CN110639226A - Method for removing impurities in propolis - Google Patents
Method for removing impurities in propolis Download PDFInfo
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- CN110639226A CN110639226A CN201910902287.XA CN201910902287A CN110639226A CN 110639226 A CN110639226 A CN 110639226A CN 201910902287 A CN201910902287 A CN 201910902287A CN 110639226 A CN110639226 A CN 110639226A
- Authority
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- Prior art keywords
- propolis
- removing impurities
- solution
- powder
- mass
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- 241000241413 Propolis Species 0.000 title claims abstract description 145
- 229940069949 propolis Drugs 0.000 title claims abstract description 145
- 239000012535 impurity Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 29
- 229910001385 heavy metal Inorganic materials 0.000 claims abstract description 29
- 239000000243 solution Substances 0.000 claims description 57
- 239000000843 powder Substances 0.000 claims description 48
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- 229910021536 Zeolite Inorganic materials 0.000 claims description 31
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 31
- 239000010457 zeolite Substances 0.000 claims description 31
- 238000003756 stirring Methods 0.000 claims description 30
- 239000007787 solid Substances 0.000 claims description 22
- 239000003463 adsorbent Substances 0.000 claims description 19
- HDSBZMRLPLPFLQ-UHFFFAOYSA-N Propylene glycol alginate Chemical compound OC1C(O)C(OC)OC(C(O)=O)C1OC1C(O)C(O)C(C)C(C(=O)OCC(C)O)O1 HDSBZMRLPLPFLQ-UHFFFAOYSA-N 0.000 claims description 17
- 239000000770 propane-1,2-diol alginate Substances 0.000 claims description 17
- 235000010409 propane-1,2-diol alginate Nutrition 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 16
- 239000000284 extract Substances 0.000 claims description 14
- 238000000605 extraction Methods 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 14
- 238000002791 soaking Methods 0.000 claims description 14
- 239000002798 polar solvent Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000010298 pulverizing process Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 229920001213 Polysorbate 20 Polymers 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000004821 distillation Methods 0.000 claims description 8
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 claims description 8
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 claims description 8
- 239000002738 chelating agent Substances 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 238000002386 leaching Methods 0.000 claims description 7
- 238000001694 spray drying Methods 0.000 claims description 7
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 6
- 150000007524 organic acids Chemical class 0.000 claims description 6
- 239000012266 salt solution Substances 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000013871 bee wax Nutrition 0.000 abstract description 14
- 239000012166 beeswax Substances 0.000 abstract description 14
- 235000015097 nutrients Nutrition 0.000 abstract description 2
- 230000000717 retained effect Effects 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 description 23
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 18
- 238000001914 filtration Methods 0.000 description 16
- 229930003935 flavonoid Natural products 0.000 description 11
- 235000017173 flavonoids Nutrition 0.000 description 11
- 229920000858 Cyclodextrin Polymers 0.000 description 10
- 239000001116 FEMA 4028 Substances 0.000 description 10
- 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 description 10
- 235000011175 beta-cyclodextrine Nutrition 0.000 description 10
- 229960004853 betadex Drugs 0.000 description 10
- 229920000609 methyl cellulose Polymers 0.000 description 9
- 239000001923 methylcellulose Substances 0.000 description 9
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 8
- 150000002215 flavonoids Chemical class 0.000 description 7
- 229920005552 sodium lignosulfonate Polymers 0.000 description 7
- 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 5
- 230000000052 comparative effect Effects 0.000 description 5
- 229930003944 flavone Natural products 0.000 description 5
- 150000002212 flavone derivatives Chemical class 0.000 description 5
- 235000011949 flavones Nutrition 0.000 description 5
- -1 flavonoid compound Chemical class 0.000 description 5
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 4
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 4
