CN105899222A - Green coffee bean extract and production method thereof - Google Patents
Green coffee bean extract and production method thereof Download PDFInfo
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- CN105899222A CN105899222A CN201380081795.7A CN201380081795A CN105899222A CN 105899222 A CN105899222 A CN 105899222A CN 201380081795 A CN201380081795 A CN 201380081795A CN 105899222 A CN105899222 A CN 105899222A
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- 241000533293 Sesbania emerus Species 0.000 title claims abstract description 123
- 229940069765 bean extract Drugs 0.000 title claims abstract description 61
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 35
- 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 claims abstract description 58
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 claims abstract description 46
- 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 claims abstract description 34
- 235000001368 chlorogenic acid Nutrition 0.000 claims abstract description 34
- 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 claims abstract description 33
- 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 claims abstract description 33
- 229940074393 chlorogenic acid Drugs 0.000 claims abstract description 33
- 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 claims abstract description 33
- 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 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 30
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 28
- CWVRJTMFETXNAD-GMZLATJGSA-N 5-Caffeoyl quinic acid 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-GMZLATJGSA-N 0.000 claims abstract description 25
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 24
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229960001948 caffeine Drugs 0.000 claims abstract description 23
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000003960 organic solvent Substances 0.000 claims abstract description 21
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 14
- 238000000638 solvent extraction Methods 0.000 claims abstract description 5
- 238000000605 extraction Methods 0.000 claims description 128
- 238000012545 processing Methods 0.000 claims description 53
- 239000000284 extract Substances 0.000 claims description 46
- 238000001914 filtration Methods 0.000 claims description 32
- 230000003068 static effect Effects 0.000 claims description 31
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000002904 solvent Substances 0.000 claims description 20
- 239000000919 ceramic Substances 0.000 claims description 19
- 239000012528 membrane Substances 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 10
- CLYOWAJOLXGKJG-BEWUSEGGSA-N (3R,5R)-3,4-bis[(E)-3-(3,4-dihydroxyphenyl)prop-2-enoyl]-1,3,4,5-tetrahydroxycyclohexane-1-carboxylic acid Chemical class C(\C=C\C1=CC(O)=C(O)C=C1)(=O)[C@]1(CC(C[C@H](C1(O)C(\C=C\C1=CC(O)=C(O)C=C1)=O)O)(C(=O)O)O)O CLYOWAJOLXGKJG-BEWUSEGGSA-N 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 5
- MBNNRMVOTYNNIX-HBEKLPNASA-N (3R,5R)-3,5-bis[(E)-3-(3,4-dihydroxyphenyl)prop-2-enoyl]-1,3,4,5-tetrahydroxycyclohexane-1-carboxylic acid Chemical class C(\C=C\C1=CC(O)=C(O)C=C1)(=O)[C@]1(CC(C[C@](C1O)(O)C(\C=C\C1=CC(O)=C(O)C=C1)=O)(C(=O)O)O)O MBNNRMVOTYNNIX-HBEKLPNASA-N 0.000 claims description 4
- 150000001298 alcohols Chemical group 0.000 claims description 4
- 150000002576 ketones Chemical class 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 150000007513 acids Chemical class 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 33
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000004615 ingredient Substances 0.000 abstract 2
- LTSOENFXCPOCHG-GQCTYLIASA-N 4-chloro-6-[[(e)-3-oxobut-1-enyl]amino]-1-n-prop-2-enylbenzene-1,3-disulfonamide Chemical compound CC(=O)\C=C\NC1=CC(Cl)=C(S(N)(=O)=O)C=C1S(=O)(=O)NCC=C LTSOENFXCPOCHG-GQCTYLIASA-N 0.000 abstract 1
- 239000000447 pesticide residue Substances 0.000 abstract 1
- 239000013557 residual solvent Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 77
- UFCLZKMFXSILNL-BBLPPJRLSA-N (-) 4,5-dicaffeoylquinic acid Natural products OC=1C=C(C=CC=1O)C=CC(=O)O[C@@H]1C[C@@](C[C@H]([C@H]1OC(C=CC1=CC(=C(C=C1)O)O)=O)O)(C(=O)O)O UFCLZKMFXSILNL-BBLPPJRLSA-N 0.000 description 24
- UFCLZKMFXSILNL-GCBRTHAASA-N 102851-07-0 Natural products OC=1C=C(C=CC=1O)C=CC(=O)O[C@@H]1C[C@](C[C@H]([C@@H]1OC(C=CC1=CC(=C(C=C1)O)O)=O)O)(C(=O)O)O UFCLZKMFXSILNL-GCBRTHAASA-N 0.000 description 24
- UFCLZKMFXSILNL-UHFFFAOYSA-N NSC 649410 Natural products C=1C=C(O)C(O)=CC=1C=CC(=O)OC1C(O)CC(O)(C(O)=O)CC1OC(=O)C=CC1=CC=C(O)C(O)=C1 UFCLZKMFXSILNL-UHFFFAOYSA-N 0.000 description 24
- GYFFKZTYYAFCTR-AVXJPILUSA-N (3r,5r)-4-[(e)-3-(3,4-dihydroxyphenyl)prop-2-enoyl]oxy-1,3,5-trihydroxycyclohexane-1-carboxylic acid Chemical compound O[C@@H]1CC(O)(C(O)=O)C[C@@H](O)C1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 GYFFKZTYYAFCTR-AVXJPILUSA-N 0.000 description 14
- GYFFKZTYYAFCTR-UHFFFAOYSA-N 5-O-(6'-O-galloyl)-beta-D-glucopyranosylgentisic acid Natural products OC1CC(O)(C(O)=O)CC(O)C1OC(=O)C=CC1=CC=C(O)C(O)=C1 GYFFKZTYYAFCTR-UHFFFAOYSA-N 0.000 description 14
