CN109111364A - A kind of method of high-pressure pulse electric combination microwave, ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid - Google Patents
A kind of method of high-pressure pulse electric combination microwave, ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid Download PDFInfo
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- CN109111364A CN109111364A CN201710478852.5A CN201710478852A CN109111364A CN 109111364 A CN109111364 A CN 109111364A CN 201710478852 A CN201710478852 A CN 201710478852A CN 109111364 A CN109111364 A CN 109111364A
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- chlorogenic acid
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- pressure pulse
- pulse electric
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- 241000208125 Nicotiana Species 0.000 title claims abstract description 63
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 63
- CWVRJTMFETXNAD-FWCWNIRPSA-N 3-O-Caffeoylquinic acid Natural products O[C@H]1[C@@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-FWCWNIRPSA-N 0.000 title claims abstract description 61
- PZIRUHCJZBGLDY-UHFFFAOYSA-N Caffeoylquinic acid Natural products CC(CCC(=O)C(C)C1C(=O)CC2C3CC(O)C4CC(O)CCC4(C)C3CCC12C)C(=O)O PZIRUHCJZBGLDY-UHFFFAOYSA-N 0.000 title claims abstract description 61
- CWVRJTMFETXNAD-KLZCAUPSSA-N Neochlorogenin-saeure Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O CWVRJTMFETXNAD-KLZCAUPSSA-N 0.000 title claims abstract description 61
- CWVRJTMFETXNAD-JUHZACGLSA-N chlorogenic acid Chemical compound O[C@@H]1[C@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-JUHZACGLSA-N 0.000 title claims abstract description 61
- 229940074393 chlorogenic acid Drugs 0.000 title claims abstract description 61
- FFQSDFBBSXGVKF-KHSQJDLVSA-N chlorogenic acid Natural products O[C@@H]1C[C@](O)(C[C@@H](CC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O FFQSDFBBSXGVKF-KHSQJDLVSA-N 0.000 title claims abstract description 61
- 235000001368 chlorogenic acid Nutrition 0.000 title claims abstract description 61
- BMRSEYFENKXDIS-KLZCAUPSSA-N cis-3-O-p-coumaroylquinic acid Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)cc2)[C@@H]1O)C(=O)O BMRSEYFENKXDIS-KLZCAUPSSA-N 0.000 title claims abstract description 61
- 239000002699 waste material Substances 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000000605 extraction Methods 0.000 title claims abstract description 33
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000000706 filtrate Substances 0.000 claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000002390 rotary evaporation Methods 0.000 claims abstract description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003480 eluent Substances 0.000 claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 18
- 239000006228 supernatant Substances 0.000 claims abstract description 18
- 239000000284 extract Substances 0.000 claims abstract description 15
- 229920005989 resin Polymers 0.000 claims abstract description 15
- 239000011347 resin Substances 0.000 claims abstract description 15
- 239000012043 crude product Substances 0.000 claims abstract description 12
- 235000019441 ethanol Nutrition 0.000 claims abstract description 12
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000013049 sediment Substances 0.000 claims abstract description 9
- 239000003223 protective agent Substances 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 238000004064 recycling Methods 0.000 claims abstract description 6
- 239000002250 absorbent Substances 0.000 claims abstract description 5
- 230000002745 absorbent Effects 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 229920001429 chelating resin Polymers 0.000 claims description 8
- 239000002736 nonionic surfactant Substances 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 6
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 6
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 claims description 5
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 3
- 235000019387 fatty acid methyl ester Nutrition 0.000 claims description 3
- 235000010378 sodium ascorbate Nutrition 0.000 claims description 3
- 229960005055 sodium ascorbate Drugs 0.000 claims description 3
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims description 3
- 229940079827 sodium hydrogen sulfite Drugs 0.000 claims description 3
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 3
- 235000010262 sodium metabisulphite Nutrition 0.000 claims description 3
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 2
- 235000010352 sodium erythorbate Nutrition 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 8
- 238000007873 sieving Methods 0.000 abstract 1
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 6
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- 238000011084 recovery Methods 0.000 description 6
- 235000019504 cigarettes Nutrition 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
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- 238000003756 stirring Methods 0.000 description 3
- 241000725303 Human immunodeficiency virus Species 0.000 description 2
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- 150000008442 polyphenolic compounds Chemical class 0.000 description 2
- 235000013824 polyphenols Nutrition 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 241000205585 Aquilegia canadensis Species 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 206010009944 Colon cancer Diseases 0.000 description 1
