CN110665470A - Adsorbent used in propolis extraction process and preparation method thereof - Google Patents
Adsorbent used in propolis extraction process and preparation method thereof Download PDFInfo
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- CN110665470A CN110665470A CN201910902280.8A CN201910902280A CN110665470A CN 110665470 A CN110665470 A CN 110665470A CN 201910902280 A CN201910902280 A CN 201910902280A CN 110665470 A CN110665470 A CN 110665470A
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- propolis
- extraction process
- adsorbent used
- aqueous solution
- chelating agent
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- 241000241413 Propolis Species 0.000 title claims abstract description 53
- 229940069949 propolis Drugs 0.000 title claims abstract description 53
- 239000003463 adsorbent Substances 0.000 title claims abstract description 30
- 238000000605 extraction Methods 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims abstract description 20
- 239000002738 chelating agent Substances 0.000 claims abstract description 16
- 150000007524 organic acids Chemical class 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 229910021536 Zeolite Inorganic materials 0.000 claims description 16
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical group O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 16
- 239000010457 zeolite Substances 0.000 claims description 16
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 229920000858 Cyclodextrin Polymers 0.000 claims description 13
- 239000001116 FEMA 4028 Substances 0.000 claims description 13
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 13
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims description 13
- 229960004853 betadex Drugs 0.000 claims description 13
- 229920000609 methyl cellulose Polymers 0.000 claims description 13
- 239000001923 methylcellulose Substances 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 12
- 229920005552 sodium lignosulfonate Polymers 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 claims description 8
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 2
- 238000007605 air drying Methods 0.000 claims description 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 2
- 235000015165 citric acid Nutrition 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 239000001630 malic acid Substances 0.000 claims description 2
- 235000011090 malic acid Nutrition 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 4
- 239000004480 active ingredient Substances 0.000 abstract description 4
- 239000013522 chelant Substances 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 3
- 230000000717 retained effect Effects 0.000 abstract 1
- 229930003935 flavonoid Natural products 0.000 description 10
- 235000017173 flavonoids Nutrition 0.000 description 10
- 235000010981 methylcellulose Nutrition 0.000 description 10
- 150000002215 flavonoids Chemical class 0.000 description 6
- 239000007787 solid Substances 0.000 description 5
- -1 flavonoid compound Chemical class 0.000 description 4
- 206010028980 Neoplasm Diseases 0.000 description 3
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 3
- 230000003078 antioxidant effect Effects 0.000 description 3
- 239000008280 blood Substances 0.000 description 3
- 210000004369 blood Anatomy 0.000 description 3
- 201000011510 cancer Diseases 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229930003944 flavone Natural products 0.000 description 3
- 150000002212 flavone derivatives Chemical class 0.000 description 3
- 235000011949 flavones Nutrition 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 3
- 241000257303 Hymenoptera Species 0.000 description 2
- 206010061218 Inflammation Diseases 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000036039 immunity Effects 0.000 description 2
- 230000004054 inflammatory process Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 201000001320 Atherosclerosis Diseases 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- OEIJRRGCTVHYTH-UHFFFAOYSA-N Favan-3-ol Chemical compound OC1CC2=CC=CC=C2OC1C1=CC=CC=C1 OEIJRRGCTVHYTH-UHFFFAOYSA-N 0.000 description 1
- CITFYDYEWQIEPX-UHFFFAOYSA-N Flavanol Natural products O1C2=CC(OCC=C(C)C)=CC(O)=C2C(=O)C(O)C1C1=CC=C(O)C=C1 CITFYDYEWQIEPX-UHFFFAOYSA-N 0.000 description 1
- 208000031226 Hyperlipidaemia Diseases 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 208000007536 Thrombosis Diseases 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 238000009098 adjuvant therapy Methods 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000002155 anti-virotic effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 150000003934 aromatic aldehydes Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 235000013871 bee wax Nutrition 0.000 description 1
- 239000012166 beeswax Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000002481 ethanol extraction Methods 0.000 description 1
- 235000011987 flavanols Nutrition 0.000 description 1
- HVQAJTFOCKOKIN-UHFFFAOYSA-N flavonol Natural products O1C2=CC=CC=C2C(=O)C(O)=C1C1=CC=CC=C1 HVQAJTFOCKOKIN-UHFFFAOYSA-N 0.000 description 1
- 150000007946 flavonol Chemical class 0.000 description 1