- GYFFKZTYYAFCTR-LMRQPLJMSA-N cryptochlorogenic acid Natural products O[C@H]1C[C@@](O)(C[C@H](O)[C@H]1OC(=O)C=Cc2ccc(O)c(O)c2)C(=O)O GYFFKZTYYAFCTR-LMRQPLJMSA-N 0.000 description 14
- KRZBCHWVBQOTNZ-UHFFFAOYSA-N (-) 3,5-dicaffeoyl-muco-quinic acid Natural products OC1C(OC(=O)C=CC=2C=C(O)C(O)=CC=2)CC(O)(C(O)=O)CC1OC(=O)C=CC1=CC=C(O)C(O)=C1 KRZBCHWVBQOTNZ-UHFFFAOYSA-N 0.000 description 13
- KRZBCHWVBQOTNZ-RDJMKVHDSA-N (3r,5r)-3,5-bis[[(e)-3-(3,4-dihydroxyphenyl)prop-2-enoyl]oxy]-1,4-dihydroxycyclohexane-1-carboxylic acid Chemical compound O([C@@H]1CC(O)(C[C@H](C1O)OC(=O)\C=C\C=1C=C(O)C(O)=CC=1)C(O)=O)C(=O)\C=C\C1=CC=C(O)C(O)=C1 KRZBCHWVBQOTNZ-RDJMKVHDSA-N 0.000 description 13
- 239000000575 pesticide Substances 0.000 description 13
- UFCLZKMFXSILNL-PSEXTPKNSA-N Isochlorogenic acid b Chemical compound O([C@@H]1C[C@@](O)(C[C@H]([C@H]1OC(=O)\C=C\C=1C=C(O)C(O)=CC=1)O)C(O)=O)C(=O)\C=C\C1=CC=C(O)C(O)=C1 UFCLZKMFXSILNL-PSEXTPKNSA-N 0.000 description 12
- 239000006166 lysate Substances 0.000 description 12
- 238000001514 detection method Methods 0.000 description 11
- 239000007788 liquid Substances 0.000 description 11
- MCWXGJITAZMZEV-UHFFFAOYSA-N dimethoate Chemical compound CNC(=O)CSP(=S)(OC)OC MCWXGJITAZMZEV-UHFFFAOYSA-N 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 10
- HOQADATXFBOEGG-UHFFFAOYSA-N isofenphos Chemical compound CCOP(=S)(NC(C)C)OC1=CC=CC=C1C(=O)OC(C)C HOQADATXFBOEGG-UHFFFAOYSA-N 0.000 description 10
- 239000012071 phase Substances 0.000 description 10
- AMFGTOFWMRQMEM-UHFFFAOYSA-N triazophos Chemical compound N1=C(OP(=S)(OCC)OCC)N=CN1C1=CC=CC=C1 AMFGTOFWMRQMEM-UHFFFAOYSA-N 0.000 description 10
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 239000000706 filtrate Substances 0.000 description 8
- 239000004480 active ingredient Substances 0.000 description 7
- 238000010790 dilution Methods 0.000 description 7
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- 230000000052 comparative effect Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000000470 constituent Substances 0.000 description 5
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- 239000003905 agrochemical Substances 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 238000002481 ethanol extraction Methods 0.000 description 4
- 231100001261 hazardous Toxicity 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- NRHBUMVXUGSZAT-IVUGMLEJSA-N (3R,5R)-3-[(E)-3-(3,4-dihydroxyphenyl)prop-2-enoyl]-1,3,4,5-tetrahydroxycyclohexane-1-carboxylic acid Chemical class O[C@@H]1CC(O)(C[C@@](O)(C1O)C(=O)\C=C\c1ccc(O)c(O)c1)C(O)=O NRHBUMVXUGSZAT-IVUGMLEJSA-N 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 241000723377 Coffea Species 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 230000001093 anti-cancer Effects 0.000 description 2
- 230000000840 anti-viral effect Effects 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- 230000000144 pharmacologic effect Effects 0.000 description 2
- QAIPRVGONGVQAS-DUXPYHPUSA-N trans-caffeic acid Chemical compound OC(=O)\C=C\C1=CC=C(O)C(O)=C1 QAIPRVGONGVQAS-DUXPYHPUSA-N 0.000 description 2
- AAWZDTNXLSGCEK-WYWMIBKRSA-N (-)-quinic acid Chemical compound O[C@@H]1C[C@](O)(C(O)=O)C[C@@H](O)[C@H]1O AAWZDTNXLSGCEK-WYWMIBKRSA-N 0.000 description 1
- ACEAELOMUCBPJP-UHFFFAOYSA-N (E)-3,4,5-trihydroxycinnamic acid Natural products OC(=O)C=CC1=CC(O)=C(O)C(O)=C1 ACEAELOMUCBPJP-UHFFFAOYSA-N 0.000 description 1
- VTMFDSJJVNQXLT-RYPCIWMOSA-N 4-O-feruloylquinic acid Natural products COc1cc(C=CC(=O)O[C@@H]2[C@H](O)C[C@](O)(C[C@H]2O)C(=O)O)ccc1O VTMFDSJJVNQXLT-RYPCIWMOSA-N 0.000 description 1
- JYECSZVOTKUSPW-GSNAECIPSA-N C(\C=C\C1=CC(OC)=C(O)C=C1)(=O)[C@@]1(C([C@@H](CC(C1)(C(=O)O)O)O)O)O Chemical class C(\C=C\C1=CC(OC)=C(O)C=C1)(=O)[C@@]1(C([C@@H](CC(C1)(C(=O)O)O)O)O)O JYECSZVOTKUSPW-GSNAECIPSA-N 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 241000123069 Ocyurus chrysurus Species 0.000 description 1
- 244000046052 Phaseolus vulgaris Species 0.000 description 1
- 235000010627 Phaseolus vulgaris Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 235000004883 caffeic acid Nutrition 0.000 description 1
- 229940074360 caffeic acid Drugs 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- QAIPRVGONGVQAS-UHFFFAOYSA-N cis-caffeic acid Natural products OC(=O)C=CC1=CC=C(O)C(O)=C1 QAIPRVGONGVQAS-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000003808 methanol extraction Methods 0.000 description 1
- 239000000401 methanolic extract Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- RAGZUCNPTLULOL-UHFFFAOYSA-N trans-3-feruloylquinic acid Natural products C1=C(O)C(OC)=CC(C=CC(=O)OC2C(C(O)CC(O)(C2)C(O)=O)O)=C1 RAGZUCNPTLULOL-UHFFFAOYSA-N 0.000 description 1
- VTMFDSJJVNQXLT-UHFFFAOYSA-N trans-4-feruloylquinic acid Natural products C1=C(O)C(OC)=CC(C=CC(=O)OC2C(CC(O)(CC2O)C(O)=O)O)=C1 VTMFDSJJVNQXLT-UHFFFAOYSA-N 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/74—Rubiaceae (Madder family)
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2300/00—Processes
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2300/00—Processes
- A23V2300/44—Supercritical state
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Botany (AREA)
- Mycology (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Medical Informatics (AREA)
- Epidemiology (AREA)
