CN118142205A - Method for extracting polyphenol characteristic components of polygonatum cyrtonema by utilizing ultrasonic wave-assisted natural eutectic solvent and application of method - Google Patents
Method for extracting polyphenol characteristic components of polygonatum cyrtonema by utilizing ultrasonic wave-assisted natural eutectic solvent and application of method Download PDFInfo
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- CN118142205A CN118142205A CN202410106142.XA CN202410106142A CN118142205A CN 118142205 A CN118142205 A CN 118142205A CN 202410106142 A CN202410106142 A CN 202410106142A CN 118142205 A CN118142205 A CN 118142205A
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- polygonatum cyrtonema
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- 241001468611 Polygonatum cyrtonema Species 0.000 title claims abstract description 60
- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 58
- 239000002904 solvent Substances 0.000 title claims abstract description 57
- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 50
- 230000005496 eutectics Effects 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000000605 extraction Methods 0.000 claims abstract description 50
- 239000000284 extract Substances 0.000 claims abstract description 34
- LEHOTFFKMJEONL-UHFFFAOYSA-N Uric Acid Chemical compound N1C(=O)NC(=O)C2=C1NC(=O)N2 LEHOTFFKMJEONL-UHFFFAOYSA-N 0.000 claims abstract description 5
- TVWHNULVHGKJHS-UHFFFAOYSA-N Uric acid Natural products N1C(=O)NC(=O)C2NC(=O)NC21 TVWHNULVHGKJHS-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229940116269 uric acid Drugs 0.000 claims abstract description 5
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 18
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- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 claims description 9
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 claims description 9
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- 238000004458 analytical method Methods 0.000 claims description 5
- 239000003814 drug Substances 0.000 claims description 5
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000000132 electrospray ionisation Methods 0.000 claims description 3
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- -1 polyphenol compounds Chemical class 0.000 abstract description 7
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- ZTOJFFHGPLIVKC-YAFCTCPESA-N (2e)-3-ethyl-2-[(z)-(3-ethyl-6-sulfo-1,3-benzothiazol-2-ylidene)hydrazinylidene]-1,3-benzothiazole-6-sulfonic acid Chemical compound S\1C2=CC(S(O)(=O)=O)=CC=C2N(CC)C/1=N/N=C1/SC2=CC(S(O)(=O)=O)=CC=C2N1CC ZTOJFFHGPLIVKC-YAFCTCPESA-N 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 108010093894 Xanthine oxidase Proteins 0.000 description 6
- 102100033220 Xanthine oxidase Human genes 0.000 description 6
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- 241000196324 Embryophyta Species 0.000 description 4
- 241000220317 Rosa Species 0.000 description 4
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- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
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- LRFVTYWOQMYALW-UHFFFAOYSA-N 9H-xanthine Chemical compound O=C1NC(=O)NC2=C1NC=N2 LRFVTYWOQMYALW-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- MGJZITXUQXWAKY-UHFFFAOYSA-N diphenyl-(2,4,6-trinitrophenyl)iminoazanium Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1N=[N+](C=1C=CC=CC=1)C1=CC=CC=C1 MGJZITXUQXWAKY-UHFFFAOYSA-N 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 2
- 210000003734 kidney Anatomy 0.000 description 2
- 150000002632 lipids Chemical class 0.000 description 2
- 238000004895 liquid chromatography mass spectrometry Methods 0.000 description 2
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- 210000000952 spleen Anatomy 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000001269 time-of-flight mass spectrometry Methods 0.000 description 2
- 238000002137 ultrasound extraction Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- OCZVHBZNPVABKX-UHFFFAOYSA-N 1,1-diphenyl-2-(2,4,6-trinitrophenyl)hydrazine;ethanol Chemical compound CCO.[O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1NN(C=1C=CC=CC=1)C1=CC=CC=C1 OCZVHBZNPVABKX-UHFFFAOYSA-N 0.000 description 1
- HUSXNIFVQFHSEA-UHFFFAOYSA-N 2-hydroxypropanoic acid;hydrochloride Chemical compound Cl.CC(O)C(O)=O HUSXNIFVQFHSEA-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 206010021143 Hypoxia Diseases 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 241000234280 Liliaceae Species 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 241000756042 Polygonatum Species 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229960001231 choline Drugs 0.000 description 1
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
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- 229930003944 flavone Natural products 0.000 description 1
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- 150000002215 flavonoids Chemical class 0.000 description 1
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- 229940074391 gallic acid Drugs 0.000 description 1
