CN110898083A - Propolis extract and preparation method thereof - Google Patents
Propolis extract and preparation method thereof Download PDFInfo
- Publication number
- CN110898083A CN110898083A CN201911306351.4A CN201911306351A CN110898083A CN 110898083 A CN110898083 A CN 110898083A CN 201911306351 A CN201911306351 A CN 201911306351A CN 110898083 A CN110898083 A CN 110898083A
- Authority
- CN
- China
- Prior art keywords
- negative pressure
- petroleum ether
- extraction
- layer
- concentrating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 241000241413 Propolis Species 0.000 title claims abstract description 47
- 229940069949 propolis Drugs 0.000 title claims abstract description 47
- 238000000605 extraction Methods 0.000 title claims abstract description 34
- 239000000284 extract Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 56
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000003208 petroleum Substances 0.000 claims abstract description 34
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 238000001914 filtration Methods 0.000 claims abstract description 18
- 238000007710 freezing Methods 0.000 claims abstract description 17
- 230000008014 freezing Effects 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000010413 mother solution Substances 0.000 claims abstract description 10
- 238000010992 reflux Methods 0.000 claims abstract description 10
- 230000005484 gravity Effects 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 238000000967 suction filtration Methods 0.000 claims abstract description 7
- 238000010298 pulverizing process Methods 0.000 claims abstract description 3
- 238000005086 pumping Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 27
- 238000004519 manufacturing process Methods 0.000 claims 1
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 abstract description 29
- 239000000447 pesticide residue Substances 0.000 abstract description 24
- 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 abstract description 9
- 229930003944 flavone Natural products 0.000 abstract description 9
- 150000002212 flavone derivatives Chemical class 0.000 abstract description 9
- 235000011949 flavones Nutrition 0.000 abstract description 9
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 abstract description 9
- 239000003292 glue Substances 0.000 abstract description 4
- 239000004480 active ingredient Substances 0.000 abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000012452 mother liquor Substances 0.000 description 9
- 239000000523 sample Substances 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000004744 fabric Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 6
- 239000012085 test solution Substances 0.000 description 6
- 238000007599 discharging Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000012488 sample solution Substances 0.000 description 5
- 239000010902 straw Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 238000010030 laminating Methods 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 description 4
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 description 4
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 description 4
- 235000005493 rutin Nutrition 0.000 description 4
- 229960004555 rutoside Drugs 0.000 description 4
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- 239000012490 blank solution Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000013558 reference substance Substances 0.000 description 3
- 235000010288 sodium nitrite Nutrition 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 238000007792 addition Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 229930003935 flavonoid Natural products 0.000 description 2
- 150000002215 flavonoids Chemical class 0.000 description 2
- 235000017173 flavonoids Nutrition 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 235000012424 soybean oil Nutrition 0.000 description 2
- 239000003549 soybean oil Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000257303 Hymenoptera Species 0.000 description 1
- 208000025157 Oral disease Diseases 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000469 ethanolic extract Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000012530 fluid Substances 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
- 230000036541 health Effects 0.000 description 1
- CKAPSXZOOQJIBF-UHFFFAOYSA-N hexachlorobenzene Chemical compound ClC1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1Cl CKAPSXZOOQJIBF-UHFFFAOYSA-N 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 208000030194 mouth disease Diseases 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
- A61P1/02—Stomatological preparations, e.g. drugs for caries, aphtae, periodontitis
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P17/00—Drugs for dermatological disorders
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P29/00—Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/10—Antimycotics
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P37/00—Drugs for immunological or allergic disorders
- A61P37/02—Immunomodulators
- A61P37/04—Immunostimulants
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Pharmacology & Pharmacy (AREA)
- Chemical & Material Sciences (AREA)
- Public Health (AREA)
- Medicinal Chemistry (AREA)
- Animal Behavior & Ethology (AREA)
- Veterinary Medicine (AREA)
- Organic Chemistry (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Engineering & Computer Science (AREA)
- Immunology (AREA)
- Insects & Arthropods (AREA)
- Communicable Diseases (AREA)
- Oncology (AREA)
- Animal Husbandry (AREA)
- Zoology (AREA)
- Epidemiology (AREA)
- Dermatology (AREA)
- Pain & Pain Management (AREA)
- Rheumatology (AREA)
- Jellies, Jams, And Syrups (AREA)
Abstract
The invention discloses a propolis extract and a preparation method thereof, wherein the preparation method comprises the following steps: (1) raw material treatment: freezing propolis, and pulverizing; (2) extraction: adding 95% ethanol into the raw materials, reflux extracting, and filtering; (3) and (3) suction filtration: pumping and filtering the feed liquid under negative pressure; (4) concentration: concentrating the feed liquid into a specific gravity of 1.0-1.2 under negative pressure to obtain a concentrated solution, and recovering ethanol; (5) and (3) extraction: adding petroleum ether into the concentrated solution for extraction, and fully and uniformly mixing, wherein the upper layer is a petroleum ether layer, and the lower layer is a mother solution layer; (6) liquid separation: concentrating the petroleum ether layer under negative pressure to recover petroleum ether; (7) and (3) drying: concentrating the mother solution layer under negative pressure, drying, and freezing to obtain propolis extract. The invention adopts petroleum ether for extraction, pesticide residues are not detected, the pesticide residues conform to the GB2763-2016 standard, the glue content is more than or equal to 95 percent, the total flavone content is more than or equal to 22 percent, and the yield of active ingredients is more than or equal to 85 percent.