- 235000017557 sodium bicarbonate Nutrition 0.000 description 4
- 206010028980 Neoplasm Diseases 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
- 230000000694 effects Effects 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- XHFLOLLMZOTPSM-UHFFFAOYSA-M sodium;hydrogen carbonate;hydrate Chemical compound [OH-].[Na+].OC(O)=O XHFLOLLMZOTPSM-UHFFFAOYSA-M 0.000 description 3
- 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 description 2
- 241000257303 Hymenoptera Species 0.000 description 2
- 206010061218 Inflammation Diseases 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 description 2
- 230000036039 immunity Effects 0.000 description 2
- 230000004054 inflammatory process Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000001993 wax Substances 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
- 208000007536 Thrombosis Diseases 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 238000009098 adjuvant therapy Methods 0.000 description 1
- 235000001014 amino acid Nutrition 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
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 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
- 239000012530 fluid Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000007760 free radical scavenging Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing 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
- 150000002500 ions Chemical class 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 235000010755 mineral Nutrition 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
- 229940074127 propolis wax Drugs 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
- 235000007586 terpenes Nutrition 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
- B01D11/028—Flow sheets
- B01D11/0284—Multistage extraction
-
- 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
-
- 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
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
-
- 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
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/20—Removal of unwanted matter, e.g. deodorisation or detoxification
- A23L5/27—Removal of unwanted matter, e.g. deodorisation or detoxification by chemical treatment, by adsorption or by absorption
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K35/00—Medicinal preparations containing materials or reaction products thereof with undetermined constitution
- A61K35/56—Materials from animals other than mammals
- A61K35/63—Arthropods
- A61K35/64—Insects, e.g. bees, wasps or fleas
- A61K35/644—Beeswax; Propolis; Royal jelly; Honey
-
- 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
- B01D11/0288—Applications, solvents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
- B01D15/38—Selective adsorption, e.g. chromatography characterised by the separation mechanism involving specific interaction not covered by one or more of groups B01D15/265 - B01D15/36
-
- 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
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
- B01D15/38—Selective adsorption, e.g. chromatography characterised by the separation mechanism involving specific interaction not covered by one or more of groups B01D15/265 - B01D15/36
- B01D2015/3838—Ligand exchange chromatography, e.g. complexation chromatography, chelation chromatography, metal interaction chromatography
Abstract
The invention relates to a method for removing impurities in propolis, which comprises the following specific steps: pretreating, removing impurities, extracting and preparing. According to the technical scheme, the impurities such as beeswax and heavy metals in the propolis can be removed without high pressure and high temperature, so that the impurities such as beeswax and heavy metals in the propolis can be removed to the maximum extent, the loss of a large amount of effective components in the propolis can be avoided, and the nutrient components 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 a method for removing impurities in propolis.
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 beeswax residues are more exist mostly.
Disclosure of Invention
The invention aims to provide a method for removing impurities in propolis without high pressure and high temperature, which can remove the impurities such as beeswax, heavy metal and the like in the propolis to the maximum extent without causing large loss of effective components in the propolis and retain the nutrient components in the propolis to the maximum extent.