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- 239000002608 ionic liquid Substances 0.000 description 1
- 229930013686 lignan Natural products 0.000 description 1
- 150000005692 lignans Chemical class 0.000 description 1
- 235000009408 lignans Nutrition 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
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- 230000000144 pharmacologic effect Effects 0.000 description 1
- 239000008363 phosphate buffer Substances 0.000 description 1
- 229940068065 phytosterols Drugs 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 229930010796 primary metabolite Natural products 0.000 description 1
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- 229940075420 xanthine Drugs 0.000 description 1
Classifications
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- 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)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/896—Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
- A61K36/8969—Polygonatum (Solomon's seal)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/12—Ketones
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/365—Lactones
- A61K31/366—Lactones having six-membered rings, e.g. delta-lactones
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/7024—Esters of saccharides
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/7028—Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages
- A61K31/7032—Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages attached to a polyol, i.e. compounds having two or more free or esterified hydroxy groups, including the hydroxy group involved in the glycosidic linkage, e.g. monoglucosyldiacylglycerides, lactobionic acid, gangliosides
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/7042—Compounds having saccharide radicals and heterocyclic rings
- A61K31/7048—Compounds having saccharide radicals and heterocyclic rings having oxygen as a ring hetero atom, e.g. leucoglucosan, hesperidin, erythromycin, nystatin, digitoxin or digoxin
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P19/00—Drugs for skeletal disorders
- A61P19/06—Antigout agents, e.g. antihyperuricemic or uricosuric agents
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- A61P39/00—General protective or antinoxious agents
- A61P39/06—Free radical scavengers or antioxidants
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0261—Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
- B01D11/0265—Applying ultrasound
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- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
- B01D11/0284—Multistage extraction
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- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- 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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Abstract
The invention discloses a method for extracting polyphenol characteristic components of Polygonatum cyrtonema Fabricius by utilizing an ultrasonic wave to assist a natural eutectic solvent and an application thereof, wherein the natural eutectic solvent is combined with the ultrasonic wave to prepare the polyphenol extract of Polygonatum cyrtonema Fabricius for the first time, and the method is established to adopt the environment-friendly natural eutectic solvent as an extraction solvent to extract polyphenol compounds in the Polygonatum cyrtonema Fabricius in a green and efficient manner, so that the extraction efficiency can be improved, the obtained extract has 17 main characteristic polyphenol compounds, has better antioxidation and uric acid reducing effects, has wide application prospect in the aspect of functional product development, is environment-friendly and high in stability, is simple to operate, has less solvent consumption, short extraction time and low production cost, can replace the traditional organic solvent, and can be suitable for large-scale industrial production, and solves the problems of high toxicity, poor biodegradability, low extraction efficiency and the like of the traditional organic solvent.
Description
Technical field:
the invention relates to the technical field of natural product extraction and application, in particular to a method for extracting polyphenol characteristic components of polygonatum cyrtonema by utilizing ultrasonic wave-assisted natural eutectic solvent and application thereof.
The background technology is as follows:
Polygonatum cyrtonema (Polygonatum cyrtonema Hua) is a tuber of a perennial herb of Polygonatum genus of Liliaceae family, and is widely distributed in the southern area of China. It grows in the under forest, shrub or hillside yin, has the altitude of 500-2100 m, tastes sweet, calms, returns to spleen, lung and kidney essence, and has the effects of tonifying qi and nourishing yin, strengthening spleen, moistening lung and tonifying kidney. Polygonatum cyrtonema is one of three medicine sources of the traditional Chinese medicine Polygonatum cyrtonema carried by the pharmacopoeia of the people's republic of China (2020 edition), and also belongs to a medicine and food homologous forest source plant.