- 208000001333 Colorectal Neoplasms Diseases 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
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- 210000003169 central nervous system Anatomy 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000008845 cholagoga Substances 0.000 description 1
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- 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
- 230000002443 hepatoprotective effect Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 201000007270 liver cancer Diseases 0.000 description 1
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- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 1
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- 230000000144 pharmacologic effect Effects 0.000 description 1
- 229930015704 phenylpropanoid Natural products 0.000 description 1
- 125000001474 phenylpropanoid group Chemical group 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a kind of methods of high-pressure pulse electric combination microwave, ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid.(1) tobacco waste is dried, is crushed, sieving；(2) smashed tobacco waste is placed in solvent, is stood, microwave treatment; then high-pressure pulse electric is handled, and then adjusts PH, ultrasonic wave extraction with hydrochloric acid solution; it filters, collects filtrate, filter residue repeats above-mentioned steps and extracts once; it filters, merges filtrate twice, discard filter residue; protective agent is added to filtrate, is refrigerated in refrigerator, removes bottom sediment; rotary evaporation recycling acetone is simultaneously concentrated, and centrifuge separation takes supernatant；(3) supernatant will be added after macroporous absorbent resin wet method dress post to adsorb, is eluted after absorption with ethanol water, collects eluent；(4) eluent rotary evaporation obtained above is recycled into ethyl alcohol and be concentrated, be then placed in refrigerator and freeze, placed into freeze drier and dry to get chlorogenic acid crude product.The method of the present invention chlorogenic acid yield is high.
Description
Technical field
The present invention relates to a kind of extracting methods of chlorogenic acid, and in particular to a kind of high-pressure pulse electric combination microwave, ultrasound
The method of wave extraction tobacco waste Content of Chlorogenic Acid.
Background technique
Chlorogenic acid (Chlorogenis Acid) is also known as coffee tannin, is one kind that plant synthesizes during aerobic respiration
Phenylpropanoids.Modern pharmacological studies have shown that chlorogenic acid is a kind of important physiological activator, have " plant gold " it
Good reputation.It not only has antibacterial, antiviral, Hepatoprotective cholagogue, lowering blood pressure and blood fat, removes free radical and stimulating central nervous system system
The multiple functions such as system, and have significant inhibiting effect to colorectal cancer, liver cancer and laryngocarcinoma, it is considered to be the effective protection of cancer
Agent.Research thinks that chlorogenic acid will promise to be the lead drug of anti AIDS virus (HIV).Modern science is to chlorogenic acid biology
Active research is deep to fields such as food, medicine, health care and daily-use chemical industries.
China is tobacco big country, and cultivated area and yield occupy first place in the world, ten thousand tons of annual yield of tobacco 450-550.Cigarette
Grass planting is processed in national economy with product and is played an important role.The tobacco planted both at home and abroad at present is mainly used as rolling up
Cigarette.Due to geographical environment, planting technology etc., there is the tobacco leaf of a certain number of inferior grades to cannot be used for cigarette every year raw
It produces, while also unavoidably generating some leftover bits and pieces during production of cigarettes, tobacco industry has a large amount of offal, mildew every year
Tobacco, low-class tobacco etc. are thrown away as waste, not only waste of resource but also have polluted environment.The effective component of tobacco waste is extracted
One of its comprehensive Utilization Ways contain a large amount of polyphenols in tobacco waste, and it is chlorogenic acid that wherein content is highest, therefore
It is necessary to be leached out.
The polyphenols such as chlorogenic acid are generally existing in plant, and traditional handicraft is mentioned from honeysuckle, folium cortex eucommiae mostly
It takes, extracts from tobacco waste and also seldom report, extracted from tobacco waste using high-pressure pulse electric combination microwave, ultrasonic wave
Chlorogenic acid is even more to have not been reported.Therefore, the invention discloses a kind of high-pressure pulse electric combination microwave, ultrasonic wave extraction tobacco are useless
Expect the method for Content of Chlorogenic Acid, opens up a new way for the comprehensive utilization of tobacco waste.
Summary of the invention
It is an object of the invention to a kind of high-pressure pulse electric combination microwaves, ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid
Method, the method for the present invention is easy to operate, and recovery rate is high, and extraction time is short, and is extracted active material and is not destroyed.
