CN112225764A - Method for extracting geniposide - Google Patents
Method for extracting geniposide Download PDFInfo
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- CN112225764A CN112225764A CN202011030734.6A CN202011030734A CN112225764A CN 112225764 A CN112225764 A CN 112225764A CN 202011030734 A CN202011030734 A CN 202011030734A CN 112225764 A CN112225764 A CN 112225764A
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- geniposide
- gardenia fruits
- extracting
- gardenia
- fruits
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- IBFYXTRXDNAPMM-BVTMAQQCSA-N Geniposide Chemical compound O([C@@H]1OC=C([C@@H]2[C@H]1C(=CC2)CO)C(=O)OC)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O IBFYXTRXDNAPMM-BVTMAQQCSA-N 0.000 title claims abstract description 29
- IBFYXTRXDNAPMM-FZEIBHLUSA-N Geniposide Natural products COC(=O)C1=CO[C@@H](O[C@H]2O[C@@H](CO)[C@H](O)[C@@H](O)[C@@H]2O)[C@H]2[C@@H]1CC=C2CO IBFYXTRXDNAPMM-FZEIBHLUSA-N 0.000 title claims abstract description 28
- VGLLGNISLBPZNL-RBUKDIBWSA-N arborescoside Natural products O=C(OC)C=1[C@@H]2C([C@H](O[C@H]3[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O3)OC=1)=C(CO)CC2 VGLLGNISLBPZNL-RBUKDIBWSA-N 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims description 12
- 241000157835 Gardenia Species 0.000 claims abstract description 36
- 235000013399 edible fruits Nutrition 0.000 claims abstract description 32
- 238000001035 drying Methods 0.000 claims abstract description 28
- 230000001007 puffing effect Effects 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000012545 processing Methods 0.000 claims abstract description 6
- 230000008961 swelling Effects 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 14
- 238000000605 extraction Methods 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 6
- 239000004480 active ingredient Substances 0.000 abstract description 4
- XJMPAUZQVRGFRE-SCHFUKFYSA-N Gardenoside Natural products O=C(OC)C=1[C@H]2[C@H]([C@H](O[C@H]3[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O3)OC=1)[C@@](O)(CO)C=C2 XJMPAUZQVRGFRE-SCHFUKFYSA-N 0.000 abstract description 2
- 230000000975 bioactive effect Effects 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- XJMPAUZQVRGFRE-AYDWLWLASA-N methyl (1s,4as,7s,7as)-7-hydroxy-7-(hydroxymethyl)-1-[(2s,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxy-4a,7a-dihydro-1h-cyclopenta[c]pyran-4-carboxylate Chemical compound O([C@@H]1OC=C([C@@H]2[C@H]1[C@](C=C2)(O)CO)C(=O)OC)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O XJMPAUZQVRGFRE-AYDWLWLASA-N 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- 239000000243 solution Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 235000013305 food Nutrition 0.000 description 4
- SEBIKDIMAPSUBY-ARYZWOCPSA-N Crocin Chemical compound C([C@H]1O[C@H]([C@@H]([C@@H](O)[C@@H]1O)O)OC(=O)C(C)=CC=CC(C)=C\C=C\C=C(/C)\C=C\C=C(C)C(=O)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)O1)O)O[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O SEBIKDIMAPSUBY-ARYZWOCPSA-N 0.000 description 3
- 235000018958 Gardenia augusta Nutrition 0.000 description 3
- 240000001972 Gardenia jasminoides Species 0.000 description 3
- 239000007853 buffer solution Substances 0.000 description 3
- 239000009627 gardenia yellow Substances 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 230000001766 physiological effect Effects 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 241001107098 Rubiaceae Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 150000008145 iridoid glycosides Chemical class 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
Abstract
The invention relates to a gardenoside extraction method, which comprises the following steps: (1) processing fresh gardenia fruits by adopting low-temperature heat pump drying equipment to obtain dried gardenia fruits; (2) carrying out differential pressure puffing treatment on the dried gardenia fruits; (3) crushing to obtain fructus Gardeniae powder; (4) mixing the fructus Gardeniae powder with solvent, and extracting to obtain geniposide. The invention adopts low temperature heat pump drying technology to dry the material at lower temperature, can preserve the content of the effective bioactive substance geniposide in the material to the maximum extent, and then adopts differential pressure puffing to further quickly vaporize the free water in the gardenia fruits, thereby improving the extraction rate of the effective active ingredient geniposide in the subsequent gardenia fruits.