- Food Science & Technology (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Nutrition Science (AREA)
- Medicinal Chemistry (AREA)
- Microbiology (AREA)
- Pharmacology & Pharmacy (AREA)
- Polymers & Plastics (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Tea And Coffee (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
Provided is a method for producing green coffee bean extract, the method comprising: conducting supercritical carbon dioxide treatment on green coffee bean raw material, and then employing organic solvent extraction to obtain the green coffee bean extractive. The obtained green coffee bean extractive product mainly contains 28-37% 5-caffeoylquinic acid, and 45-60% total chlorogenic acid. The present invention has no harmful residual solvent, dramatically reduces pesticide residue, and ensures no loss of content of effective ingredients while removing caffeine; the obtained green coffee bean extract product has high weight yield, high earnings, and low costs, greatly increases the content of effective ingredients, and is superior to the prior art, thus being suitable for large-scale industrial production and having broad application prospects and economic value.
Description
A kind of green coffee bean extract and its production method technical field
The present invention relates to extract and extractive technique field, in particular it relates to a kind of green coffee bean extract, and the extract production method.Background technology
Green coffee bean extract is from the green coffee bean of madder wort（Coffea sp.) in seed extract and separate and obtain, its main component is 5-CQA (5-CQAs）And its homologue 3-CQA (3-caffeoylquinic acids）, 4-CQA (4-CQs）, 3-FQA (3- feruloylquinic acids）, 4-FQA (4-FQAs）With 5-FQA (5-FQAs）Deng these are into belonging to chlorogenic acid or its isomer.
The pharmacological activity such as green coffee bean extract has anti-oxidant, antiviral, anticancer, the antibacterial or fat that disappears.American scientist newest research results show that green coffee bean extract has good weight losing function, and the plurality kinds of health care product by main component of green coffee bean extract are largely introduced to the market.
Produce at present after the prevailing technology of green coffee bean extract is crushed for green coffee bean with dilute alcohol product.The product that related process production is obtained has the hazardous solvents such as just own protective embankment, dichloromethane protective embankment residual；And the U.S. and EU market require just own below protective embankment content l ppm, dichloromethane protective embankment also has strict limitation, and above-mentioned technique is difficult to realize.The secondary coffee bean of powdery is used methanol extraction by India Kulathooran Ramalakshmi et al., just own protective embankment reflux extraction removes the oil substances in coffee bean extract, chloroform removes caffeine, Η Ρ -20 purification with macroreticular resin products, the weight yield for obtaining product is 7.46 ~ 10.46%, is dried to obtain methanolic extract and draws total chlorogenic acid content between 28.70 ~ 30.50 % using gradient method progress detection.
Chinese patent application CN201310116237.1 (publication numbers：CN103232346A, publication date：On August 7th, 2013）A kind of production process for extraction of chlorogenic acid from green coffee bean is disclosed, it is size-reduced using green coffee bean as raw material, extracted, concentration, centrifugal ultrafiltration, resin separation, elution are refining to obtain chlorogenic acid.There are some problems：Handled without deoiling step,
Product mobility can be impacted；Extraction temperature is too high（90 °C or so）, chlorogenic acid can be caused to lose.
Although also useful supercritical technology handles coffee bean in the technology reported at present, contribute to remove the caffeine in coffee bean, the condition of supercritical technology can influence active ingredient（Such as chlorogenic acid）Content and yield；Such as：Gen Foods Corp companies of the U.S. apply for a patent（EP 19800304045, publication date：On June 3rd, 1981) in mention using supercritical technology temperature be more than 70 °C, the technology main purpose is the caffeine in the green coffee bean of reduction, does not consider the situation of product content that the extraction and extraction of wherein main component chlorogenic acid obtain and yield.
Therefore, if a kind of production method can be developed, this method is simple to operate, and active ingredient is can guarantee that again while caffeine is removed（Chlorogenic acid）Content do not lose；Obtained extract product chlorogenic acid content height, income height, no hazardous solvent residual, low residues of pesticides, good fluidity, and suitable for industrialized production, huge application prospect and economic value certainly will be had.The content of the invention
In order to solve the above-mentioned technical problem, an object of the present invention is that there is provided a kind of method for producing green coffee bean extract.