In order to solve the above technical problem, the present invention provides following technical solutions:
A kind of method of high-pressure pulse electric combination microwave, ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid, including walk as follows
It is rapid:
(1) tobacco waste is dried at 50-60 DEG C, is crushed, cross 20-40 mesh；
(2) smashed tobacco waste is placed in the solvent for being equivalent to 10-15 times of tobacco waste weight, stands 1-2h,
Microwave treatment 2-3 times, each 20-30s, then it is 0.1mol/L's with molar concentration that then high-pressure pulse electric, which handles 1-3ms,
It is 5-6, ultrasonic wave extraction 20-30min that hydrochloric acid solution, which adjusts PH, is filtered, and filtrate is collected, and filter residue repeats above-mentioned steps and extracts one
It is secondary, it filters, merges filtrate twice, discard filter residue, the protective agent for being equivalent to tobacco waste quality 0.2-0.3% is added to filtrate,
It is placed in 2-5 DEG C of refrigerator and refrigerates 24-48h, remove bottom sediment, rotary evaporation recycling acetone and the 1/3- for being concentrated into original volume
1/2, centrifuge separation takes supernatant；
(3) supernatant will be added after macroporous absorbent resin wet method dress post to adsorb, the ratio between column diameter and resin height are 1: 6-
8, it is eluted after absorption with the ethanol water that volume fraction is 40-60%, adjusting flow velocity is 3-6BV/h, and collection is washed
De- liquid；
(4) eluent rotary evaporation obtained above is recycled into ethyl alcohol and is concentrated into the 3/5-4/5 of original volume, then put
Enter in -50~-65 DEG C of refrigerators and freeze 30-50min, places into freeze drier and dry 24-48h to get chlorogenic acid crude product.
Further, the solvent is the solution that acetone and water form, and wherein the volume ratio of acetone and water is 1:1-2.
Further, nonionic surfactant is also added in the solvent, the nonionic surfactant adds
Dosage be solvent quality 1-3%, the nonionic surfactant be collateralization 13 carbon Guerbet alcohol polyoxyethylene ether,
One of 12-14 carbon primary alconol polyoxyethylene ether, fatty acid methyl ester APEO.
Further, the field strength of the high-pressure pulse electric is 25-40kV/cm, pulse frequency 400-600pps.
Further, the power of the microwave is 200-300W, frequency 10-20GHz.
Further, the power of the ultrasonic wave is 300-400W, frequency 30-40KHz.
Further, the protective agent is sodium hydrogensulfite, in sodium pyrosulfite, sodium ascorbate, sodium isoascorbate
One kind.
Further, the temperature of the rotary evaporation is 40-50 DEG C.
Further, the macroporous absorbent resin is U.S.'s Amberlite XAD-16 macroreticular resin.
The beneficial effects obtained by the present invention are as follows being:
(1) present invention efficiently can quickly smash tobacco in leaching process mesohigh impulse electric field combination microwave, ultrasonic wave
The cell wall of waste material, maximization penetrate into intracellular effective component release in solution, significantly improve the recovery rate of chlorogenic acid；
(2) it joined protective agent in extraction process of the present invention to prevent chlorogenic acid from aoxidizing, the present invention adds in Extraction solvent
Nonionic surfactant is entered, solvent can be improved to the affinity of chlorogenic acid, protective agent and non-ionic surface active is added
Agent improves the recovery rate of chlorogenic acid；
(3) the method for the present invention is easy to operate, and recovery rate is high, and extraction time is short, and is extracted active material and is not destroyed.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention.
Embodiment 1
A kind of method of high-pressure pulse electric combination microwave, ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid, including walk as follows
It is rapid:
(1) 100g tobacco waste is dried at 50 DEG C, is crushed, cross 20 meshes；
(2) smashed tobacco waste is placed in 560mL acetone and 560mL water mixes in the solvent of composition, and 12g is added
13 carbon Guerbet alcohol polyoxyethylene ether are branched, stand 1h after stirring, are 200W, frequency 10GHz in power
Microwave under handle 2 times, each 30s, be then 25kV/cm in field strength, pulse frequency be the high-voltage pulse electric of 400pps off field
1ms is handled, it is 5 that the hydrochloric acid solution for being then 0.1mol/L with molar concentration, which adjusts PH, is 300W, frequency 30KHz in power
Ultrasonic wave under extract 30min, filter, collect filtrate, filter residue repeats above-mentioned steps and extracts primary, filters, merging is filtered twice
Liquid discards filter residue, and 0.2g sodium hydrogensulfite is added to filtrate, is placed in 2 DEG C of refrigerators and refrigerates for 24 hours, bottom sediment is removed, at 40 DEG C
Lower rotary evaporation recycles acetone and is concentrated into the 1/3 of original volume, and centrifuge separation takes supernatant；
(3) supernatant will be added after U.S.'s Amberlite XAD-16 macroreticular resin wet method dress post to adsorb, column diameter and tree
The ratio between rouge height is 1: 6, is eluted after absorption with the ethanol water that volume fraction is 40%, and adjusting flow velocity is 3BV/h,
Collect eluent；
(4) by eluent obtained above, rotary evaporation recycles ethyl alcohol and is concentrated into the 3/5 of original volume at 40 DEG C, so
After be put into -50 DEG C of refrigerators and freeze 50min, place into freeze drier and dry for 24 hours to get chlorogenic acid crude product 4.35g.