Description
Technical Field
The invention relates to a method for extracting geniposide.
Background
Gardenia jasminoides is a plant of Gardenia genus in Rubiaceae family, is mainly produced in southern and mid-southern areas of China, the area of the whole country is more than 60 ten thousand mu, wherein the planting area of the Gardenia jasminoides is 9.1 ten thousand mu in Zhejiang province, the planting area of the whole city in Wenzhou is only 6 ten thousand mu nearby, and the first planting area of all Chinese medicinal plants in Wenzhou becomes one of main sources of income of local farmers, thereby playing an important role in assisting the pleasure of villages. Gardenia jasminoides is used as a traditional Chinese medicinal material in China, has a long use history and rich physiological activity, and is a first dual-purpose resource for food and medicine issued by the Ministry of health. Researches show that the main physiological active ingredients of gardenia comprise geniposide, gardenia yellow pigment and the like, and the gardenia yellow pigment is widely applied to other fields such as medicines, foods and the like and is an active ingredient with great market potential.
Iridoid glycoside compounds represented by jasminoidin have physiological effects of protecting liver, relieving pain, resisting inflammation, resisting bacteria, resisting tumor, resisting oxidation, clearing away heat and toxic materials, reducing blood sugar and blood lipid, and preventing cardiovascular diseases. At present, the gardenoside for extracting the weight of the gardenia fruits is usually prepared by crushing fresh gardenia fruits, extracting by hot water, buffer solutions with different pH values or hydrophilic solvents such as methanol, ethanol, acetone and the like, and purifying by common purification methods such as extraction, column separation, crystallization and the like. Because the gardenia fruits are rich in oil, the prior method adopts hot water, buffer solutions with different pH values or hydrophilic solvents such as methanol, ethanol, acetone and the like to directly extract, partial geniposide is wrapped in gardenia fruit residues rich in oil and cannot be well extracted, and the output of the geniposide is influenced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for extracting geniposide.
The technical scheme adopted by the invention is as follows: a method for extracting geniposide comprises the following steps:
(1) processing fresh gardenia fruits by adopting low-temperature heat pump drying equipment to obtain dried gardenia fruits;
(2) carrying out differential pressure puffing treatment on the dried gardenia fruits;
(3) crushing to obtain fructus Gardeniae powder;
(4) mixing the fructus Gardeniae powder with solvent, and extracting to obtain geniposide.
Preferably, in the step (1), the circulating air speed is 2.0 m/s, the humidity is 30-40%, and the drying temperature is 41-47 ℃.
In the step (2), the swelling temperature is set to be 80-110 ℃, the swelling pressure is set to be 0.5-0.8MPa, the heating is carried out for 10-30min, and then the pressure is released, the vacuum degree is kept to be-0.098-0.090 MPa, and the vacuum degree is maintained for 5-10 min.
In the step (2), the puffing temperature is set to be 90-100 ℃.
Wherein, in the step (4), the solvent is hot water, buffer solutions with different pH values or hydrophilic solvents such as methanol, ethanol and acetone or one or more mixed solvents of water and hydrophilic solvents such as methanol, ethanol and acetone.
The invention has the following beneficial effects: the invention adopts low temperature heat pump drying technology to dry the material at lower temperature, can preserve the content of the effective bioactive substance geniposide in the material to the maximum extent, and then adopts differential pressure puffing to further quickly vaporize the free water in the gardenia fruits, thereby improving the extraction rate of the effective active ingredient geniposide in the subsequent gardenia fruits.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is within the scope of the present invention for those skilled in the art to obtain other drawings based on the drawings without inventive exercise.