Another object of the present invention is to there is provided a kind of green coffee bean extract.
To achieve these goals, the method for producing green coffee bean extract that the present invention is provided, including：Green coffee bean is subjected to CO 2 supercritical processing, is then extracted, produced using organic solvent.
Wherein, the CO 2 supercritical processing, including the technique that static and dynamic extraction is combined.
Wherein, the CO 2 supercritical processing, the technique for including two-stage parsing.
Using the CO 2 supercritical technology of the present invention, oil substances can be removed simultaneously
(such as coffee soya-bean oil）And caffeine；And static extracting is wherein used, on the other hand its advantage can save energy consumption for that on the one hand can reach extraction purpose.
Wherein, in the CO 2 supercritical processing, the extraction of static extracting and dynamic extraction
Temperature is 30 ~ 60 °C;Preferably 30 ~ 50 °C of the extraction temperature of static extracting, preferably 45 ~ 60 °C of the extraction temperature of dynamic extraction.The extraction temperature of quiet dynamic extraction can be operated more convenient with identical or different when temperature is identical.
Wherein, in the CO 2 supercritical processing, the resolution temperature of two-stage parsing is 30 ~ 50 °C.
Further, the temperature of two-stage parsing can be with identical or differ, when the temperature that two-stage is parsed is differed, preferably 40 ~ 50 °C of one-level resolution temperature, two grades of preferred 30-35 °C of resolution temperatures;When the temperature that two-stage is parsed is identical, preferably 35 ~ 45 °C of resolution temperature.
Wherein, in the CO 2 supercritical processing, the condition of static extracting also includes：Extracting pressure is 8 ~ 12 MPa, and extraction time is 20 ~ 30 minutes.
Wherein, in the CO 2 supercritical processing, the condition of dynamic extraction also includes：Extracting pressure is 21 ~ 30 MPa, and extraction time is 3 ~ 7 hours.
Wherein, in the CO 2 supercritical processing, during dynamic extraction, the mass ratio of solvent carbon dioxide and green coffee bean is 10: 1~70: 1.
Wherein, in the CO 2 supercritical processing, the condition of two-stage parsing also includes：One-level parsing pressure is 7.5 ~ 10 MPa, and two grades of parsing pressure are 4 ~ 6 MPa.
In the present invention, in CO 2 supercritical processing procedure, carbon dioxide flow is 1000-1500 L/h.
Wherein, extracted using organic solvent, condition includes：Solid-liquid ratio is set（The mass volume ratio of i.e. green coffee bean and organic solvent）For 1:3~1 :5；Extraction temperature is 40 ~ 60 °C, preferably 45 ~ 50 °C;Extraction 2 ~ 5 times, preferably 4 times；Every time during extraction, extraction time is 1 ~ 2 hour, preferably 1.5 hours.The condition extracted every time can be operated more convenient with identical or different when condition is identical.
Wherein, extracted using organic solvent, the water content of the organic solvent is 20 ~ 50%.Wherein, extracted using organic solvent, the organic solvent is alcohols or ketones solvent.Every time during extraction, the organic solvent used can be operated more convenient with identical or different when identical.
Further, the alcohols solvent is ethanol or isopropanol.
Further, the ketones solvent is acetone.
Method for producing green coffee bean extract of the present invention, before green coffee bean is carried out into CO 2 supercritical processing, in addition to：By green coffee bean roller sheet.
Wherein, it is described by green coffee bean roller sheet, including：Green coffee bean is under the conditions of 50 ~ 60 °C through roller sheet after water process 10 ~ 20 minutes, preferably 15 ~ 20 minutes.
Wherein, by green coffee bean roller sheet, water accounts for the 10 ~ 30% of green coffee bean quality.Wherein, by green coffee bean roller sheet, the parameter of roller sheet equipment used, that is, it is 0.1-0.3 mm to set piece thickness.
Further, by green coffee bean roller sheet, the water is pure water, and effect is that green coffee bean is humidified to soften.
Method for producing green coffee bean extract of the present invention, after using organic solvent extraction, in addition to：The extract being obtained by extraction using organic solvent is subjected to refinement treatment with ceramic membrane.
Wherein, the extract being obtained by extraction using organic solvent is subjected to refinement treatment with ceramic membrane, including：By the ceramic membrane filter that extract filtering accuracy is 10 ~ 50 KDa, temperature during filtering is 25 ~ 35 °C.It is removing protein, carbohydrate and microbial impurities with ceramic membrane filter purpose.
Method for producing green coffee bean extract of the present invention, the extract being obtained by extraction using organic solvent is carried out after refinement treatment with ceramic membrane, then be concentrated under reduced pressure to give paste；Paste by being dried in vacuo and crushing, obtains green coffee bean extract product again.
Wherein, paste is concentrated under reduced pressure to give, wherein the condition being concentrated under reduced pressure includes：Gas phase temperature is 55 ~ 65 °C, preferably 55 °C;Vacuum is -0.08 0.1 MPa.
Wherein, the vacuum drying temperature of paste is 50 ~ 60 °C, and vacuum is -0.08 ~ -0.1 MPa;Paste is crushed to 80 ~ 100 mesh.
Contain the composition of following weight/mass percentage composition in the green coffee bean extract that the present invention is provided, the extract product：5-CQA (5-CQAs）For 28-37%, 3-CQA (3- caffeoylquinic acids）For 2 ~ 7%, 4-CQA (4-CQs）For 2 ~ 6%,
3.4- diCQA (3,4- dicaffeoylquinic acids）For 0.2-4%, 3,5-diCQA (3,5- dicaffeoylquinic acids）For 0.2 ~ 4%, 4,5-diCQA (4,5- dicaffeoylquinic acids）For 0.15 ~ 2%.