The technical scheme adopted by the invention for realizing the purpose is as follows: a method for removing impurities in propolis comprises the following steps:
1) pretreatment: pulverizing propolis raw material at low temperature to obtain propolis powder, dissolving propolis powder in deionized water 2-5 times of its mass, adding dispersant, stirring, adding inorganic salt solution, heating and stirring for 20-60min, cooling, standing, and removing solid to obtain pretreatment solution;
2) removing impurities: uniformly stirring the pretreatment solution obtained in the step 1), adding a heavy metal adsorbent based on zeolite, stirring for 20-60min, standing, and removing solids to obtain a propolis solution;
3) extraction and preparation: dissolving the propolis solution obtained in the step 2) in a polar solvent with the mass 1-5 times of that of the propolis solution, heating and pressurizing for leaching for 2-7h, then carrying out reduced pressure distillation and recovering the polar solvent, and carrying out spray drying to obtain an impurity-removed propolis extract;
further, the low-temperature crushing temperature in the step 1) is 0-5 ℃;
furthermore, the low-temperature crushing temperature in the step 1) is 3-5 ℃;
further, the cooling and standing temperature in the step 1) is-5-15 ℃;
further, in the step 1), the propolis raw material is crushed to 60-80 meshes;
further, the inorganic salt solution in the step 1) is one or a mixture of more of sodium bicarbonate, sodium chloride and sodium carbonate;
further, the inorganic salt solution in the step 1) is an aqueous solution of sodium bicarbonate;
further, the dispersing agent in the step 1) is one or a mixture of more of propylene glycol alginate, starch sugar ester and polyoxyethylene sorbitan monolaurate;
further, in the step 1), the dispersing agent is propylene glycol alginate or a mixture of the propylene glycol alginate and polyoxyethylene sorbitan monolaurate in a mass ratio of 2: 0.3-0.5;
further, heating and stirring for 20-30min in the step 2);
further, the preparation method of the zeolite-based heavy metal adsorbent in the step 2) is as follows: pulverizing zeolite into 50-80 mesh powder, soaking with organic acid solution at 50-70 deg.C, and adding chelating agent for soaking;
furthermore, the organic acid solution is an aqueous solution with the citric acid mass fraction of 20-40%, and the chelating agent is an aqueous solution of beta-cyclodextrin, methylcellulose and sodium lignosulfonate;
furthermore, the amount of the organic acid solution is 5 to 20 times of the mass of the powder;
furthermore, 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;
further, the polar solvent in the step 3) is one or more of water, ethanol and acetone;
further, the polar solvent in the step 3) is ethanol water solution with the mass fraction of 80-99.5%;
further, the dosage of the polar solvent in the step 3) is 1-2 times of that of the propolis solution;
further, in the step 3), the heating temperature is 40-70 ℃, and the pressurizing pressure is 0.2-0.5 MPa;
furthermore, the heating temperature in the step 3) is 40-50 ℃, and the pressurizing pressure is 0.2-0.3 MPa.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
(1) by adding propylene glycol alginate or a mixture of propylene glycol alginate and polyoxyethylene sorbitan monolaurate as a dispersing agent, on one hand, flavonoid, organic acid and aromatic aldehyde compounds in the propolis can be emulsified, homogenized and dispersed in an aqueous solution, and on the other hand, a proper amount of propylene glycol alginate has a certain microgel effect and can assist active ingredients in the propolis to stably exist in a grid formed by crosslinking the propylene glycol alginate;
(2) the pH of the aqueous solution of the propolis raw material is adjusted by using sodium bicarbonate as an inorganic salt to enable the environment to be alkalescent, and the excessive esters in the propolis raw material, namely the useless components in the beeswax which is generally considered, can be effectively removed after heating, and the wax removing temperature can be obviously lower than the heating temperature required in the traditional propolis wax removing process by compounding the mixture of propylene glycol alginate or propylene glycol alginate and polyoxyethylene sorbitan monolaurate, so that the loss of effective active components in the propolis is reduced to the maximum extent;
(3) 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 efficiency is high, heavy metal ions possibly contained in the propolis can be chelated to the maximum extent by a chelating agent compounded by the beta-cyclodextrin, the methylcellulose and the sodium lignin sulfonate and insoluble in ethanol, impurities cannot be introduced in the subsequent alcohol extraction step, the beta-cyclodextrin and the chelated heavy metal can be prevented from being desorbed from a zeolite carrier by crosslinking of the methylcellulose and the sodium lignin sulfonate, the beta-cyclodextrin with a lower dosage is only needed to be used, and the contact area between the zeolite surface porous structure and the propolis can be enlarged, so that the heavy metal removal efficiency is improved;
(4) by using 80-99.5% of ethanol aqueous solution as a polar solvent, propylene glycol alginate or a mixture of propylene glycol alginate and polyoxyethylene sorbitan monolaurate is not introduced in the alcohol extraction process of the propolis, impurities are prevented from being introduced to a greater extent, and the highly homogenized aqueous solution after wax and heavy metal removal improves the efficiency of the alcohol extraction process, so that the extraction of effective components in the propolis can be realized without high temperature and high pressure, excessive crushing is not required in the pretreatment process of the propolis by using a dispersing agent, and the propolis alcohol has the effects of no energy waste and low equipment requirement so as to reduce the production cost, and is suitable for large-scale production and use; the activity of the effective components in the product is not influenced by high temperature.