FIG. 1 is a schematic flow chart of example 1;
FIG. 2 is a graph showing the dynamic curve of the effect of different low temperature heat pump drying temperatures on the water content of gardenia fruits.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings.
Example 1:
a method for extracting geniposide comprises the following steps:
(1) processing fresh gardenia fruits by adopting low-temperature heat pump drying equipment, selecting a circulating air speed of 2.0 m/s and a humidity of 30-40%, carrying out heat pump drying at the drying temperature of 25 ℃, 30 ℃, 35 ℃, 38 ℃, 41 ℃, 44 ℃ and 47 ℃ respectively, preheating for 30min by using a machine before drying, paving the gardenia fruits on a screen mesh after reaching a stable temperature, wherein the thickness of the gardenia fruits is 2cm, and monitoring a dynamic change curve of the water content of the gardenia fruits during the whole drying process; and stopping drying until the water content of the gardenia fruits is stable and unchanged, and drawing a low-temperature heat pump drying kinetic curve of the gardenia fruits. The data drying dynamics curves are drawn in parallel for 3 times, and the average value is taken;
wherein the Gardenia fruit treated at 25 deg.C and 30 deg.C has odor such as acid odor during drying, and can not be used. Wherein, the drying dynamics curve of the gardenia fruits processed under the conditions of 35 ℃, 38 ℃, 41 ℃, 44 ℃ and 47 ℃ is shown in figure 2, the total drying time is rapidly reduced along with the rising of the low-temperature heat pump drying temperature, and the water content of the gardenia fruits is stable for about 152.8 hours when the drying temperature is 35 ℃; when the drying temperature is raised to 38 ℃, the water content of the gardenia fruits is stable and only 83.3 hours are needed; the drying temperature rise can obviously reduce the drying rate of the gardenia fruits; and when the drying temperature is continuously increased to 41 ℃, 44 ℃ and 47 ℃, the drying kinetic curve fitting performance of the gardenia fruit moisture is very good, the time for reaching the stability is 66.7-55.6 hours, the moisture difference is small after the drying treatment at 41 ℃, 44 ℃ and 47 ℃, the subsequent steps are carried out on the mixing, the mixed gardenia fruit is defined as a sample 1, and the moisture content is about 13%.
(2) Heating fructus Gardeniae dried by low temperature heat pump at 80-110 deg.C for 10-30min to expand pressure of 0.5-0.8MPa, and maintaining vacuum degree of-0.098-0.090 MPa for 5-10 min;
the swelling temperature of 80 ℃ treatment is defined as sample 2, and the water content is reduced to 7.9%; the puffing temperature is 90 ℃ and the processing is defined as sample 3, and the water content is reduced to 4.1%; the puffing temperature is 100 ℃, the processing is defined as sample 4, and the water content is reduced to 4.0 percent; the puffing temperature of 110 ℃ treatment is defined as sample 5, and the moisture content is reduced to 3.4%.
(3) Crushing the samples 1-5 by a universal crusher and sieving the crushed samples with a 40-mesh sieve to obtain gardenia powder;
(4) mixing the gardenia powder with a solvent to extract the geniposide, which comprises the following steps: dispersing fructus Gardeniae powder (40 mesh) in 50% ethanol solution at a ratio of 1:20, and mixing with ethanol solution at a ratio of 20%oC, carrying out constant temperature ultrasonic treatment (power of 100W and frequency of 40 KHz) for 30min, centrifuging, taking 0.5mL of filtrate, diluting to fix the volume to 50mL, measuring the light absorption value at 238nm, calculating the content of the geniposide according to a standard curve of a geniposide standard product, calculating the result by using the average value of the results of 3 independent parallel experiments, and keeping 2 significant digits.
Among them, the extraction rate of test 1 was 22%, the extraction rate of test 2 was 24%, the extraction rate of test 3 was 38%, the extraction rate of test 4 was 58%, and the extraction rate of test 5 was 21%. Therefore, the differential pressure puffing temperature has obvious influence on the extraction rate of the geniposide, and compared with a control group without differential pressure puffing, the puffing temperature is 90 DEG oCAnd 100oC can obviously improve the extraction yield of the geniposide.