Description
Technical Field
The invention relates to the technical field of natural product active ingredient extraction, and particularly relates to a propolis extract and a preparation method thereof.
Background
Propolis is a fragrant colloidal solid obtained by bees from plant spores, trunks, etc., and is converted into a yellow brown block by mixing with bee secretion. The product is hardened and embrittled at the temperature of lower than 15 ℃ and can be powdered; the temperature is higher than 36 ℃ and lower than 50 ℃, and the product has plasticity and viscosity; temperatures greater than 55 ℃ may become fluid.
Propolis is called purple gold, and is very limited, but effective components contained in propolis are particularly complex, and about 20 to 300 nutrient components are contained, and mainly comprise flavonoids, dilute terpenoids, esters, organic acids, aldehydes, phenols and the like. At present, the market mainly takes the gum content and the total flavone as measurement indexes, the traditional process is an immersion method at present, namely the process is immersed in ethanol for about 12 hours, and the process is time-consuming, long in period and low in content.
All the components in propolis have certain special functions. The propolis can promote cell regeneration, has good repairing function on various oral diseases, and has effects of enhancing immunity, caring skin, relieving pain, and resisting bacteria. Propolis has been widely used in various fields such as health products, cosmetics, medicines, etc. However, the propolis extract has the problem of pesticide residue, and is increasingly attracting wide attention. The traditional process at present has an active carbon removal method, but the effect is not ideal, and the effective components are only retained by about 60 percent.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the technical defects of the background technology and provides a propolis extract and a preparation method thereof. The invention adopts petroleum ether for extraction, pesticide residues are not detected, the pesticide residues conform to the GB2763-2016 standard, the glue content is more than or equal to 95 percent, the total flavone content is more than or equal to 22 percent, and the yield of active ingredients is more than or equal to 85 percent.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for preparing propolis extract comprises the following steps:
(1) raw material treatment: freezing propolis, and pulverizing;
(2) extraction: adding 95% ethanol into the raw materials, reflux extracting, and filtering;
(3) and (3) suction filtration: pumping and filtering the feed liquid under negative pressure;
(4) concentration: concentrating the feed liquid into a specific gravity of 1.0-1.2 under negative pressure to obtain a concentrated solution, and recovering ethanol;
(5) and (3) extraction: adding petroleum ether into the concentrated solution for extraction, and fully and uniformly mixing, wherein the upper layer is a petroleum ether layer, and the lower layer is a mother solution layer;
(6) liquid separation: concentrating the petroleum ether layer under negative pressure to recover petroleum ether;
(7) and (3) drying: concentrating the mother solution layer under negative pressure, drying, and freezing to obtain propolis extract.
Preferably, in the step (1), the freezing time is 24 h.
Preferably, in the step (2), the adding amount of the ethanol is 6-10 times of that of the raw materials according to the mass-to-volume ratio; the mass volume ratio of 1 means that 1000g of raw material and 1000ml of ethanol are added.
Preferably, in the step (2), the reflux extraction time is 2 h.
Preferably, in the step (2), the filtration is performed by using a filter cloth.
More preferably, in the step (2), the mesh number of the filter cloth is 100-300 meshes.
Preferably, in the step (2), after filtering with a filter cloth, the extraction operation is repeated for 1 time on the filter residue.