Polygonatum cyrtonema Fabricius is rich in various active ingredients including polysaccharides, steroids, saponins, flavones, alkaloids, lignans, phytosterols, etc. Modern pharmacological researches also find that Polygonatum cyrtonema has the effects of resisting oxidation, fatigue, aging, hypoxia, regulating immunity, reducing blood lipid and blood sugar, resisting tumor, reducing blood sugar, resisting bacteria, inflammation, virus, improving memory and the like. The polysaccharide is used as the main functional component in the Polygonatum cyrtonema Fabricius, is an important index for evaluating the quality of the Polygonatum cyrtonema Fabricius, the content of the Polygonatum cyrtonema Fabricius polysaccharide specified in the Chinese pharmacopoeia (2020 edition) is not lower than 7.0%, and the most research and application of the Polygonatum cyrtonema Fabricius are total polysaccharide at present. In addition, the flavonoid component is a special component in the polygonatum cyrtonema, and is mainly concentrated on the aspects of content analysis and extraction preparation process optimization. However, there are few reports on the study of total polyphenol of Polygonatum cyrtonema Fabricius.
The natural eutectic solvent (natural deep eutectic solvents, NADES) is a novel green solvent, and has the potential of replacing the traditional organic solvent to realize the efficient extraction of natural active substances. It is a eutectic solvent composed of natural components such as primary metabolites, which is considered to be the third liquid phase naturally occurring in organisms, independent of water and lipids, and a homogeneous liquid mixture composed of hydrogen bond donors and hydrogen bond acceptors in a certain ratio. At present, the NADES can be prepared by adopting a plurality of methods such as hot mixing, vacuum evaporation, freeze drying or grinding, and the like, and has simple operation and low requirement on equipment. According to the compounds used in the synthesis of NADES, NADES can be divided into five main categories of ionic liquid type, neutral acid type, neutral alkali type and amino acid-containing NADES, wherein the formation process is to combine natural compounds such as saccharides, organic acid, amino acid and choline derivative according to a certain molar ratio to form a low-melting-point liquid mixture under certain conditions, and the formation principle is that hydrogen bonds formed between hydrogen bond donors and hydrogen bond acceptors separate charges, so that the melting point of the mixture is reduced, and finally, a liquid eutectic system is presented at room temperature. The NADES has the characteristics of green safety, low melting point (lower than any single component), good heat stability, high chemical stability and low volatilization, and has great advantages in the aspects of natural product extraction, organic synthesis and the like because hydroxyl or carboxyl in the component structure can form hydrogen bonds with the extract. For example, the prior art provides cases of extracting polyphenols from different plant bodies using eutectic solvents, see publications: wang Xiaoyi, li Peikun, li Jingong, etc. ultrasonic assisted extraction of rose polyphenols with eutectic solvents and their antioxidant activity [ J ]. Food research and development 2022,43 (8): 8. An efficient and rapid extraction of polyphenols in rose flowers using an ultrasonic assisted DES method is disclosed, and compared with conventional ethanol extraction methods. The optimal technological conditions for extracting rose polyphenol by the DES method through the optimized single-factor test are as follows: choline chloride-lactic acid with water content of 30% (molar ratio of 1:2) is used as the optimal extractant, the feed liquid ratio of 1:40 (g/mL), the ultrasonic time of 10min, the ultrasonic power of 400W, the ultrasonic temperature of 50 ℃ and the extraction time of 2 times, and the extraction amount of rose polyphenol under the condition is 136.20 +/-1.23 mg/g.
However, the different plants have different structures and components, and the types and content ratios of the polyphenols contained are different, so that the eutectic solvent formula and the extraction conditions suitable for extracting the polyphenols in the different plants are not consistent, and obvious individual differences exist. There is no disclosure of extracting polyphenol from Polygonatum cyrtonema Fabricius by using eutectic solvents.
The invention comprises the following steps:
The invention aims to provide a method for extracting polyphenol characteristic components of polygonatum cyrtonema by utilizing ultrasonic wave to assist a natural eutectic solvent and application thereof, wherein the natural eutectic solvent is combined with ultrasonic wave to prepare the polyphenol extract of polygonatum cyrtonema for the first time, so that the problems of high toxicity, poor biodegradability, low extraction efficiency and the like of the traditional organic solvent serving as an extractant are solved.