Embodiment 2
A kind of method of high-pressure pulse electric combination microwave, ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid, including walk as follows
It is rapid:
(1) 100g tobacco waste is dried at 55 DEG C, is crushed, cross 30 meshes；
(2) smashed tobacco waste is placed in 524mL acetone and 786mL water mixes in the solvent of composition, and be added
24g12-14 carbon primary alconol polyoxyethylene ether, stands 1.5h after stirring, and is 250W in power, frequency is the micro- of 15GHz
It is handled under wave 3 times, each 25s, is then 32kV/cm in field strength, pulse frequency is that the high-voltage pulse electric of 500pps is handled off field
It is 5.5 that then hydrochloric acid solution that 2ms is 0.1mol/L with molar concentration, which adjusts PH, is 350W in power, frequency is 35KHz's
25min is extracted under ultrasonic wave, is filtered, and filtrate is collected, filter residue repeats above-mentioned steps and extracts once, filters, merge filtrate twice,
Filter residue is discarded, 0.25g sodium pyrosulfite is added to filtrate, is placed in 3 DEG C of refrigerators and refrigerates 36h, bottom sediment is removed, at 45 DEG C
Rotary evaporation recycling acetone is simultaneously concentrated into the 1/3 of original volume, and centrifuge separation takes supernatant；
(3) supernatant will be added after U.S.'s Amberlite XAD-16 macroreticular resin wet method dress post to adsorb, column diameter and tree
The ratio between rouge height is 1: 7, is eluted after absorption with the ethanol water that volume fraction is 50%, and adjusting flow velocity is 4BV/h,
Collect eluent；
(4) by eluent obtained above, rotary evaporation recycles ethyl alcohol and is concentrated into the 3/5 of original volume at 45 DEG C, so
After be put into -60 DEG C of refrigerators and freeze 40min, place into freeze drier dry 36h to get chlorogenic acid crude product 4.51g.
Embodiment 3
A kind of method of high-pressure pulse electric combination microwave, ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid, including walk as follows
It is rapid:
(1) tobacco waste is dried at 60 DEG C, is crushed, cross 40 meshes；
(2) smashed tobacco waste is placed in 538mL acetone and 1076mL water mixes in the solvent of composition, and added
Enter 42g fatty acid methyl ester APEO, stand 2h after stirring, is 300W in power, frequency is the microwave of 20GHz
Then lower processing 3 times, each 20s is 40kV/cm in field strength, pulse frequency is that the high-voltage pulse electric of 600pps is handled off field
It is 6 that then hydrochloric acid solution that 1ms is 0.1mol/L with molar concentration, which adjusts PH, is 400W in power, frequency is 40KHz ultrasound
Wave extracts 20min, filters, and collects filtrate, and filter residue repeats above-mentioned steps and extracts once, filter, merges filtrate twice, discard filter
Slag is added 0.3g% sodium ascorbate to filtrate, is placed in 5 DEG C of refrigerators and refrigerates 48h, removes bottom sediment, rotate at 50 DEG C
Evaporation recycling acetone is simultaneously concentrated into the 1/2 of original volume, and centrifuge separation takes supernatant；
(3) supernatant will be added after U.S.'s Amberlite XAD-16 macroreticular resin wet method dress post to adsorb, column diameter and tree
The ratio between rouge height is 1: 8, is eluted after absorption with the ethanol water that volume fraction is 60%, and adjusting flow velocity is 6BV/h,
Collect eluent；
(4) by eluent obtained above, rotary evaporation recycles ethyl alcohol and is concentrated into the 4/5 of original volume at 50 DEG C, so
After be put into -65 DEG C of refrigerators and freeze 30min, place into freeze drier dry 48h to get chlorogenic acid crude product 4.42.