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 removing impurities in propolis comprises the following steps;
1) pretreatment: crushing a propolis raw material at a low temperature of 3 ℃ to 60 meshes to obtain propolis powder, dissolving the propolis powder in deionized water 2 times the mass of the propolis powder, adding a mixture of propylene glycol alginate 0.01 time the mass of the propolis powder and polyoxyethylene sorbitan monolaurate in a mass ratio of 2:0.3, uniformly stirring, adding a sodium bicarbonate aqueous solution 0.5 time the mass of the propolis powder and accounting for 60% of the mass fraction of the propolis powder, heating to 50 ℃, stirring for 30min, cooling to 25 ℃, standing for 0.5h, and performing refrigerated centrifugation at 3000r/min to remove solids to obtain a pretreatment solution;
2) removing impurities: uniformly stirring the pretreatment solution obtained in the step 1), adding a zeolite-based heavy metal adsorbent with the same mass as the propolis powder, stirring for 30min, standing for 0.5h, and filtering to remove solids to obtain a propolis solution;
3) extraction and preparation: dissolving the propolis solution obtained in the step 2) in 90% ethanol aqueous solution with mass fraction 1 time of the mass of the propolis solution, leaching for 4h at 50 ℃ under 0.2MPa, and then carrying out reduced pressure distillation and recovering ethanol to obtain the propolis non-critical fluid extract.
The preparation method of the zeolite-based heavy metal adsorbent comprises the following steps:
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.
Example 2
A method for removing impurities in propolis comprises the following steps;
1) pretreatment: pulverizing propolis raw material at 5 deg.C to 60 mesh to obtain propolis powder, dissolving propolis powder in deionized water 2 times its mass, adding propylene glycol alginate 0.01 times the mass of propolis powder, stirring, adding 40% sodium bicarbonate water solution 0.5 times the mass of propolis powder, heating to 50 deg.C, stirring for 30min, cooling to 25 deg.C, standing for 0.5h, and centrifuging at 3000r/min to remove solid to obtain pretreated solution;
2) removing impurities: uniformly stirring the pretreatment solution obtained in the step 1), adding a zeolite-based heavy metal adsorbent with the same mass as the propolis powder, stirring for 30min, standing for 0.5h, and filtering to remove solids to obtain a propolis solution;
3) extraction and preparation: dissolving the propolis solution obtained in the step 2) in 80% ethanol aqueous solution with mass fraction of 1 time of the mass of the propolis solution, leaching for 4h at 50 ℃ under 0.3MPa, then carrying out reduced pressure distillation and recovering ethanol, and carrying out spray drying to obtain the impurity-removed propolis extract. The preparation method of the zeolite-based heavy metal adsorbent comprises the following steps:
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.
Example 3
A method for removing impurities in propolis comprises the following steps;
1) pretreatment: pulverizing propolis raw material at 5 ℃ to 80 meshes to obtain propolis powder, dissolving the propolis powder in deionized water with the mass of 3 times of that of the propolis powder, adding a mixture of propylene glycol alginate and polyoxyethylene sorbitan monolaurate with the mass ratio of 2:0.3, the mass of which is 0.02 time of that of the propolis powder, uniformly stirring, adding a sodium bicarbonate aqueous solution with the mass fraction of 40%, the mass of which is 0.5 time of that of the propolis powder, heating to 50 ℃, stirring for 30min, cooling to 25 ℃, standing for 0.5h, and freezing and centrifuging at 3000r/min to remove solids to obtain a pretreatment solution;
2) removing impurities: uniformly stirring the pretreatment solution obtained in the step 1), adding a zeolite-based heavy metal adsorbent with the same mass as the propolis powder, stirring for 30min, standing for 0.5h, and filtering to remove solids to obtain a propolis solution;
3) extraction and preparation: dissolving the propolis solution obtained in the step 2) in an ethanol aqueous solution with the mass fraction of 95% and the mass of 2 times of the propolis solution, leaching for 3 hours at 50 ℃ and 0.2MPa, then carrying out reduced pressure distillation and recovering ethanol, and carrying out spray drying to obtain the impurity-removed propolis extract.