Preferably, in the step (3), the negative pressure is-0.08 MPa.
Preferably, in the step (3), the two feed liquids are combined.
Preferably, in the step (4), the negative pressure is-0.06 to-0.1 MPa.
Preferably, in the step (4), the temperature during concentration is 40-60 ℃.
Preferably, in the step (5), the addition amount of the petroleum ether is 1.5 to 2.5 times of the concentrated solution by volume ratio.
Preferably, in the step (6), the petroleum ether layer is laminated by repeating the operation of the step (5) after discharging the mother liquor layer.
More preferably, in the step (6), the number of times of the repeated operation is 1 to 2.
Preferably, in the step (6), the negative pressure concentration condition is 50 ℃ and-0.08 MPa.
Preferably, in the step (7), the negative pressure concentration condition is 60 ℃ and-0.08 MPa.
Preferably, in the step (7), the drying is air-blast drying.
More preferably, in the step (7), the drying temperature is 80-90 ℃, and the drying time is 5 hours.
Preferably, in the step (7), the temperature of the freezing is-18 ℃.
A propolis extract is prepared by the above preparation method.
In the technical scheme, the percentage is mass percentage.
Through a large number of experiments, the invention finds that the specific technical effect of the invention can be realized only by adopting the specific technical scheme of the invention, and other technical schemes can not realize the specific technical effect of the invention.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention adopts petroleum ether for extraction, pesticide residues are not detected (the pesticide residue content is lower than 0.01ppm and is considered as not detected), the pesticide residues conform to the GB2763-2016 standard, the glue content is more than or equal to 95 percent, the total flavone content is more than or equal to 22 percent, and the yield of effective components is more than or equal to 85 percent;
(2) the process of the invention adopts ethanol reflux extraction, and greatly shortens the extraction period compared with ethanol soaking extraction.
Detailed Description
For a better understanding of the present invention, reference is made to the following examples. It is to be understood that these examples are for further illustration of the invention and are not intended to limit the scope of the invention. In addition, it should be understood that the invention is not limited to the above-described embodiments, but is capable of various modifications and changes within the scope of the invention.
Example 1
A method for preparing propolis extract comprises the following steps:
(1) treating propolis raw materials: freezing 1000g of propolis raw material for 24h, and powdering;
(2) extraction: adding 6 times of 95% ethanol into the raw materials, extracting under reflux for 2h, filtering with 100 mesh filter cloth, and repeating the extraction on the filter residue for 1 time;
(3) and (3) suction filtration: suction-filtering the feed liquid under negative pressure of-0.08 MPa, and combining the feed liquid for two times;
(4) concentration: concentrating the feed liquid obtained in the step 3 to specific gravity of 1.0 at the negative pressure of-0.06 MPa and the temperature of 60 ℃, and simultaneously recovering ethanol;
(5) and (3) extraction: adding 1.5 times of petroleum ether into the concentrated solution obtained in the step 4 to extract pesticide residues, and fully and uniformly mixing, wherein the upper layer is a petroleum ether layer, and the lower layer is a mother solution layer;
(6) liquid separation: discharging the lower mother liquor layer and repeating the operation of the step 5 for 1 time; laminating the petroleum ether layers obtained in the step 5 together, and concentrating and recovering the petroleum ether layers at the temperature of 50 ℃ and under the negative pressure of-0.08 MPa;
(7) and (3) drying: concentrating the mother liquor at 60 deg.C under-0.08 MPa, air-blast drying at 80 deg.C for 5 hr, and freezing at-18 deg.C to obtain propolis extract.
Example 2
A method for preparing propolis extract comprises the following steps:
(1) treating propolis raw materials: freezing 1000g of propolis raw material for 24h, and powdering;
(2) extraction: adding 10 times of 95% ethanol into the raw materials, extracting under reflux for 2h, filtering with 300 mesh filter cloth, and repeating the extraction on the filter residue for 1 time;
(3) and (3) suction filtration: suction-filtering the feed liquid under negative pressure of-0.08 MPa, and combining the feed liquid for two times;
(4) concentration: concentrating the feed liquid obtained in the step 3 to specific gravity of 1.2 at 40 ℃ under negative pressure of-0.1 MPa, and recovering ethanol;
(5) and (3) extraction: adding 2.5 times of petroleum ether into the concentrated solution obtained in the step 4 to extract pesticide residues, and fully and uniformly mixing, wherein the upper layer is a petroleum ether layer, and the lower layer is a mother solution layer;
(6) liquid separation: discharging the lower mother liquor layer and repeating the operation of the step 5 for 1 time; laminating the petroleum ether layers obtained in the step 5 together, and concentrating and recovering the petroleum ether layers at the temperature of 50 ℃ and under the negative pressure of-0.08 MPa;
(7) and (3) drying: concentrating the mother liquor at 60 deg.C under-0.08 MPa, air-blast drying at 90 deg.C for 5 hr, and freezing at-18 deg.C to obtain propolis extract.