- 235000011957 flavonols Nutrition 0.000 description 1
- 230000007760 free radical scavenging Effects 0.000 description 1
- 210000004907 gland Anatomy 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000004165 myocardium Anatomy 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 230000004792 oxidative damage Effects 0.000 description 1
- 230000036542 oxidative stress Effects 0.000 description 1
- 210000003254 palate Anatomy 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 150000007965 phenolic acids Chemical class 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000022558 protein metabolic process Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L21/00—Marmalades, jams, jellies or the like; Products from apiculture; Preparation or treatment thereof
- A23L21/20—Products from apiculture, e.g. royal jelly or pollen; Substitutes therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/165—Natural alumino-silicates, e.g. zeolites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2300/00—Processes
- A23V2300/14—Extraction
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4837—Lignin
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Nutrition Science (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Jellies, Jams, And Syrups (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
Abstract
The invention relates to an adsorbent used in a propolis extraction process, which comprises the following raw materials in parts by weight: 10-20 parts of carrier, 50-200 parts of organic acid aqueous solution and 50-200 parts of chelating agent; the invention also discloses a preparation method of the adsorbent used in the propolis extraction process. The technical scheme of the invention provides the adsorbent which can chelate heavy metal ions possibly contained in the propolis to the maximum extent in the extraction process of the propolis and can not introduce impurities in the subsequent alcohol extraction step, the heavy metal removal step in the extraction process of the propolis can be simplified, the adsorbent can be recycled, and effective active ingredients in the propolis can be retained to the maximum extent.
Description
Technical Field
The invention belongs to the technical field of natural product extraction, and particularly relates to an adsorbent used in a propolis extraction process and a preparation method thereof.
Background
Propolis is a gum collected by bees from buds and buds, and is a colloidal solid with special aromatic odor formed by combining the secretions of the palate glands of the bees and beeswax. Propolis is called purple gold, and has the main active ingredients of flavonoids, organic acids, terpenes, aromatic aldehydes, esters, various amino acids, vitamins, mineral substances and the like, has physiological functions of bacteriostasis, antivirus, antioxidation, cancer prevention and resistance, immunity regulation and the like, can regulate hyperlipidemia, hypertension and the like by oral administration of propolis, and prevents atherosclerosis and thrombosis, and is known as blood cleaner. Propolis is also called 'treasury of flavonoids', and mainly comprises flavone, flavonol, flavanol, phenolic acid and the like, wherein 5-hydroxy-5-4, 7-dimethoxy dihydroflavone and 5, 7-dihydroxy-3, 4-dimethoxy flavone are special components of propolis, and the physiological and pharmacological activities of most of propolis are related to the compounds. The antioxidant activity of the flavonoid compound is closely related to the molecular structure of the flavonoid compound, 3, 4-dihydroxy on the B ring of the flavonoid compound is a key part for eliminating free radicals, and the antioxidant effect of the flavonoid compound can be improved to different degrees by hydroxyl on other rings. Free radicals are the normal metabolites of an organism, normally in a dynamic equilibrium of production and clearance; under the condition of oxidative stress, the propolis flavone has good free radical scavenging activity, and can cause oxidative damage of organism and diseases such as aging, inflammation and cancer.
The propolis has wide health-care function and adjuvant therapy function. The research shows that the propolis has the functions of delaying grease aging, regulating immunity, resisting bacteria, inflammation, virus, cancer and radiation, eliminating free radicals, and reducing blood sugar and blood fat. In addition, the research shows that the propolis can regulate the protein metabolism in the body of a diabetic rat and has a protective effect on the kidney of the body. In addition, literature research shows that propolis and its active components can protect damaged cardiac muscle and improve antioxidant index. However, propolis has special physical and chemical properties, is insoluble in water, has high viscosity at normal temperature, and is not beneficial to processing. Although propolis resources in China are rich, the number of propolis products on the market is small, and the problems that heavy metals are difficult to remove and more propolis active ingredients are lost in the heavy metal removing process are more existed.