The adopted fresh gardenia fruits are provided by Zhejiang starlight agriculture development Co., Ltd, and the content of the geniposide and the content of the gardenia yellow in the raw materials are respectively detected to be 7.68 percent and 10.45 percent.
The adopted instruments specifically comprise: 5HP low-temperature heat pump drying equipment (Hangzhou European Electrical appliances); differential pressure puffing equipment; model WL-6F crown sub-moisture meter (Shenzhen crown sub-moisture meter science and technology Co., Ltd.); an ultrasonic cleaner; a universal pulverizer; an electronic analytical balance; spectrophotometers, and the like.
The moisture content is measured by using a Guanya moisture tester (WL-6F) to refer to the moisture in GB 5009.3-2016 food safety national standard food.
Comparative example 1:
pulverizing fresh fructus Gardeniae, mixing with 50% ethanol solution at a ratio of 1:20, and mixing at a ratio of 20%oC constant temperature ultrasonic treatment (power 100W, frequency 40 KHz) for 30min, centrifuging, taking 0.5mL of filtrate, diluting to constant volume to 50mL, measuring light absorption value at 238nm, calculating geniposide content according to standard curve of geniposide standard, calculating result by average value of 3 independent parallel experiment results, and keeping 2-digit effective numberA word. The extraction rate was measured to be 20%.
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention, and it is therefore to be understood that the invention is not limited by the scope of the appended claims.
Claims (4)
1. A method for extracting geniposide is characterized by comprising the following steps:
(1) processing fresh gardenia fruits by adopting low-temperature heat pump drying equipment to obtain dried gardenia fruits;
(2) carrying out differential pressure puffing treatment on the dried gardenia fruits;
(3) crushing to obtain fructus Gardeniae powder;
(4) mixing the fructus Gardeniae powder with solvent, and extracting to obtain geniposide.
2. The method for extracting geniposide according to claim 1, wherein: in the step (1), the circulating wind speed is 2.0 m/s, the humidity is 30-40%, and the drying temperature is 41-47 ℃.
3. The method for extracting geniposide according to claim 1, wherein: in the step (2), the swelling temperature is set to be 80-110 ℃, the swelling pressure is set to be 0.5-0.8MPa, the heating is carried out for 10-30min, and then the pressure is released, the vacuum degree is kept to be-0.098-0.090 MPa, and the vacuum degree is maintained for 5-10 min.
4. The method for extracting geniposide according to claim 3, wherein: in the step (2), the puffing temperature is set to be 90-100 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011030734.6A CN112225764A (en) | 2020-09-27 | 2020-09-27 | Method for extracting geniposide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011030734.6A CN112225764A (en) | 2020-09-27 | 2020-09-27 | Method for extracting geniposide |
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| CN112225764A true CN112225764A (en) | 2021-01-15 |
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| CN202011030734.6A Pending CN112225764A (en) | 2020-09-27 | 2020-09-27 | Method for extracting geniposide |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1939457A (en) * | 2006-09-30 | 2007-04-04 | 福州大学 | Preparation of gardenia jasminoides extracts |
| CN103444943A (en) * | 2012-09-17 | 2013-12-18 | 陈小强 | Method for comprehensively extracting theabrownin and tea polysaccharide by taking dark tea as active ingredients |
| CN111592929A (en) * | 2020-06-02 | 2020-08-28 | 温州科技职业学院 | Method for preparing gardenia seed oil by using variable-temperature differential pressure puffing technology |
-
2020
- 2020-09-27 CN CN202011030734.6A patent/CN112225764A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1939457A (en) * | 2006-09-30 | 2007-04-04 | 福州大学 | Preparation of gardenia jasminoides extracts |
| CN103444943A (en) * | 2012-09-17 | 2013-12-18 | 陈小强 | Method for comprehensively extracting theabrownin and tea polysaccharide by taking dark tea as active ingredients |
| CN111592929A (en) * | 2020-06-02 | 2020-08-28 | 温州科技职业学院 | Method for preparing gardenia seed oil by using variable-temperature differential pressure puffing technology |
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