Example 3
A method for preparing propolis extract comprises the following steps:
(1) treating propolis raw materials: freezing 1000g of propolis raw material for 24h, and powdering;
(2) extraction: adding 8 times of 95% ethanol into the raw materials, extracting under reflux for 2h, filtering with 200 mesh filter cloth, and repeating the extraction on the filter residue for 1 time;
(3) and (3) suction filtration: suction-filtering the feed liquid under negative pressure of-0.08 MPa, and combining the feed liquid for two times;
(4) concentration: concentrating the feed liquid obtained in the step 3 to specific gravity of 1.1 at 50 ℃ under negative pressure of-0.08 MPa, and recovering ethanol;
(5) and (3) extraction: adding 2 times of petroleum ether into the concentrated solution obtained in the step 4 to extract pesticide residues, and fully and uniformly mixing, wherein the upper layer is a petroleum ether layer, and the lower layer is a mother solution layer;
(6) liquid separation: discharging the lower mother liquor layer and repeating the operation of the step 5 for 2 times; laminating the petroleum ether layers obtained in the step 5 together, and concentrating and recovering the petroleum ether layers at the temperature of 50 ℃ and under the negative pressure of-0.08 MPa;
(7) and (3) drying: concentrating the mother liquor at 60 deg.C under-0.08 MPa, air-blast drying at 90 deg.C for 5 hr, and freezing at-18 deg.C to obtain propolis extract.
Comparative example 1
A method for preparing propolis extract comprises the following steps:
(1) treating propolis raw materials: freezing 1000g of propolis raw material for 24h, and powdering;
(2) extraction: adding 6 times of 95% ethanol into the raw materials, extracting under reflux for 2h, filtering with 100 mesh filter cloth, and repeating the extraction on the filter residue for 1 time;
(3) and (3) suction filtration: suction-filtering the feed liquid under negative pressure of-0.08 MPa, and combining the feed liquid for two times;
(4) concentration: concentrating the feed liquid obtained in the step 3 to specific gravity of 1.0 at the negative pressure of-0.06 MPa and the temperature of 60 ℃, and simultaneously recovering ethanol;
(5) and (3) extraction: adding soybean oil in an amount which is 1.5 times that of the concentrated solution obtained in the step 4 to extract pesticide residues, and fully and uniformly mixing, wherein the upper layer is a petroleum ether layer, and the lower layer is a mother solution layer;
(6) liquid separation: discharging the lower mother liquor layer and repeating the operation of the step 5 for 1 time; laminating the petroleum ether layers obtained in the step 5 together, and concentrating and recovering the petroleum ether layers at the temperature of 50 ℃ and under the negative pressure of-0.08 MPa;
(7) and (3) drying: concentrating the mother liquor at 60 deg.C under-0.08 MPa, air-blast drying at 80 deg.C for 5 hr, and freezing at-18 deg.C to obtain propolis extract.
Effects of the embodiment
Method for measuring glue content
1 instrument and appliance: an analytical balance, a drying dish, an electric heating air blast drying box, a 100ml beaker, an ultrasonic instrument, a glass rod, a 250ml conical flask, weighing paper 70mm multiplied by 35mm and a glass funnel phi 60 mm.
2 reagent
Ethanol: analytically pure (more than or equal to 95%);
the filter paper phi 12.5cm was quantified.
3, an operation method: weighing about 5g of crushed propolis sample, weighing, placing in a 100ml beaker, precisely adding 100ml of 95% ethanol, sealing, performing ultrasonic treatment, pouring the supernatant into a filter paper and a glass funnel which are dried and weighed in advance, filtering into a conical flask, repeating the steps for several times until the supernatant is completely dissolved, and washing the beaker and the filter paper with a small amount of ethanol for several times. The residue and filter paper were then dried with a glass funnel at 50 ℃ to constant weight. Parallel experiments were performed under the same conditions.
