22 kinds of quinic acid and 14 kinds of apigenin.
2. The fresh parsley leaf aqueous extract powder of claim 1, characterized in that the 2 sucrose are 6-O- [ E-2, 6-dihydroxy-2, 5-bis- (2, 4-hexadienocarbonyloxy) -4- (1, 3-butadiene-carbonyloxy) cinnamoyl ] sucrose and 6-O- [ E-3-hydroxy-4-acryloyloxy-5- (2-butenyloxy) cinnamoyl ] sucrose.
3. the fresh parsley leaf aqueous extract powder of claim 1, wherein the 22 kinds of quinic acids are respectively 3-O- [ E-2, 6-dihydroxy-3, 5-di (carboxy n-butyldienoyloxy) -4- (hydroxy n-butyldienoyloxy) cinnamoyl ] quinic acid, 3-O- [ E-2, 6-dihydroxy-3, 4, 5-tri (acryloyloxy) cinnamoyl ] quinic acid, 3-O- [ E-3, 5-di (carboxy n-butyldienoyloxy) -4- (carbonyl n-butyldienoyloxy) cinnamoyl ] quinic acid, 3-O- [ E-2, 6-dihydroxy-3, 5-di (carboxy n-butyldienoyloxy) -4- (carboxyacryloyloxy) cinnamoyl ] quinic acid, 3-O- [ E-3, 5-bis (carboxypropenoyloxy) -4- (carboxyn-butyldienoyloxy) cinnamoyl ] quinic acid, 3-O- [ E-2-hydroxy-3, 5-bis (carboxypropenoyloxy) -4- (carboxyacetoxy) cinnamoyl ] quinic acid, 3-O- [ E-2, 6-dihydroxy-3, 5-bis (carboxy-n-propylcarbonyloxy) -4- (hydroxy-n-propylcarbonyloxy) cinnamoyl ] quinic acid, 3-O- [ E-3, 5-bis (carboxy-n-butyldienoyloxy) -4- (carboxyacetoxy) cinnamoyl ] quinic acid, 3-O- [ E-2-hydroxy-3, 5-bis (carboxy-n-butylcarbonyloxy) -4- (hydroxy-n-butylcarbonyloxy) cinnamoyl ] quinic acid, 3-O- [ E-2, 6-dihydroxy-3, 5-di (carboxy n-propylcarbonyloxy) -4- (hydroxy n-propylcarbonyloxy) cinnamoyl ] quinic acid, 3-O- [ E-2, 6-dihydroxy-3, 5-di (carboxybutadienylcarbonyloxy) -4- (carboxy-2-butenyloxy) cinnamoyl ] quinic acid, 3-O- [ E-3, 5-di (carboxybutadienylcarbonyloxy) -4- (carboxy-3, 5-hexadienylcarbonyloxy) cinnamoyl ] quinic acid, 3-O- [ E-2-hydroxy-6-acetoxy-3, 5-di (carboxybutadienylcarbonyloxy) -4- (carboxy n-propyloxy) cinnamoyl ] quinic acid, 3-O- [ E-2, 6-bis (carboxy-n-acryloyloxy) -3-formyloxy-4, 5-bis (carboxyacetoxy) cinnamoyl ] quinic acid, 3-O- [ E-3- (carboxy-n-butyldienylcarbonyloxy) -4- (carboxyacetoxy) -5- (carboxy-3-n-butenylcarbonyloxy) cinnamoyl ] quinic acid, 3-O- [ E-2-hydroxy-3, 5-bis (carboxy-n-butyldienylcarbonyloxy) -4- (carboxy-n-butylcarbonyloxy) cinnamoyl ] quinic acid, 3-O- [ E-2-hydroxy-3, 5-bis (carboxy-n-acryloyloxy) -4- (hydroxymethyl) cinnamoyl ] quinic acid, 3-O- [ E-3- (hydroxy-n-propylcarbonyloxy) -4- (acryloyloxy) -5- (formyl-1, 3-butadiene carbonyloxy) cinnamoyl ] quinic acid, 3-O- [ E-3- (carboxy-3-n-butenylcarbonyloxy) -4- (carboxy n-butylcarbonyloxy) -5- (hydroxy-4-n-pentenylcarbonyloxy) cinnamoyl ] quinic acid, 3-O- [ E-2-hydroxy-3, 4-bis (hydroxy n-propylcarbonyloxy) -5- (carboxypropylcarbonyloxy) cinnamoyl ] quinic acid, 3-O- [ E-2, 6-dihydroxy-3, 4, 5-tris (hydroxy n-propylcarbonyloxy) cinnamoyl ] quinic acid and 3-O- [ E-3, 5-bis (hydroxy n-propylcarbonyloxy) -4- (hydroxypropionyloxy) cinnamoyl ] quinic acid.
4. The fresh parsley leaf aqueous extract powder of claim 1, wherein 14 kinds of apigenin are 2, 6-dihydroxy-3, 4-di (n-undecyloxycarbonyloxy) -5- (n-undecyloxycarbonyloxy) apigenin, 3, 4-di (n-butylcarbonyloxy) apigenin, 3- (7-n-heptenecarbonyloxy) -4- (n-hexylcarbonyloxy) apigenin, 2, 6-dihydroxy-3, 4-di (9-n-decaenecarbonyloxy) -5- (n-undecyloxycarbonyloxy) apigenin, 3- (acryloyloxy) -4- (hydroxymethyl oxy) apigenin, 3-hydroxy-4- (n-propylcarbonyloxy) apigenin, 3-formyloxy-4-acetoxyapigenin, 3, 5-di (acetyloxy) -4- (n-acryloylcarbonyloxy) apigenin, api, 3- (3,5,7, 9-decatetraenyloxy) -4- (1,3,5,7, 9-decapentaenyloxy) apigenin, 3-acetoxy-4-hydroxyapigenin, 3, 4-di (n-butyldienoyloxy) apigenin, 3- (3, 4-pentadienoyloxy) -4- (1,3, 5-n-hexatrienylcarbonyloxy) apigenin, 3- (3,5, 7-n-heptatrienylcarbonyloxy) -4- (3, 5-n-hexadienoyloxy) apigenin, and 4- (4-n-pentenoyloxy) apigenin.
5. A process for preparing an aqueous extract powder of freshly flavored celery leaves according to claim 1, which process comprises the steps of:
(1) Washing 1000g of fresh celery leaves without silt on the surface with 3000mL of tap water for 2 times, then transferring to a sterile environment, washing with 3000mL of triple-distilled water for 3 times, and filtering water to obtain clean fresh celery leaves;
(2) Soaking clean fresh celery leaves in triple-distilled water at 60-90 ℃ for 3 times, soaking in 3000mL of triple-distilled water for at least 30 minutes each time, and slowly stirring during soaking;
(3) After each soaking, the water extract flows out slowly and automatically, and the time for use is not less than 30 minutes;
(4) Concentrating the obtained 9000mL of aqueous extract at 60-90 deg.C under reduced pressure to obtain about 24g of powder of fresh parsley leaf aqueous extract;
(5) The components contained in the aqueous extract powder are defined by its characteristic UPLC-mass spectrometry total ion current spectrum and 38 peaks therein, and the mass of the aqueous extract powder is also defined by its characteristic UPLC-mass spectrometry total ion current spectrum and 38 peaks therein.
6. Use of the fresh parsley leaf aqueous extract powder of claim 1 for the preparation of a vasodilator.
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