Disclosure of Invention
The invention aims to provide an adsorbent which can chelate heavy metal ions possibly contained in propolis to the maximum extent in the extraction process of the propolis without introducing impurities in the subsequent alcohol extraction step, can simplify the heavy metal removal step in the extraction process of the propolis, can be recycled, and can retain effective active ingredients in the propolis to the maximum extent.
The technical scheme adopted by the invention for realizing the purpose is as follows: an adsorbent used in the propolis extraction process comprises the following raw materials in parts by weight: 10-20 parts of carrier, 50-200 parts of organic acid aqueous solution and 50-200 parts of chelating agent;
further, the carrier is 50-80 mesh zeolite;
further, the organic acid aqueous solution is an aqueous solution with the mass fraction of organic acid of 20-40%;
further, the organic acid is one or more of malic acid, oxalic acid, citric acid and tartaric acid;
further, the chelating agent is an aqueous solution of one or a mixture of more of beta-cyclodextrin, methylcellulose and sodium lignosulfonate;
further, the chelating agent is an aqueous solution of a mixture of beta-cyclodextrin, methylcellulose and sodium lignosulfonate in a mass ratio of 5:1-3: 1-3;
further, the chelating agent is an aqueous solution with the mass fraction of 30-50% of a mixture of beta-cyclodextrin, methylcellulose and sodium lignosulfonate at the mass ratio of 5:1-3: 1-3;
the invention also discloses a preparation method of the adsorbent used in the propolis extraction process, which comprises the following specific steps; pulverizing zeolite into 50-80 mesh powder, heating and soaking with organic acid solution, filtering, adding chelating agent, soaking, filtering, and air drying;
further, the heating temperature is 50-70 ℃, and the organic acid solution dipping time is 1-5 h;
further, the immersion time of the chelating agent is 1-5 h.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
the zeolite impregnated with the organic acidic agent has the characteristics of being more suitable as a carrier of the chelating agent, and simultaneously, the zeolite can be in a slightly acidic environment, and the chelating agent and heavy metals such as Pb can be improved2+The chelating agent compounded by beta-cyclodextrin, methylcellulose and sodium lignosulfonate can chelate heavy metal ions possibly contained in propolis to the maximum extent and is insoluble in ethanol, impurities are not introduced in the subsequent ethanol extraction step, and the methylcellulose and the lignin are not introducedThe sodium sulfonate crosslinking can prevent beta-cyclodextrin and chelated heavy metal from desorbing from zeolite carrier and only need to use lower dosage of beta-cyclodextrin, the porous structure on the surface of zeolite can enlarge the contact area with propolis, thus improving the efficiency of removing heavy metal.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A method for preparing adsorbent used in propolis extraction process comprises:
crushing 100g of zeolite into 50-mesh powder, soaking the powder for 1h at 50 ℃ by using 2L of aqueous solution with the citric acid mass fraction of 20%, filtering, soaking the solid in 2L of aqueous solution with the beta-cyclodextrin, the methylcellulose and the sodium lignosulfonate mass ratio of 5:1:1, wherein the mixture is 30% in mass fraction, filtering and airing to obtain the heavy metal adsorbent based on the zeolite. .
Example 2
A method for preparing adsorbent used in propolis extraction process comprises:
crushing 100g of zeolite into 50-mesh powder, soaking the powder for 1h at 50 ℃ by using 2L of aqueous solution with the citric acid mass fraction of 30%, filtering, soaking the solid in 2L of aqueous solution with the beta-cyclodextrin, the methylcellulose and the sodium lignosulfonate mass ratio of 5:1:1, wherein the mass fraction of the mixture is 40%, filtering and airing to obtain the heavy metal adsorbent based on the zeolite.