Preferably, the composition of following weight/mass percentage composition is contained in the green coffee bean extract that the present invention is provided, the extract product：5-CQA is 28-37%, and 3-CQA is 2.0-2.7%, and 4-CQA is that 3.7 ~ 4.6%, 3,4-diCQA is that 1.0 ~ 1.3%, 3,5-diCQA is 3.0 ~ 4.0%,
4.5- diCQA are 12 ~ 17%.
Wherein, 5-CQA is preferably 34 ~ 37%.
The weight/mass percentage composition of the total chlorogenic acid contained in the green coffee bean extract that the present invention is provided, the extract product is 45 ~ 60%；Preferably 54 ~ 60%.
In the present invention, the amount of the amount of total chlorogenic acid and each chlorogenic acid isomer is all based on what green coffee bean extract product was calculated.
The green coffee bean extract that the present invention is provided, is obtained by above-mentioned any one method production of the invention, wherein the composition containing following weight/mass percentage composition：5-CQA (5-CQAs）For 28 ~ 37%, 3-CQA (3-caffeoylquinic acids）For 2 ~ 7%, 4-CQA (4-CQs）For 2-6%, 3,4-diCQA (3,4- dicaffeoylquinic acids）For 0.2-4%, 3,5-diCQA (3,5- dicaffeoylquinic acids）For 0.2-4%, 4,5-diCQA (4,5- dicaffeoylquinic acids）For 0.15 ~ 2%.
Preferably, the green coffee bean extract that the present invention is provided, is obtained by above-mentioned any one method production of the invention, wherein the composition containing following weight/mass percentage composition：5-CQA is 28-37%, and 3-CQA is that 2.0 ~ 2.7%, 4-CQA is that 3.7 ~ 4.6%, 3,4-diCQA is 1.0-1.3%, and 3,5-diCQA is that 30 ~ 40%, 4,5-diCQA is 12 ~ 17%.
Wherein, 5-CQA is preferably 34 ~ 37%.
The green coffee bean extract that the present invention is provided, is obtained by above-mentioned any one method production of the invention, wherein the weight/mass percentage composition of the total chlorogenic acid contained is 45 ~ 60%；Preferably 54 ~ 60%.
In any one above-mentioned green coffee bean extract that the present invention is provided, 5-CQA 28 ~ 37%, total chlorogenic acid 45 ~ 60% are mainly contained.
In any one above-mentioned green coffee bean extract that the present invention is provided, the weight/mass percentage composition of caffeine is less than 1.5%.
The production method that the present invention is provided, has the beneficial effect that：
1st, using C02Supercritical technology substitutes just own protective embankment and dichloromethane protective embankment removes oil substances and caffeine so that content of caffeine is less than 1.5% in extract;And product is remained without hazardous solvent, other dissolvent residuals are also very low（Less than 50ppm).
2nd, supercritical extract temperature control is at 30 ~ 60 °C, and resolution temperature is 30 ~ 50 °C, avoids influence of the high temperature to product content.Because chlorogenic acid is the ester that is formed by caffeic acid and chinic acid, there are ester bond, three l fractions of unsaturated double-bond and polyhydric phenols in its molecular structure, if environment meeting saboteur's structure for a long time more than 70 °C, so as to cause content loss, and then influence the yield of green coffee bean extract product.
3rd, without the total residual of the agricultural chemicals such as isofenphos, Hostathion, Rogor in the green coffee bean extract product of first supercritical processing in 3 ~ 5 ppm;And the agricultural chemicals total residual for using product after supercritical technology of the present invention processing is greatly reduced residues of pesticides in 0.01 below ppm.
4th, specific extractive technique and condition are applied in the extraction of specific green coffee bean, obtain the weight yield of product more than 11%, total chlorogenic acid content is more than 45% in dry products（Effect preferably for 54 ~ 60%), single chlorogenic acid content is more than 28% (effect is preferably 34 ~ 37%), and active constituent content is greatly promoted.
5th, in addition, because powder raw material using organic solvent extraction when filtration difficulty, the inventive method by green coffee bean carry out roller sheet processing, relative to whole beans extraction for improve product content and weight yield；Filter efficiency is improved relative to milling, production cost is reduced.
6th, the present invention is filtered with ceramic membrane, macromolecular substances of the molecular cut off more than 50000, to replace resin to realize the purifying of product；The water-soluble rear lysate clear of product can be realized.
7th, the good product mobility that the present invention is obtained, quality is high.
Therefore, the invention provides a kind of method simple and easy to apply, this method is remained without hazardous solvent, residues of pesticides are greatly reduced, and containing for active ingredient is can guarantee that again while caffeine is removed
Amount is not lost；Obtained green coffee bean extract product weight yield is high, and active constituent content is greatly promoted, and income is high, cost is low, better than prior art, and suitable for large-scale industrial production, with huge application prospect and economic value.Brief description of the drawings
Fig. 1 is green coffee bean extract production technological process of the invention.Embodiment
Following examples further illustrate present disclosure, but should not be construed as limiting the invention.Without departing from the spirit and substance of the case in the present invention, the modifications or substitutions made to the inventive method, step or condition, belong to the scope of the present invention.
Unless otherwise specified, the conventional meanses that NM technological means is well known to those skilled in the art in embodiment.The one-level parsing occurred is exactly first order parsing, and two grades of parsings are exactly second level parsing.The detection method of extract product（Liquid phase gradient detection method, the content of chlorogenic acid each component can be detected simultaneously）Also it is the conventional method and equipment of this area with relevant device.