Comparative example 1
A kind of method of microwave combination ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid, includes the following steps:
(1) 100g tobacco waste is dried at 50 DEG C, is crushed, cross 20 meshes；
(2) smashed tobacco waste is placed in 560mL acetone and 560mL water mixes in the solvent of composition, be sufficiently stirred
1h is stood after uniformly, is 200W in power, is handled 2 times under the microwave that frequency is 10GHz, then each 30s is with molar concentration
It is 5 that the hydrochloric acid solution of 0.1mol/L, which adjusts PH, is 300W in power, extracts 30min under the ultrasonic wave that frequency is 30KHz, filter,
Filtrate is collected, filter residue repeats above-mentioned steps and extracts once, filter, merges filtrate twice, discard filter residue, filtrate is placed in 2 DEG C of ice
It is refrigerated in case for 24 hours, removes bottom sediment, rotary evaporation recycles acetone and is concentrated into the 1/3 of original volume at 40 DEG C, centrifugation point
From taking supernatant；
(3) supernatant will be added after U.S.'s Amberlite XAD-16 macroreticular resin wet method dress post to adsorb, column diameter and tree
The ratio between rouge height is 1: 6, is eluted after absorption with the ethanol water that volume fraction is 40%, and adjusting flow velocity is 3BV/h,
Collect eluent；
(4) by eluent obtained above, rotary evaporation recycles ethyl alcohol and is concentrated into the 3/5 of original volume at 40 DEG C, so
After be put into -50 DEG C of refrigerators and freeze 50min, place into freeze drier and dry for 24 hours to get chlorogenic acid crude product 3.26.
Comparative example 2
A kind of method of microwave combination ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid, includes the following steps:
(1) 100g tobacco waste is dried at 55 DEG C, is crushed, cross 30 meshes；
(2) smashed tobacco waste is placed in 524mL acetone and 786mL water mixes in the solvent of composition, be sufficiently stirred
1.5h is stood after uniformly, is 250W in power, is handled 3 times under the microwave that frequency is 15GHz, then each 25s uses molar concentration
It is 5.5 for the hydrochloric acid solution adjusting PH of 0.1mol/L, is 350W in power, extracts 25min under the ultrasonic wave that frequency is 35KHz,
It filters, collects filtrate, filter residue repeats above-mentioned steps and extracts once, filter, merges filtrate twice, discard filter residue, filtrate is placed in 3
36h is refrigerated in DEG C refrigerator, removes bottom sediment, rotary evaporation recycling acetone and is concentrated into the 1/3 of original volume at 45 DEG C, from
Heart separation takes supernatant；
(3) supernatant will be added after U.S.'s Amberlite XAD-16 macroreticular resin wet method dress post to adsorb, column diameter and tree
The ratio between rouge height is 1: 7, is eluted after absorption with the ethanol water that volume fraction is 50%, and adjusting flow velocity is 4BV/h,
Collect eluent；
(4) by eluent obtained above, rotary evaporation recycles ethyl alcohol and is concentrated into the 3/5 of original volume at 45 DEG C, so
After be put into -60 DEG C of refrigerators and freeze 40min, place into freeze drier dry 36h to get chlorogenic acid crude product 3.58g.
Comparative example 3
A kind of method of microwave combination ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid, includes the following steps:
(1) tobacco waste is dried at 60 DEG C, is crushed, cross 40 meshes；
(2) smashed tobacco waste is placed in 538mL acetone and 1076mL water mixes in the solvent of composition, sufficiently
2h is stood after mixing evenly, is 300W in power, is handled under the microwave that frequency is 20GHz 3 times, each 20s, it is then dense with mole
It is 6 that the hydrochloric acid solution that degree is 0.1mol/L, which adjusts PH, is 400W in power, and frequency is 40KHz ultrasonic wave extraction 20min, is filtered,
Filtrate is collected, filter residue repeats above-mentioned steps and extracts once, filter, merges filtrate twice, discard filter residue, filtrate is placed in 5 DEG C of ice
48h is refrigerated in case, removes bottom sediment, and rotary evaporation recycles acetone and is concentrated into the 1/2 of original volume at 50 DEG C, centrifugation point
From taking supernatant；
(3) supernatant will be added after U.S.'s Amberlite XAD-16 macroreticular resin wet method dress post to adsorb, column diameter and tree
The ratio between rouge height is 1: 8, is eluted after absorption with the ethanol water that volume fraction is 60%, and adjusting flow velocity is 6BV/h,
Collect eluent；
(4) by eluent obtained above, rotary evaporation recycles ethyl alcohol and is concentrated into the 4/5 of original volume at 50 DEG C, so
After be put into -65 DEG C of refrigerators and freeze 30min, place into freeze drier dry 48h to get chlorogenic acid crude product 3.41g.