4, calculating:
calculating according to the formula (1): x1＝(M1-M2)/M1×100％ (1)
Wherein X1-the content of ethanol extract in the sample,%;
M1-sample mass in grams (g);
M2-residue mass in grams (g);
the error of the parallel experiment is not more than 1.5%, and the average value of three determinations is taken.
Second, method for measuring total flavone content
1 preparation of control solutions
Taking 10.0mg of rutin reference substance, precisely weighing (one hundred thousand), placing in a 50ml volumetric flask, adding about 40ml of ethanol solution, performing ultrasonic treatment to dissolve, taking out, and cooling to room temperature; adding ethanol solution to desired volume, shaking, and making into control solution containing rutin 0.20mg per 1 ml.
Preparation of 2 Standard Curve
Taking a 10ml straw, precisely measuring 1ml, 2ml, 3ml, 4ml, 5ml and 6ml of reference substance solution, respectively placing the reference substance solution, adding deionized water to 6ml (5ml, 4ml, 3ml, 2ml, 1ml and 0ml), respectively adding 1ml of 5% sodium nitrite solution into the 1ml straw, uniformly mixing, placing for 6 minutes, adding 1ml of 10% aluminum nitrate solution into the 1ml straw, shaking up, placing for 6 minutes, taking the 10ml straw, adding 10ml of sodium hydroxide test solution into the 1ml straw, adding deionized water to scale, shaking up, and placing for 15 minutes; adding 6ml of deionized water into a 25ml volumetric flask, adding 1ml of 5% sodium nitrite solution, uniformly mixing, standing for 6 minutes, adding 1ml of 10% aluminum nitrate solution, shaking up, standing for 6 minutes, adding 10ml of sodium hydroxide test solution, adding deionized water to the scale, shaking up, standing for 15 minutes to obtain a blank solution. The absorbance was measured at a wavelength of 500nm, and a standard curve was drawn with the absorbance as the ordinate and the concentration as the abscissa.
3 preparation of test solutions
Taking 0.15g of the product, precisely weighing (one hundred thousand parts) and placing in a 25ml volumetric flask, adding diluted ethanol to a constant volume to scale, sealing, shaking up, carrying out ultrasonic treatment for 5 minutes, standing for more than 3 hours, filtering (medium-speed qualitative filter paper), taking a 2ml pipette, precisely measuring 2ml of subsequent filtrate, placing in a 25ml volumetric flask, diluting to scale with deionized water, and shaking up to obtain a sample solution.
4 assay method
Taking a 2ml pipette, precisely measuring 2ml of the sample solution, putting the sample solution into a 25ml volumetric flask, adding deionized water to the scale, and shaking up to obtain a blank solution; taking a 2ml pipette, precisely measuring 2ml of the sample solution, and placing the sample solution in a 25ml volumetric flask; taking a 5ml pipette, and precisely measuring 4ml of deionized water into a volumetric flask; taking a 1ml pipette, precisely measuring 1ml of 5% sodium nitrite solution into a volumetric flask, uniformly mixing, and standing for 6 minutes; taking a 1ml pipette, precisely measuring 1ml of 10% aluminum nitrate solution into a volumetric flask, shaking up, and standing for 6 minutes; taking a 10ml pipette, precisely measuring 10ml of sodium hydroxide test solution into a volumetric flask, adding deionized water to the scale, shaking up, and standing for 15 minutes; and (3) taking the blank solution as a blank, measuring the absorbance at the wavelength of 500nm, reading the amount of rutin in the test solution on a standard curve, and calculating to obtain the rutin contained in the test solution.
5 calculation of
CSample (A): obtaining the concentration (mg/mL) of the total flavonoids of the sample to be detected according to a standard curve;
Msample (A): the sample mass to be measured (mg);
Vsample (A): volume of sample to be tested (mL).
Third, calculation method of propolis recovery rate
N％＝M1/M2×100；
N%: is weight yield, i.e. yield;
m1: drying the product;
m2: the product before treatment.
The pesticide residue content of the raw material propolis in the embodiments 1 to 3 and the comparative example 1 is as follows: hexachlorobenzene: 8.2ppm, sixty-six: 5.6ppm, DDT: 4.3ppm, and the rest pesticide residues are not detected.