Ceramic membrane used in the embodiment of the present invention is inorganic filter film, is the commodity CERMFIL of my long high-tech company of Nanjing.Water used is pure water.Using to unclassified stores be the conventional material that can commercially obtain.
In the present invention, the percentage " % " represented by active constituent content is mass percent.In the present invention, the unit K Da of filtering accuracy is kilodalton." total chlorogenic acid " occurred refers to all chlorogenic acids or the general name of its isomer, and " single chlorogenic acid " that refer to is exactly 5-CQA.Embodiment 1
The green coffee beans of 120 kg are weighed, raw material total acid is detected（That is total chlorogenic acid）Content is 7.0%, sets water to account for the 10% of material quality, and sofening treatment is humidified through water under the conditions of 60 °C（Material moisture is improved, and plays a part of entrainer in follow-up first supercritical processing）Roller sheet after 20min, flaking machine sets piece thickness to be 0.1 mm (roller sheet process raw material frees of losses）.
The technique that raw material after roller sheet is combined using static and dynamic extraction carries out first supercritical processing：Static extracting pressure is 8 MPa, and extraction time is 20min;Dynamic extraction pressure is
21 MPa, extraction time is 7h;The extraction temperature of static extracting is 42 °C, and the extraction temperature of dynamic extraction is 55 °C;During dynamic extraction, solvent C02Mass ratio with green coffee bean after roller sheet is 70: 1 ;CO 2 supercritical processing, is parsed using two-stage：One-level parsing pressure is 7.5 MPa, and-level resolution temperature is 45 °C;Two grades of parsing pressure are 4 MPa, and two grades of resolution temperatures are 30 °C.Carbon dioxide flow is 1000 L/h.
Green coffee bean roller sheet raw material after first supercritical processing, with 50% (mass fraction）Isopropyl alcohol extraction, feed liquid mass volume ratio be 1:4, temperature is 45 °C;Extraction 4 times, the time extracted every time is 1.5h.
The extract that will be obtained using isopropyl alcohol extraction, be concentrated under reduced pressure it is solvent-free after be diluted (normal condition）, dilution filtering accuracy is 50 KDa ceramic membrane filter, and temperature during filtering is 30 °C;After filtering is refined, filtrate is concentrated under reduced pressure to give paste under conditions of 55 °C of gas phase temperature, the MPa of vacuum -0.085；Paste obtains the green kg of coffee bean extract product 13.8 under 55 °C, the MPa of vacuum -0.085 by being dried in vacuo and being crushed to after 90 mesh, allotment;The water-soluble rear lysate clear of product, good fluidity.
The weight yield of product is 11.50%;Total chlorogenic acid content is 54.7%;5-CQA contents are that 34.2%, 3-CQA contents are that 2.46%, 4-CQA contents are that 4.21%, 3,4-diCQA contents are that 1.26%, 3,5-diCQA contents are that 3.75%, 4,5-diCQA contents are 1.53%, and other related isomer contents are 7.29%;Content of caffeine is 1.45%;The residues of pesticides of isofenphos, Hostathion and Rogor are 0.005 ppm in product, and dissolvent residual is 27 ppm.Embodiment 2
The green coffee beans of 120 kg are weighed, detection raw material total acid content is 6.7%, sets water to account for the 30% of material quality, and roller sheet after humidifying sofening treatment 15min through water under the conditions of 50 °C, flaking machine sets piece thickness to be 0.3 mm.
The technique that raw material after roller sheet is combined using static and dynamic extraction carries out first supercritical processing：Static extracting pressure is 12 MPa, and extraction time is 30min;Dynamic extraction pressure is 30 MPa, and extraction time is 3h;The extraction temperature of static extracting is 30 °C, and the extraction temperature of dynamic extraction is 60 °C;During dynamic extraction, solvent C02With green coffee bean after roller sheet
Mass ratio be 10:1 ;CO 2 supercritical processing, is parsed using two-stage：One-level parsing pressure is lO MPa, and-level resolution temperature is 40 °C;Two grades of parsing pressure are 6 MPa, and two grades of resolution temperatures are 30 °C.Carbon dioxide flow is 1400 L/h.
Green coffee bean roller sheet raw material after first supercritical processing, with 70% (mass fraction）Ethanol extraction, feed liquid mass volume ratio be 1:4,50 °C of temperature;Extraction 4 times, the time extracted every time is 1.5h.
The extract that will be obtained by extraction using ethanol, be concentrated under reduced pressure it is solvent-free after be diluted, dilution filtering accuracy is 30 KDa ceramic membrane filter, and temperature during filtering is 35 °C;After filtering is refined, filtrate is concentrated under reduced pressure to give paste under conditions of 55 °C of gas phase temperature, the MPa of vacuum -0.096；Paste obtains the green kg of coffee bean extract product 14.2 under 50 °C, the MPa of vacuum -0.096 by being dried in vacuo and being crushed to after 80 mesh, allotment;The water-soluble rear lysate clear of product, good fluidity.
The weight yield of product is 11.83%;Total chlorogenic acid content is 55.6%;5-CQA contents are that 35.03%, 3-CQA contents are that 2.5%, 4-CQA contents are that 4.28%, 3,4-diCQA contents are that 1.28%, 3,5-diCQA contents are that 3.81%, 4,5-diCQA contents are 1.56%, and other related isomer contents are 7.14%;Content of caffeine is 1.15%;The residues of pesticides of isofenphos, Hostathion and Rogor are 0.006 ppm in product, and dissolvent residual is 24 ppm.Embodiment 3
The green coffee beans of 120 kg are weighed, detection raw material total acid content is 6.7%, sets water to account for the 20% of material quality, and roller sheet after humidifying sofening treatment 15min through water under the conditions of 55 °C, flaking machine sets piece thickness to be 0.2 mm.