The invention is realized by the following technical scheme:
A method for extracting polyphenol characteristic components of Polygonatum cyrtonema Fabricius by using ultrasonic wave assisted natural eutectic solvent comprises the following steps: adding the polygonatum cyrtonema powder into the prepared natural eutectic solvent, wherein the feed liquid ratio of the polygonatum cyrtonema powder sample to the natural eutectic solvent is 1:10-30 g/mL, and extracting by adopting ultrasonic assistance, and the ultrasonic conditions are as follows: the temperature is 25-45 ℃, the power is 50-200W, and the extraction time is 5-35 min; after the extraction is finished, centrifuging the sample solution at 3500-5000 rpm for 5-15 min to obtain supernatant as Polygonatum cyrtonema Sieb extract; then drying to obtain an extract sample; the natural eutectic solvent component comprises betaine and lactic acid; the preparation method comprises the following steps: mixing betaine and lactic acid according to the mass ratio of 2:1-1:2, heating and stirring at 80-100 ℃ until the betaine and lactic acid are in uniform, clear and transparent liquid without crystallization precipitation at room temperature, and adding water according to the mass ratio.
Preferably, the preparation method of the polygonatum cyrtonema powder comprises the following steps: taking a fresh collected polygonatum cyrtonema sample, washing, slicing, drying at 40-60 ℃, crushing, sieving with a 60-80 mesh sieve, and placing in a fresh-keeping bag and placing in a dryer for standby.
Preferably, the natural eutectic solvent has a water content of 20wt% to 50wt%.
Most preferably, the water content of the natural eutectic solvent prepared by betaine and lactic acid is 50%, the feed liquid ratio of the polygonatum cyrtonema powder sample to the natural eutectic solvent is 1:19 g/mL, and the extraction time is 35min.
Preferably, the drying means is freeze-drying or spray-drying.
The polyphenol chemical composition of the Polygonatum cyrtonema Fabricius extract is analyzed by adopting ultra-high liquid chromatography-four-level rod/time-of-flight mass spectrometry (UPLC-Q-TOF-MS/MS). Chromatographic conditions: agilent ultra-high liquid chromatograph 1290, chromatographic column is waters BEH C182.1 x 100mm 1.7um, flow rate is 0.3mL/min, sample injection amount is 5uL, mobile phase A is 0.1% formic acid aqueous solution, mobile phase B is acetonitrile solution, gradient elution ：0～8min,95％～79％A;8～17min,79％～78％A;17～20min,78％～60％A,20～30min,60％～55％A,30～40min,55％～27％A,40～45min,27％～0％A,45～50min,0％～95％A,50～55min,95％A. mass spectrum conditions: agilent Q-TOF6550, electrospray ionization source, mass spectrum scan range: the primary temperature is 50-1500 m/z, and the sheath gas temperature is 350 ℃; the sheath gas flow rate was 12L/min.
The extract has 17 polyphenol characteristic components and has the following structural formula:
At present, the polyphenol substances of Polygonatum cyrtonema Fabricius are mainly found in the aspect of total content detection, characteristic compounds are not analyzed and compared in reports of Polygonatum cyrtonema Fabricius component extraction by utilizing a eutectic solvent, and meanwhile, substances with polyphenol hydroxyl structures such as a compound (2), a compound (7), a compound (9), a compound (10), a compound (13) and a compound (14) are found in the substances for the first time based on a liquid chromatography-mass spectrometry technology, so that the ultrasonic-assisted natural eutectic solvent can be used for effectively extracting the polyphenol substances of Polygonatum cyrtonema Fabricius.
The polyphenol characteristic extract obtained by the invention also has better antioxidation and uric acid reducing effects, so the invention also protects the application of the extract in preparing antioxidants and uric acid reducing medicaments.