Embodiment 1-3 and comparative example 1-3 chlorogenic acid yield are measured:
1. chlorogenic acid crude product Content of Chlorogenic Acid measuring method
Eluent takes 0.2mL filtrate with 0.45 μm of membrane filtration before taking 2mL to be concentrated, and is placed in 10mL volumetric flask, with nothing
Water methanol dilution and constant volume, shake up.Sampling carries out reversed-phased high performace liquid chromatographic (RP-HPLC) measurement.Using with standard items ratio
It is legal compared with retention time, quantified by external standard method, analysis condition are as follows: chromatographic column: AgilentEclipseXDB-C18 (4.6mm ×
150mm,5μm)；Column temperature: room temperature；Mobile phase: acetonitrile: 2% acetic acid (volume ratio 13: 87), 1mL/min；Detection wavelength: 328nm；
Sample volume: 20 μ L.
2. chlorogenic acid yield calculation method
Chlorogenic acid quality/tobacco waste quality × 100%=chlorogenic acid crude product matter in chlorogenic acid yield=extract
Amount × chlorogenic acid crude product Content of Chlorogenic Acid/tobacco waste quality × 100%
3. result
Table 1
As seen from the above table, of the invention in conjunction with microwave compared with the method for ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid
High-pressure pulse electric combination microwave, ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid method can significantly improve the extraction of chlorogenic acid
Rate.This is that have following two reason: (1) with microwave in conjunction with ultrasonic wave compared with, high-pressure pulse electric combination microwave, ultrasonic wave tool
There is stronger penetration power, efficiently can quickly smash the cell wall of tobacco waste, maximization seeps intracellular effective component release
Thoroughly into solution, to improve the recovery rate of chlorogenic acid；(2) joined protective agent to prevent chlorogenic acid from aoxidizing, be additionally added it is non-from
Solvent can be improved to the affinity of chlorogenic acid in sub- surfactant, to improve the recovery rate of chlorogenic acid.Therefore, it uses
High-pressure pulse electric combination microwave, ultrasonic wave are the relatively good methods for extracting tobacco waste Content of Chlorogenic Acid.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to design of the invention
It is defined with range, without departing from the design concept of the invention, ordinary engineering and technical personnel is to this hair in this field
The all variations and modifications that bright technical solution is made should all fall into protection scope of the present invention, claimed skill of the invention
Art content is all documented in technical requirements book.
Claims (9)
1. a kind of method of high-pressure pulse electric combination microwave, ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid, it is characterised in that: packet
Include following steps:
(1) tobacco waste is dried at 50-60 DEG C, is crushed, cross 20-40 mesh；
(2) smashed tobacco waste is placed in the solvent for being equivalent to 10-15 times of tobacco waste weight, stands 1-2h, microwave
Processing 2-3 times, each 20-30s, then high-pressure pulse electric handles 1-3ms, the hydrochloric acid for being then 0.1mol/L with molar concentration
Solution adjusting PH is 5-6, ultrasonic wave extraction 20-30min, is filtered, and filtrate is collected, and filter residue repeats above-mentioned steps and extracts once,
It filters, merges filtrate twice, discard filter residue, the protective agent for being equivalent to tobacco waste quality 0.2-0.3% is added to filtrate, is placed in
24-48h is refrigerated in 2-5 DEG C of refrigerator, removes bottom sediment, rotary evaporation recycling acetone and the 1/3-1/2 for being concentrated into original volume,
Centrifuge separation takes supernatant；
(3) supernatant will be added after macroporous absorbent resin wet method dress post to adsorb, the ratio between column diameter and resin height are 1: 6-8, are inhaled
It is eluted after attached with the ethanol water that volume fraction is 40-60%, adjusting flow velocity is 3-6BV/h, collects eluent；
(4) eluent rotary evaporation obtained above is recycled into ethyl alcohol and is concentrated into the 3/5-4/5 of original volume, be then placed in-
30-50min is freezed in 50~-65 DEG C of refrigerators, places into freeze drier and dries 24-48h to get chlorogenic acid crude product.