The technique that raw material after roller sheet is combined using static and dynamic extraction carries out first supercritical processing：Static extracting pressure is 10 MPa, and extraction time is 25min;Dynamic extraction pressure is 24 MPa, and extraction time is 5h;The extraction temperature of static extracting is 36 °C, and the extraction temperature of dynamic extraction is 54 °C;During dynamic extraction, solvent C02Mass ratio with green coffee bean after roller sheet is 40:1 ;CO 2 supercritical processing, is parsed using two-stage：One-level parsing pressure is 8 MPa, and-level resolution temperature is 50 °C;Two grades of parsing pressure are 5 MPa, two grades of solutions
Eutectoid temperature is 35 °C.Carbon dioxide flow is 1500 L/h.
Green coffee bean roller sheet raw material after first supercritical processing, with 80% (mass fraction）Acetone extract, feed liquid mass volume ratio be 1:4,50 °C of temperature;Extraction 4 times, the time extracted every time is 1.5h.
The extract that will be obtained using acetone extract, be concentrated under reduced pressure it is solvent-free after be diluted, dilution is with the ceramic membrane filter that filtering accuracy is lO KDa, and temperature during filtering is 25 °C;After filtering is refined, filtrate is concentrated under reduced pressure to give paste under conditions of 55 °C of gas phase temperature, the MPa of vacuum -0.09；Paste obtains the green kg of coffee bean extract product 13.2 under 60 °C, the MPa of vacuum -0.09 by being dried in vacuo and being crushed to after 100 mesh, allotment;The water-soluble rear lysate clear of product, good fluidity.
The weight yield of product is 11.0%;Total chlorogenic acid content is 60.0%;5-CQA contents are that 36.8%, 3-CQA contents are that 2.70%, 4-CQA contents are that 4.62%, 3,4-diCQA contents are that 1.38%, 3,5-diCQA contents are that 3.67%, 4,5-diCQA contents are 1.68%, other related isomer contents 9.15%;Content of caffeine is 1.21%;The residues of pesticides of isofenphos, Hostathion and Rogor are 0.006 ppm in product, and dissolvent residual is 18 ppm.
As can be seen from the above-described embodiment：The extract product effect that embodiment 1 ~ 3 is obtained is suitable.
Embodiment 4
The green coffee beans of 120 kg are weighed, 20 mesh sieves were crushed, detection raw material total acid content is 6.7%.
The technique that raw material after crushing is combined using static and dynamic extraction carries out first supercritical processing：Static extracting pressure is 10 MPa, and extraction time is 25min;Dynamic extraction pressure is 24 MPa, and extraction time is 5h;The extraction temperature of static extracting is 39 °C, and the extraction temperature of dynamic extraction is 46 °C;During dynamic extraction, solvent C02Mass ratio with the green coffee bean after crushing is 40:1 ;CO 2 supercritical processing, is parsed using two-stage：One-level parsing pressure is 8 MPa, and two grades of parsing pressure are 5 MPa, and two-stage resolution temperature is 40 °C.Carbon dioxide flow is 1500 L/h.
Green coffee bean powder raw material after first supercritical processing, with 80% (mass fraction）Acetone extract, feed liquid mass volume ratio be 1:3,50 °C of temperature;Extraction 4 times, the time extracted every time is 1.5h, and extract solution filtering is more difficult.
The extract that will be obtained using acetone extract, be concentrated under reduced pressure it is solvent-free after be diluted, dilution is with the ceramic membrane filter that filtering accuracy is lO KDa, and temperature during filtering is 25 °C;After filtering is refined, filtrate is concentrated under reduced pressure to give paste under conditions of 55 °C of gas phase temperature, the MPa of vacuum -0.09；Paste obtains the green kg of coffee bean extract product 16.5 under 60 °C, the MPa of vacuum -0.09 by being dried in vacuo and being crushed to after 100 mesh, allotment;The water-soluble rear lysate clear of product, good fluidity.
The weight yield of product is 13.75%;Total chlorogenic acid content is 48.7%;5-CQA contents are that 29.8%, 3-CQA contents are that 2.19%, 4-CQA contents are that 3.75%, 3,4-diCQA contents are that 1.12%, 3,5-diCQA contents are that 3.34%, 4,5-diCQA contents are 1.36%, and other related isomer contents are 7.14%;Content of caffeine is 1.22%;The residues of pesticides of isofenphos, Hostathion and Rogor are 0.009 ppm in product, and dissolvent residual is 35.8 ppm.
By the present embodiment it can be seen that：Without roller sheet processing raw material, when being extracted after first supercritical processing, extract solution filtering is more difficult；Product yield is not affected, but the content of active ingredient decreases in product.
Embodiment 5
The green coffee beans of 120 kg are weighed, detection raw material total acid content is 6.7%, sets water to account for the 20% of material quality, and roller sheet after humidifying sofening treatment 15min through water under the conditions of 55 °C, flaking machine sets piece thickness to be 0.2 mm.
The technique that raw material after roller sheet is combined using static and dynamic extraction carries out first supercritical processing：Static extracting pressure is 10 MPa, and extraction time is 25min;Dynamic extraction pressure is 24 MPa, and extraction time is 5h;The extraction temperature of quiet dynamic extraction is 45 °C;During dynamic extraction, solvent C02Mass ratio with green coffee bean after roller sheet is 40:1 ;CO 2 supercritical processing, is parsed using two-stage：One-level parsing pressure is 8 MPa, and two grades of parsing pressure are 5 MPa, and two-stage resolution temperature is 38 °C.Carbon dioxide flow is 1500 L/h.