The preparation method of the zeolite-based heavy metal adsorbent comprises the following steps:
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.
Example 4
A method for removing impurities in propolis comprises the following steps;
1) pretreatment: pulverizing propolis raw material at 5 deg.C to 80 mesh to obtain propolis powder, dissolving propolis powder in deionized water 3 times its mass, adding propylene glycol alginate 0.02 times the mass of propolis powder, stirring, adding 40% sodium bicarbonate water solution 0.5 times the mass of propolis powder, heating to 50 deg.C, stirring for 30min, cooling to 25 deg.C, standing for 0.5h, and centrifuging at 3000r/min to remove solid to obtain pretreated solution;
2) removing heavy metals: uniformly stirring the pretreatment solution obtained in the step 1), adding a zeolite-based heavy metal adsorbent with the same mass as the propolis powder, stirring for 30min, standing for 0.5h, and filtering to remove solids to obtain a propolis solution;
3) extraction and preparation: dissolving the propolis solution obtained in the step 2) in an ethanol water solution with the mass fraction of 99.5 percent, which is 2 times of the mass of the propolis solution, extracting for 2 hours at 40 ℃ under 0.2MPa, then carrying out reduced pressure distillation and recovering ethanol, and carrying out spray drying to obtain the impurity-removed propolis extract.
The preparation method of the zeolite-based heavy metal adsorbent comprises the following steps:
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 1
A process for removing impurities in propolis comprises the following steps;
1) pretreatment: pulverizing propolis raw material at 5 deg.C to 80 mesh to obtain propolis powder, dissolving propolis powder in 3 times of deionized water, adding 40% sodium bicarbonate water solution 0.5 times of propolis powder, heating to 50 deg.C and stirring for 30min, cooling to 25 deg.C, standing for 0.5 hr, and centrifuging at 3000r/min to remove solid to obtain pretreatment solution;
2) removing impurities: adding a zeolite-based heavy metal adsorbent with the same mass as the propolis powder into the pretreatment solution obtained in the step 1), stirring for 30min, standing for 0.5h, and filtering to remove solids to obtain a propolis solution;
3) extraction and preparation: dissolving the propolis solution obtained in the step 2) in an ethanol water solution with the mass fraction of 99.5 percent, the mass of the propolis solution is 2 times that of the propolis solution, leaching for 5 hours at 40 ℃ and 0.2MPa, then carrying out reduced pressure distillation and recovering ethanol, and carrying out spray drying to obtain the propolis extract product.
The preparation method of the zeolite-based heavy metal adsorbent comprises the following steps:
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 2
A process for removing impurities in propolis comprises the following steps;
1) pretreatment: pulverizing propolis raw material at 5 deg.C to 80 mesh to obtain propolis powder, dissolving the propolis powder obtained in step 1) in deionized water 3 times its mass, heating to 70 deg.C and stirring for 30min, cooling to 25 deg.C, standing for 0.5h, and centrifuging at 3000r/min to remove solid to obtain pretreatment solution;
2) removing impurities: adding propylene glycol alginate which is 0.02 times of the mass of the propolis powder into the pretreatment solution obtained in the step 1), uniformly stirring, adding 50-mesh zeolite which is equal to the mass of the propolis powder, stirring for 30min, standing for 0.5h, and filtering to remove solids to obtain a propolis solution;
3) extraction and preparation: dissolving the propolis solution obtained in the step 2) in an ethanol water solution with the mass fraction of 99.5 percent, the mass of the propolis solution is 2 times that of the propolis solution, leaching for 5 hours at 40 ℃ and 0.2MPa, then carrying out reduced pressure distillation and recovering ethanol, and carrying out spray drying to obtain the propolis extract product.