The propolis extracts prepared in the embodiments 1 to 3 and the comparative example 1 are detected by the method, wherein the propolis extract prepared in the embodiment 1 is detected by a third-party detection mechanism (continental analysis technology service (Suzhou) Co., Ltd.), pesticide residues are not detected, and the pesticide residues meet the GB2763-2016 standard; the content of gum is 95%, the content of total flavone is 22%, and the weight yield is 85%.
The propolis extract prepared in the embodiment 2 is detected by a third-party detection mechanism (continental analytical technology service (Suzhou) Co., Ltd.), pesticide residues are not detected, and the pesticide residues meet the GB2763-2016 standard; the content of gum is 96%, the content of total flavone is 24%, and the weight yield is 88%.
The propolis extract prepared in the embodiment 3 is detected by a third-party detection mechanism (continental analytical technology service (Suzhou) Co., Ltd.), pesticide residues are not detected, and the pesticide residues meet the GB2763-2016 standard; the gum content is 98%, the total flavone content is 25%, and the weight yield is 90%.
Comparative example 1 the propolis extract prepared by the technical scheme of extracting pesticide residues with soybean oil is detected by a third-party detection mechanism (continental analytical technical service (suzhou) limited), pesticide residues are not detected, and the pesticide residues meet the GB2763-2016 standard; the gum content is 90%, the total flavone content is 20%, and the weight yield is 60%.
The invention has the beneficial effects that:
(1) the prior art adopts an ethanol soaking method, so that the period is long, the efficiency is low, and the method adopts ethanol reflux extraction, so that the period is short, and the efficiency is high;
(2) the invention adopts the petroleum ether extraction pesticide residue removal method, the yield is more than or equal to 85 percent, and the productivity is greatly improved.
The above description is not intended to limit the present invention, and the present invention is not limited to the above examples. Those skilled in the art should also realize that changes, modifications, additions and substitutions can be made without departing from the true spirit and scope of the invention.
Claims (10)
1. The preparation method of the propolis extract is characterized by comprising the following steps:
(1) raw material treatment: freezing propolis, and pulverizing;
(2) extraction: adding 95% ethanol into the raw materials, reflux extracting, and filtering;
(3) and (3) suction filtration: pumping and filtering the feed liquid under negative pressure;
(4) concentration: concentrating the feed liquid into a specific gravity of 1.0-1.2 under negative pressure to obtain a concentrated solution, and recovering ethanol;
(5) and (3) extraction: adding petroleum ether into the concentrated solution for extraction, and fully and uniformly mixing, wherein the upper layer is a petroleum ether layer, and the lower layer is a mother solution layer;
(6) liquid separation: concentrating the petroleum ether layer under negative pressure to recover petroleum ether;
(7) and (3) drying: concentrating the mother solution layer under negative pressure, drying, and freezing to obtain propolis extract.
2. The method of claim 1, wherein in the step (2), the amount of the ethanol added is 6-10 times of the raw material by mass/volume ratio.
3. The method of claim 1, wherein the negative pressure in step (3) is-0.08 MPa.
4. The method of claim 1, wherein the negative pressure is-0.06 to-0.1 MPa and the temperature during concentration is 40 to 60 ℃ in the step (4).
5. The method of claim 1, wherein the petroleum ether is added in an amount of 1.5 to 2.5 times the volume of the concentrated solution in the step (5).