Example 3
A method for preparing adsorbent used in propolis extraction process comprises:
crushing 100g of zeolite into 50-mesh powder, soaking the powder for 1h at 50 ℃ by using 2L of aqueous solution with the citric acid mass fraction of 40%, filtering, soaking the solid in 2L of aqueous solution with the beta-cyclodextrin, the methylcellulose and the sodium lignosulfonate mass ratio of 5:1:1, wherein the mixture is 50% in mass fraction, filtering and airing to obtain the heavy metal adsorbent based on the zeolite.
Comparative example
A method for preparing adsorbent used in propolis extraction process comprises:
crushing 100g of zeolite into 50-mesh powder, soaking the powder for 1h at 50 ℃ by using 2L of deionized water, filtering, soaking the solid in an aqueous solution of which the mass fraction is 50% of a mixture of 2L of beta-cyclodextrin, methylcellulose and sodium lignosulfonate and the mass ratio of the methyl cellulose to the sodium lignosulfonate is 5:1:1, filtering and airing to obtain the heavy metal adsorbent based on the zeolite.
Example 4
The adsorbents used in the extraction process of propolis obtained in examples 1-3 and the adsorbents obtained in the comparative examples were used for removing heavy metals in the extraction process of propolis, and the contents of total flavonoids and lead in the obtained product propolis (all referred to as propolis extract in the table) were calculated.
TABLE 1 lead content and Total Flavonoids content*Measured value
| Example 1 | Example 2 | Example 3 | Comparative example | |
| Raw material lead content/ppm | 35.27 | 35.27 | 35.27 | 35.27 |
| Propolis extract with lead content/ppm | 0.017 | 0.016 | 0.016 | 0.19 |
| The total flavone content of propolis extract is mg-1 | 297.43 | 297.18 | 298.51 | 295.76 |
Injecting: the method for measuring lead comprises the following steps: refer to GB/T5009.12 method for measuring lead in food. The method for measuring the content of the total flavonoids in the propolis comprises the following steps: referring to a method for measuring the content of total flavonoids in GB/T24283-2018.
The above embodiments are only for illustrating the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention accordingly, and not to limit the protection scope of the present invention accordingly. All equivalent changes or modifications made in accordance with the spirit of the present disclosure are intended to be covered by the scope of the present disclosure.
Claims (10)
1. The adsorbent used in the propolis extraction process is characterized by comprising the following raw materials in parts by weight: 10-20 parts of carrier, 50-200 parts of organic acid aqueous solution and 50-200 parts of chelating agent.
2. The adsorbent used in the propolis extraction process as claimed in claim 1, wherein the carrier is zeolite of 50-80 mesh.
3. The adsorbent used in the propolis extraction process according to claim 1, wherein the aqueous solution of organic acid is an aqueous solution having a mass fraction of organic acid of 20-40%.
4. The adsorbent used in the propolis extraction process as claimed in claim 3, wherein the organic acid is one or more of malic acid, oxalic acid, citric acid, and tartaric acid.
5. The adsorbent used in the propolis extraction process according to claim 1, wherein the chelating agent is an aqueous solution of one or more of beta-cyclodextrin, methylcellulose, and sodium lignosulfonate.
6. The adsorbent used in the propolis extraction process according to claim 5, wherein the chelating agent is an aqueous solution of a mixture of β -cyclodextrin, methylcellulose, and sodium lignosulfonate at a mass ratio of 5:1-3: 1-3.
7. The adsorbent used in the propolis extraction process as claimed in claim 6, wherein the chelating agent is an aqueous solution of 30-50% by mass of a mixture of β -cyclodextrin, methylcellulose, and sodium lignosulfonate at a mass ratio of 5:1-3: 1-3.
8. The method for preparing the adsorbent used in the propolis extraction process according to any one of claims 1 to 7, wherein the specific steps are as follows; pulverizing zeolite into 50-80 mesh powder, soaking in organic acid solution under heating, filtering, adding chelating agent, soaking, filtering, and air drying.
9. The method for preparing the adsorbent used in the propolis extraction process according to claim 8, wherein the heating temperature is 50-70 ℃ and the organic acid solution immersion time is 1-5 hours.
10. The method of preparing an adsorbent used in the propolis extraction process as claimed in claim 8, wherein the chelating agent is impregnated for 1-5 hours.
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