The beneficial effects of the invention are as follows: according to the invention, the natural eutectic solvent is combined with ultrasonic extraction to prepare the polyphenol extract of the polygonatum cyrtonema, and the NADES of different systems is screened to establish a method for green and high-efficiency extraction of polyphenol compounds in the polygonatum cyrtonema by using the environment-friendly natural eutectic solvent as an extraction solvent, so that the extraction efficiency can be improved, the obtained extract has 17 main characteristic polyphenol compounds, has better antioxidation and uric acid reducing effects, has wide application prospects in the aspect of functional product development, and the substances of polyphenol hydroxyl structures such as the compound (2), the compound (7), the compound (9), the compound (10), the compound (13) and the compound (14) are also found in the substances for the first time.
Description of the drawings:
FIG. 1 is a response surface diagram of a polyphenol characteristic component extraction process.
FIG. 2 shows the DPPH radical scavenging effect of the sample
FIG. 3 shows the effect of sample on ABTS radical scavenging
FIG. 4 shows the inhibition of xanthine oxidase by the samples.
The specific embodiment is as follows:
the following is a further illustration of the invention and is not a limitation of the invention.
In the embodiment, different types of eutectic solvents are firstly screened to extract the polyphenol substances of the polygonatum cyrtonema, the optimal preparation process is obtained by optimizing the extraction temperature, the extraction time and the extraction condition of the feed liquid ratio, and the anti-oxidation effect evaluation is carried out on the samples prepared by the optimal preparation process, so that the method for preparing the characteristic components of the polygonatum cyrtonema by extracting the natural eutectic solvents is aimed to be established.
For a better explanation of the present invention, the present invention will be described in detail by way of specific embodiments with reference to the accompanying drawings. The following examples are further illustrative of the invention and are not intended to be limiting thereof.
Sample and solution preparation
Taking a fresh collected polygonatum cyrtonema sample, cleaning, slicing, drying at 60 ℃, crushing, sieving with a 80-mesh sieve, and placing in a fresh-keeping bag and placing in a dryer for standby.
According to the pre-experiment result, lactic acid is selected as a hydrogen donor, betaine is selected as a hydrogen acceptor, and the natural eutectic solvent is prepared according to the mass ratio of 1:2. The mixture was placed in a magnetic stirring heater and stirred at a constant temperature of 85 ℃ until a homogeneous, clear, transparent liquid was obtained. Adding 30% (V/V) deionized water for dilution for later use.
Sample extraction and preparation process
Weighing about 0.5g of Polygonatum cyrtonema Fabricius powder of a sample to be detected and a triangular bottle with a stopper, correspondingly adding an extraction solvent according to the feed liquid ratio of 1:20 (g/mL), after weighing the mass, carrying out ultrasonic auxiliary extraction at room temperature for 30min, compensating for lost mass, centrifuging the sample for 20min under the condition of 4000r/min, and taking a proper amount of supernatant for analyzing the total polyphenol content.
Total polyphenol detection method
Accurately transferring 1.0mL of the solution to be measured, adding 5.0mL of 10% Fu Lin Fen reagent, shaking uniformly, adding 4.0mL of 7.5% sodium carbonate solution, and adding water to fix the volume to the scale. Standing at room temperature for 60min, detecting absorbance at 765nm, and drawing standard curve with gallic acid as reference substance.
The betaine-lactic acid eutectic solvent (DES S) is selected as the extraction solvent of total polyphenol of Polygonatum cyrtonema Fabricius through a pre-test, and factors such as DESs solvent composition, extraction conditions and the like are systematically examined in order to obtain optimal extraction conditions. Factors examined include the water content of the betaine-lactic acid eutectic solvent (30%, 40%, 50%, 60%, 70%), the extraction time (10 min, 20min, 30min, 40min, 50 min), and the feed-to-liquid ratio (1:10 g/mL, 1:15 g/mL, 1:20 g/mL, 1:25 g/mL, 1:30 g/mL).
And (3) taking a central combination Design principle as a theoretical basis, taking the total polyphenol yield as a response value, and using Design-Expert software to Design a three-factor and three-level response surface test. Based on a single factor test, the factor levels are determined as solvent moisture content, extraction time and feed to liquid ratio. The factors and levels are shown in Table 1, the test group designs and results are shown in Table 2, and the analysis of variance is shown in Table 3.