6. The method of claim 1, wherein the negative pressure concentration in step (6) is performed at 50 ℃ and-0.08 MPa.
7. The method of claim 1, wherein the negative pressure concentration in step (7) is performed at 60 ℃ and-0.08 MPa.
8. The method of claim 1, wherein the drying in step (7) is performed by air-blast drying at 80-90 ℃ for 5 h.
9. The method of claim 1, wherein the freezing temperature in the step (7) is-18 ℃.
10. A propolis extract characterized by being produced by the method for producing a propolis extract according to any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911306351.4A CN110898083A (en) | 2019-12-18 | 2019-12-18 | Propolis extract and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911306351.4A CN110898083A (en) | 2019-12-18 | 2019-12-18 | Propolis extract and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110898083A true CN110898083A (en) | 2020-03-24 |
Family
ID=69826194
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911306351.4A Pending CN110898083A (en) | 2019-12-18 | 2019-12-18 | Propolis extract and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110898083A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112451548A (en) * | 2020-12-08 | 2021-03-09 | 宁波杰顺生物科技有限公司 | Propolis extract and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103054907A (en) * | 2012-12-05 | 2013-04-24 | 天津隆顺榕发展制药有限公司 | Propolis flavonoid extractive and preparation method thereof |
| US10024827B1 (en) * | 2017-07-05 | 2018-07-17 | Institute of Food Science and Technology, Chinese Academy of Agricultural Sciences | Method for simultaneously detecting four isomers of resveratrol in peanut |
| CN108553527A (en) * | 2018-06-25 | 2018-09-21 | 昆明贝泰妮生物科技有限公司 | A kind of preparation method of blueness bur benevolence extractive of general flavone |
-
2019
- 2019-12-18 CN CN201911306351.4A patent/CN110898083A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103054907A (en) * | 2012-12-05 | 2013-04-24 | 天津隆顺榕发展制药有限公司 | Propolis flavonoid extractive and preparation method thereof |
| US10024827B1 (en) * | 2017-07-05 | 2018-07-17 | Institute of Food Science and Technology, Chinese Academy of Agricultural Sciences | Method for simultaneously detecting four isomers of resveratrol in peanut |
| CN108553527A (en) * | 2018-06-25 | 2018-09-21 | 昆明贝泰妮生物科技有限公司 | A kind of preparation method of blueness bur benevolence extractive of general flavone |
Non-Patent Citations (1)
| Title |
|---|
| 孙丽萍等: "蜂胶不同溶剂萃取物组成和抗氧化性的研究", 《食品科学》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112451548A (en) * | 2020-12-08 | 2021-03-09 | 宁波杰顺生物科技有限公司 | Propolis extract and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107936072A (en) | A kind of method using eutectic solvent extraction blackberry anthocyanin | |
| CN104688801B (en) | A kind of complex enzyme combination ultrasound extracts the production technology of eucommia bark flavone from folium cortex eucommiae | |
| CN107309438A (en) | A kind of method that polysaccharide from Phyllanthus Emblica L prepares Nano Silver compound particle | |
| CN103525542B (en) | Method for extracting shiny-leaved yellowhorn grease containing nervonic acid from shiny-leaved yellowhorn | |
| CN105237654A (en) | Method for extracting pectin from orange peel | |
| CN105535029B (en) | Countercurrent ultrasonic preparation method of propolis extract | |
| CN110898083A (en) | Propolis extract and preparation method thereof | |
| CN107759709A (en) | A kind of extracting method of Siberian solomonseal rhizome polysaccharide | |
| CN108315361B (en) | Method for synthesizing p-hydroxybenzaldehyde by using microorganisms | |
| CN106620067A (en) | Method for extracting pineapple peel flavonoid compound | |
| CN102808046B (en) | Method for extracting fructose from apple pomace | |
| CN103289969A (en) | Method for extracting superoxide dismutase from plant stem leaves | |
| CN107459547B (en) | Method for coproducing and separating various bioactive substances in egg yolk | |
| CN107474152B (en) | A kind of preparation method and Inonotus obliquus extracting solution of Inonotus obliquus crude extract | |
| CN116020163A (en) | Green method for efficiently removing mucilaginous substances on surface of high-gel-content plant material by using superheated water | |
| CN115626958A (en) | Method for separating edible fungus polysaccharide based on silicon carbide ceramic membrane technology and application | |
| CN105001284B (en) | A kind of purple spring wheat wheat bran anthocyanin extracting method | |
| CN106518653A (en) | Membrane extraction process for hydroxycitric acid | |
| CN102229755A (en) | Method for producing purple sweet potato haematochrome | |
| CN103451254A (en) | Method for preparing gingko microporous starch with high specific surface area by bio-enzyme method | |
| CN102993768B (en) | Blackcurrant pigment extract and production method thereof | |
| CN102776298B (en) | Extractive of apple pomace fructose | |
| CN109721666A (en) | A kind of ultrasonic auxiliary extraction method of Sphallerocerpus gracilis polysaccharide | |
| CN115716854B (en) | Method for extracting polyphenol from lettuce | |
| CN101785559A (en) | Processing method utilizing gingko to prepare gingko detoxifying powder and co-generate crude ginkgo phenolic acid extract |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200324 |
|
| RJ01 | Rejection of invention patent application after publication |