2. a kind of high-pressure pulse electric combination microwave according to claim 1, ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid
Method, which is characterized in that the solvent is the solution that acetone and water form, and wherein the volume ratio of acetone and water is 1:1-2.
3. a kind of high-pressure pulse electric combination microwave according to claim 2, ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid
Method, which is characterized in that nonionic surfactant is also added in the solvent, the nonionic surfactant adds
Dosage be solvent quality 1-3%, the nonionic surfactant be collateralization 13 carbon Guerbet alcohol polyoxyethylene ether,
One of 12-14 carbon primary alconol polyoxyethylene ether, fatty acid methyl ester APEO.
4. a kind of high-pressure pulse electric combination microwave according to claim 1, ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid
Method, which is characterized in that the field strength of the high-pressure pulse electric be 25-40kV/cm, pulse frequency 400-600pps.
5. a kind of high-pressure pulse electric combination microwave according to claim 1, ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid
Method, which is characterized in that the power of the microwave be 200-300W, frequency 10-20GHz.
6. a kind of high-pressure pulse electric combination microwave according to claim 1, ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid
Method, which is characterized in that the power of the ultrasonic wave be 300-400W, frequency 30-40KHz.
7. a kind of high-pressure pulse electric combination microwave according to claim 1, ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid
Method, which is characterized in that the protective agent be sodium hydrogensulfite, sodium pyrosulfite, sodium ascorbate, in sodium isoascorbate
One kind.
8. a kind of high-pressure pulse electric combination microwave according to claim 1, ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid
Method, which is characterized in that the temperature of the rotary evaporation be 40-50 DEG C.
9. a kind of high-pressure pulse electric combination microwave according to claim 1, ultrasonic wave extraction tobacco waste Content of Chlorogenic Acid
Method, which is characterized in that the macroporous absorbent resin be U.S.'s Amberlite XAD-16 macroreticular resin.
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| CN1634853A (en) * | 2004-11-04 | 2005-07-06 | 南京师范大学 | Use of tobacco as raw materials for preparing chlorogenic acid and method for preparing chlorogenic acid by using tobacco |
| CN101805261A (en) * | 2010-03-26 | 2010-08-18 | 汉中天然谷生物科技有限公司 | Method for preparing competitive product of chlorogenic acid by folium cortex eucommiae |
| CN102491899A (en) * | 2011-11-24 | 2012-06-13 | 浙江大学 | Method for extracting natural antioxidant from waste tobacco powder by rotary focusing ultrasound-assisted extraction |
| CN104048866A (en) * | 2014-06-24 | 2014-09-17 | 广西中烟工业有限责任公司 | Method for extracting polyphenols from tobacco wastes |
| CN105130810A (en) * | 2015-09-30 | 2015-12-09 | 桂林三宝药业有限公司 | Method for extracting chlorogenic acid from honeysuckle |
| CN106478578A (en) * | 2016-08-30 | 2017-03-08 | 惠州学院 | A kind of method of physical field assisted extraction Exocarpium Litchi procyanidin |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1634853A (en) * | 2004-11-04 | 2005-07-06 | 南京师范大学 | Use of tobacco as raw materials for preparing chlorogenic acid and method for preparing chlorogenic acid by using tobacco |
| CN101805261A (en) * | 2010-03-26 | 2010-08-18 | 汉中天然谷生物科技有限公司 | Method for preparing competitive product of chlorogenic acid by folium cortex eucommiae |
| CN102491899A (en) * | 2011-11-24 | 2012-06-13 | 浙江大学 | Method for extracting natural antioxidant from waste tobacco powder by rotary focusing ultrasound-assisted extraction |
| CN104048866A (en) * | 2014-06-24 | 2014-09-17 | 广西中烟工业有限责任公司 | Method for extracting polyphenols from tobacco wastes |
| CN105130810A (en) * | 2015-09-30 | 2015-12-09 | 桂林三宝药业有限公司 | Method for extracting chlorogenic acid from honeysuckle |
| CN106478578A (en) * | 2016-08-30 | 2017-03-08 | 惠州学院 | A kind of method of physical field assisted extraction Exocarpium Litchi procyanidin |
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