TABLE 1 factor level Table
Table 2 test design
TABLE 3 analysis of variance table
Note that: * Represents very significant levels (P < 0.01); * Representing significant levels (P < 0.05).
The regression model P <0.01, which is obvious, shows that the model is true; while the model mismatch term p=0.2572 >0.05 appears insignificant, indicating that no higher order term equation need to be fitted, further indicating that the effect of factors on total polyphenol extraction yield is reasonable using this model analysis. The analysis of variance results show that the influence of the primary term X 1、X2, the interactive term X 1X3 and the secondary term X 1 2、X2 2、X3 2 on the yield of total polyphenols of the model is extremely remarkable (P < 0.01), while the influence of the primary term X 3 and the interactive term X 1X2、X2X3 on the yield of total polyphenols of polygonatum cyrtonema is not remarkable (P > 0.05). In addition, the experimental model has the characteristics of R 2 = 0.9877, which shows that the predictability and consistency of the experimental result are good, and R adj 2 = 0.9718, which shows that the model can explain the change of 97.18% response value, and shows that the model has good fitting degree and small experimental error. In the model, the variation Coefficient (CV) =1.54% indicates that the random error of the test is small, which also indicates the sufficiency and rationality of the model, can accurately reflect the test result, and has higher accuracy. F value and P value of each factor are comprehensively analyzed, and the primary and secondary size orders of the factors affecting the total polyphenol yield are solvent water content > extraction time > feed-liquid ratio. The influence degree of each interactive factor on the total polyphenol yield of polygonatum cyrtonema is X 1X3 to the greatest extent. Applying Design Expert 10.0.4 to fit the numerical values in Table 4 to obtain a quadratic polynomial regression model ：Y＝0.70+0.030X1+0.026X2－4.625E-003X3－8.250E-003X1X2－0.028X1X3－0.011X2X3－0.047X1 2－0.035X2 2－0.064X3 2., and according to analysis, when the total polyphenol of the polygonatum cyrtonema is extracted by taking sweet theophylline-lactic acid as the optimal eutectic solvent, the optimal extraction condition is that the water content of the solvent is 50%, the extraction time is 35min, the feed-liquid ratio is 1:19 (g/mL), and under the condition, the extraction yield predicted value of the total polyphenol of the polygonatum cyrtonema is 0.706%. The results of three verification tests show that the total polyphenol yield of the polygonatum cyrtonema is (0.706+/-0.002)%, and is close to a predicted value.
In the response surface diagram shown in fig. 1, the curved surface shape reflects the influence of interaction of the curved surface points of the response surface on the extraction rate of total polyphenol of polygonatum cyrtonema, and the larger the gradient of the curved surface is, the larger the influence is, the smaller the gradient of the curved surface is, and the smaller the influence is; if the contour is circular, it is stated that the interaction between the two factors is not significant. The contour lines of the extraction factors are approximate to ellipses, which shows that certain interaction exists among the factors, and in a certain range, along with the change of the water content of the solvent, the extraction time and the feed-liquid ratio, the change trend of the polyphenol yield is firstly increased and then decreased, wherein the interaction of the water content of the solvent and the feed-liquid ratio is obvious in the extraction yield of the total polyphenol of the polygonatum cyrtonema, and the interaction is consistent with the analysis of variance result.
Based on the sample of the polygonatum cyrtonema polyphenol extract obtained by the optimization test, the chemical components of the extract polyphenol are analyzed by adopting ultra-high liquid chromatography-quaternary rod/time-of-flight mass spectrometry (UPLC-Q-TOF-MS/MS). Chromatographic conditions: agilent ultra-high liquid chromatograph 1290, chromatographic column is waters BEH C182.1 x 100mm 1.7um, flow rate is 0.3mL/min, sample injection amount is 5uL, mobile phase A is 0.1% formic acid aqueous solution, mobile phase B is acetonitrile solution, gradient elution ：0～8min,95％～79％A;8～17min,79％～78％A;17～20min,78％～60％A,20～30min,60％～55％A,30～40min,55％～27％A,40～45min,27％～0％A,45～50min,0％～95％A,50～55min,95％A. mass spectrum conditions: agilent Q-TOF6550, electrospray ionization source, mass spectrum scan range: the primary temperature is 50-1500 m/z, and the sheath gas temperature is 350 ℃; the sheath gas flow rate was 12L/min. The analytical results show the main characteristic polyphenol composition as shown in Table 4.