Example 5
The contents of total flavonoids and lead in the depurated propolis extracts obtained in examples 1-4 and the propolis products obtained in comparative examples 1-2 (in tables, the propolis extracts are abbreviated as propolis extracts) are calculated, the beeswax obtained in the extraction process of the propolis extracts is taken out, dried and weighed, and the yield of the beeswax and the content of the total flavonoids in the beeswax are calculated according to the weight of the propolis raw materials.
TABLE 1 lead content, beeswax yield, total flavone content in propolis and beeswax*Measured value
| Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 | |
| Raw material lead content/ppm | 36.52 | 36.52 | 36.52 | 36.52 | 36.52 | 36.52 |
| Propolis extract with lead content/ppm | 0.014 | 0.016 | 0.010 | 0.011 | 0.16 | 0.25 |
| The total flavone content of propolis extract is mg-1 | 305.77 | 302.12 | 303.54 | 308.64 | 303.29 | 297.36 |
| Yield of beeswax | 52.72 | 52.15 | 53.74 | 52.33 | 47.58 | 17.85 |
| G-1 g of beeswax total flavone content/mg | 6.12 | 6.45 | 6.01 | 6.02 | 12.97 | 19.73 |
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 and the beeswax 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. A method for removing impurities in propolis is characterized by comprising the following specific steps:
1) pretreatment: pulverizing propolis raw material at low temperature to obtain propolis powder, dissolving propolis powder in deionized water 2-5 times of its mass, adding dispersant, stirring, adding inorganic salt solution, heating and stirring for 20-60min, cooling, standing, and removing solid to obtain pretreatment solution;
2) removing impurities: uniformly stirring the pretreatment solution obtained in the step 1), adding a heavy metal adsorbent based on zeolite, stirring for 20-60min, standing, and removing solids to obtain a propolis solution;
3) extraction and preparation: dissolving the propolis solution obtained in the step 2) in a polar solvent with the mass 1-5 times of that of the propolis solution, heating and pressurizing for leaching for 2-7h, then carrying out reduced pressure distillation and recovering the polar solvent, and carrying out spray drying to obtain the impurity-removed propolis extract.
2. The method for removing impurities from propolis according to claim 1, wherein the low-temperature pulverization temperature in step 1) is 0 to 5 ℃.
3. The method for removing impurities from propolis according to claim 1, wherein the propolis raw material is pulverized to 60-80 mesh in step 1).
4. The method for removing impurities in propolis according to claim 1, wherein the inorganic salt solution in step 1) is one or a mixture of sodium bicarbonate, sodium chloride and sodium carbonate.
5. The method for removing impurities in propolis according to claim 1, wherein the dispersing agent in step 1) is one or a mixture of propylene glycol alginate, starch sugar ester, polyoxyethylene sorbitan monolaurate.
6. The method for removing impurities from propolis according to claim 1, wherein the zeolite-based heavy metal adsorbent in step 2) is prepared by the following method: pulverizing zeolite into 50-80 mesh powder, soaking in organic acid solution at 50-70 deg.C, and adding chelating agent for soaking.
7. The method for removing impurities in propolis according to claim 1, wherein the polar solvent in step 3) is one or more of water, ethanol, and acetone.
8. The method for removing impurities from propolis as claimed in claim 7, wherein the polar solvent in step 3) is an aqueous ethanol solution with a mass fraction of 80-99.5%.
9. The method for removing impurities from propolis according to claim 1, wherein the amount of the polar solvent used in step 3) is 1-2 times that of the propolis solution.
10. The method for removing impurities from propolis as claimed in claim 1, wherein the heating temperature in step 3) is 40-70 ℃ and the pressure is 0.2-0.5 MPa.
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