TABLE 4 Main characterization of polyphenols
Through UPLC-Q-TOF-MS/MS analysis, the result shows that the natural eutectic solvent system formed based on betaine-lactic acid can effectively extract and prepare polyphenol substances, 17 main characteristic polyphenol compounds are obtained through screening, and the structural formula is as follows:
At present, the polyphenol substances of Polygonatum cyrtonema Fabricius are mainly found in the aspect of total content detection, characteristic compounds are not analyzed and compared in reports of Polygonatum cyrtonema Fabricius component extraction by utilizing a eutectic solvent, and meanwhile, substances with polyphenol hydroxyl structures such as a compound (2), a compound (7), a compound (9), a compound (10), a compound (13) and a compound (14) are found in the substances for the first time based on a liquid chromatography-mass spectrometry technology, so that the ultrasonic-assisted natural eutectic solvent can realize effective extraction of the polyphenol substances of Polygonatum cyrtonema Fabricius.
Preparing an extracting solution according to the optimized process, concentrating under reduced pressure, and freeze-drying to obtain an extract sample; in addition, DES extraction solvent was replaced with 60% ethanol and water, and samples were prepared with reference to the above extraction process. Sample solutions with different concentration gradients are prepared, and in-vitro antioxidation and xanthine oxidase activity inhibition tests are carried out.
DPPH radical scavenging test
Placing 2.0mL of sample solution with different concentrations in a 10mL colorimetric tube with a plug, adding an equal volume of 0.1mmol/L DPPH ethanol solution, uniformly mixing, placing in a dark place for reaction for 30min, detecting the absorbance value (A 1) at 517nm by using an ultraviolet spectrophotometer, uniformly mixing 2mL of extraction solvent and 2mL of DPPH, measuring the absorbance value (A 2), and measuring the absorbance value (A 0) by using a mixed solution of 2mL of DPPH and 2mL of ethanol as a control group.
As can be seen from fig. 2, the scavenging effect of different types of polygonatum cyrtonema extracts (DES extract, ethanol extract and water extract) on DPPH free radicals all increased with increasing sample concentration, but the scavenging effect of DES extract on DPPH free radicals was significantly higher than that of ethanol extract and water extract in the examined sample concentration range.
ABTS free radical scavenging assay
ABTS stock solution was prepared by mixing ABTS solution (7.4 mM) with potassium persulfate solution (2.6 mM) at a volume ratio of 1:1 and then reacting in the dark for 12 hours. The concentration of the ABTS stock solution was then adjusted with phosphate buffer (200 mM, pH 7.4) to give a absorbance at 734nm of 0.700.+ -. 0.02. Then, 0.05mL of the sample extract with different concentrations is added with 4mL of LABSS working solution respectively, and after being mixed uniformly, the mixture is reacted at room temperature in a dark place for 6min, and the absorbance value (A 1) is measured at 734 nm. A mixed solution sample was prepared as described above using the extraction solvent as a blank control instead of the sample solution, and its absorbance value was measured (A 0).
As can be seen from fig. 3, the scavenging effect of different types of polygonatum cyrtonema extracts (DES extract, ethanol extract and water extract) on ABTS free radicals increases with increasing sample concentration, and although the scavenging effect of different samples on ABTS free radicals at the initial concentration is equivalent, the scavenging effect of DES extract on ABTS free radicals is higher than that of ethanol extract and water extract in the examined sample concentration range with increasing sample concentration.
Xanthine oxidase Activity inhibition assay
Taking 0.6mL of phosphoric acid buffer solution (0.10 mol/L, pH=8.5), 0.2mL of xanthine solution (2.0 mmol/L) and 0.1mL of sample solution with different concentrations, and uniformly mixing in a 1.5mL centrifuge tube; then, 0.2mL of xanthine oxidase solution (0.1U/mL) was added, and the mixture was reacted in a water bath at 25℃for 30 minutes, and after the completion of the reaction, 0.2mL of HCl solution (1.0 mol/L) was added to terminate the reaction. The absorbance was measured at 290 nm.
Wherein: a 1: adding enzyme and not adding absorbance value of the sample group;
a 2: enzyme-free and sample-free absorbance values;
A 3: adding enzyme and adding absorbance value of the sample group;
a 4: no enzyme was added to the absorbance values of the sample groups.
As can be seen from FIG. 4, the inhibition effect of the DES extract on xanthine oxidase was also increased with increasing concentration, wherein the inhibition effect of the DES extract on xanthine oxidase was significantly higher than that of the ethanol extract and the water extract.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be apparent to one skilled in the art that modifications may be made to the technical solutions described in the foregoing embodiments, or equivalents may be substituted for some of the technical features thereof; such modifications and substitutions do not depart from the spirit and scope of the corresponding technical solutions.
Claims (8)
1. A method for extracting polyphenol characteristic components of polygonatum cyrtonema by utilizing ultrasonic wave to assist natural eutectic solvents, which is characterized by comprising the following steps: adding the polygonatum cyrtonema powder into the prepared natural eutectic solvent, wherein the feed liquid ratio of the polygonatum cyrtonema powder sample to the natural eutectic solvent is 1:10-30 g/mL, and extracting by adopting ultrasonic assistance, and the ultrasonic conditions are as follows: the temperature is 25-45 ℃, the power is 50-200W, and the extraction time is 5-35 min; after the extraction is finished, centrifuging the sample solution at 3500-5000 rpm for 5-15 min to obtain supernatant as Polygonatum cyrtonema Sieb extract; then drying to obtain an extract sample; the natural eutectic solvent component comprises betaine and lactic acid; the preparation method comprises the following steps: mixing betaine and lactic acid according to the mass ratio of 2:1-1:2, heating and stirring at 80-100 ℃ until the betaine and lactic acid are in uniform, clear and transparent liquid without crystallization precipitation at room temperature, and adding water according to the mass ratio.
2. The method according to claim 1, wherein the polygonatum cyrtonema powder is prepared by the following steps: taking a fresh collected polygonatum cyrtonema sample, washing, slicing, drying at 40-60 ℃, crushing, sieving with a 60-80 mesh sieve, and placing in a fresh-keeping bag and placing in a dryer for standby.
3. A method according to claim 1, wherein the natural eutectic solvent has a water content of 20 to 50wt%.
4. The method according to claim 1, wherein the natural eutectic solvent prepared from betaine and lactic acid has a water content of 50%, the ratio of the powder sample of Polygonatum cyrtonema to the natural eutectic solvent is 1:19 g/mL, and the extraction time is 35min.
5. The method according to claim 1, wherein the drying is freeze-drying or spray-drying.
6. The method of claim 1, further comprising the step of: the analytical method comprises the steps of analyzing polyphenol chemical components of the Polygonatum cyrtonema Fabricius extract by adopting ultra-high liquid chromatography-four-stage rod/flight time mass spectrometry, wherein chromatographic conditions are as follows: agilent ultra-high liquid chromatograph 1290, chromatographic column is waters BEH C18, flow rate is 0.3mL/min, sample injection amount is 5uL, mobile phase A is 0.1% formic acid aqueous solution, mobile phase B is acetonitrile solution, gradient elution ：0～8min,95％～79％A;8～17min,79％～78％A;17～20min,78％～60％A,20～30min,60％～55％A,30～40min,55％～27％A,40～45min,27％～0％A,45～50min,0％～95％A,50～55min,95％A; mass spectrum conditions: agilent Q-TOF6550, electrospray ionization source, mass spectrum scan range: the primary temperature is 50-1500 m/z, and the sheath gas temperature is 350 ℃;
The sheath gas flow rate was 12L/min.
7. The method according to claim 1 or 6, wherein the number of polyphenols is 17, and the structural formula is as follows:
8. Use of the extract obtained by the method of claim 1 for the preparation of antioxidants and uric acid lowering drugs.
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