Green coffee bean roller sheet raw material after first supercritical processing, with 80% (mass fraction）Acetone extract, feed liquid mass volume ratio be 1:5,50 °C of temperature;Extraction 3 times, extraction 2 hours, are extracted 1 hour every time in second and third time for the first time.
The extract obtained using acetone extract is concentrated under reduced pressure to give paste under conditions of 55 °C of gas phase temperature, the MPa of vacuum -0.09；Paste obtains the green kg of coffee bean extract product 15.1 under 60 °C, the MPa of vacuum -0.09 by being dried in vacuo and being crushed to after 100 mesh, allotment;The water-soluble rear lysate muddiness of product is opaque, and mobility is not so good.
The weight yield of product is 12.5%;Total chlorogenic acid content is 52.5%;5-CQA contents are that 32.55%, 3-CQA contents are that 2.36%, 4-CQA contents are that 4.04%, 3,4-diCQA contents are that 1.21%, 3,5-diCQA contents are that 3.60%, 4,5-diCQA contents are 1.47%, and other related isomer contents are 7.27%;Content of caffeine is 1.17%;The residues of pesticides of isofenphos, Hostathion and Rogor are 0.01 ppm in product, and dissolvent residual is 45.7 ppm.
By the present embodiment it can be seen that：After using acetone extract, without ceramic membrane refinement treatment extract, the water-soluble rear lysate muddiness of product is opaque；The yield of product is not affected, but the content of active ingredient decreases in product.
Embodiment 6
The green coffee beans of 120 kg are weighed, 20 mesh sieves were crushed, detection raw material total acid content is 6.7%.
The technique that raw material after crushing is combined using static and dynamic extraction carries out first supercritical processing：Static extracting pressure is 10 MPa, and extraction time is 25min;Dynamic extraction pressure is 24 MPa, and extraction time is 5h;The extraction temperature of quiet dynamic extraction is 49 °C;During dynamic extraction, solvent C02Mass ratio with the green coffee bean after crushing is 40:1 ;CO 2 supercritical processing, is parsed using two-stage：One-level parsing pressure is 8 MPa, and two grades of parsing pressure are 5 MPa, and two-stage resolution temperature is 45 °C.Carbon dioxide flow is 1500 L/h.
Green coffee bean powder raw material after first supercritical processing, with 80% (mass fraction）Acetone extract, feed liquid mass volume ratio be 1:4,50 °C of temperature;Extraction 4 times, the time extracted every time is 1.5h, and extract solution filtering is more difficult.
The extract that will be obtained using acetone extract, after being filtered with 1 μ η ι bag filters, filtrate is concentrated under reduced pressure to give paste under conditions of 55 °C of gas phase temperature, the MPa of vacuum -0.09；Paste obtains green coffee bean extract product 17.1kg under 60 °C, the MPa of vacuum -0.09 by being dried in vacuo and being crushed to after 100 mesh, allotment;The water-soluble rear lysate muddiness of product is opaque, and mobility is not so good.
The weight yield of product is 14.25%;Total chlorogenic acid content is 46.2%;5-CQA contents are that 28.6%, 3-CQA contents are that 2.08%, 4-CQA contents are that 3.56%, 3,4-diCQA contents are that 1.06%, 3,5-diCQA contents are that 3.17%, 4,5-diCQA contents are 1.29%, and other related isomer contents are 6.44%;Content of caffeine is 1.27%;The residues of pesticides of isofenphos, Hostathion and Rogor are 0.005 ppm in product, and dissolvent residual is 16.8 ppm.
By the present embodiment it can be seen that：Raw material is handled without roller sheet, while when being extracted after using acetone extract after extracted by filtration liquid in other ways, first supercritical processing, extract solution filtering is more difficult；Product yield is not affected, but the water-soluble rear lysate muddiness of product is opaque；And active constituent content decreases in product, to obtain total chlorogenic acid content be 50% extract product, it is necessary to be further purified.
Comparative example 1
The green coffee beans of 120 kg are weighed, detection raw material total acid content is 6.7%, sets water to account for the 30% of material quality, and roller sheet after humidifying sofening treatment 15min through water under the conditions of 50 °C, flaking machine sets piece thickness to be 0.3 mm.
The technique that raw material after roller sheet is combined using static and dynamic extraction carries out first supercritical processing：Static extracting pressure is 12 MPa, and extraction time is 30min;Dynamic extraction pressure is 30 MPa, and extraction time is 3h;The extraction temperature of quiet dynamic extraction is 78 °C;During dynamic extraction, solvent C02Mass ratio with green coffee bean after roller sheet is 10:1 ;CO 2 supercritical processing, is parsed using two-stage：One-level parsing pressure is 10 MPa, and two grades of parsing pressure are 6 MPa, and two-stage resolution temperature is 40 °C.Carbon dioxide flow is 1400 L/h.
Green coffee bean roller sheet raw material after first supercritical processing, with 70% (mass fraction）Ethanol extraction, feed liquid mass volume ratio be 1:4,50 °C of temperature;Extraction 4 times, extract every time when
Between be 1.5h.
The extract that will be obtained by extraction using ethanol, be concentrated under reduced pressure it is solvent-free after be diluted, dilution filtering accuracy is 30 KDa ceramic membrane filter, and temperature during filtering is 35 °C;After filtering is refined, filtrate is concentrated under reduced pressure to give paste under conditions of 55 °C of gas phase temperature, the MPa of vacuum -0.096；Paste obtains the green kg of coffee bean extract product 11.28 under 50 °C, the MPa of vacuum -0.096 by being dried in vacuo and being crushed to after 80 mesh, allotment;The water-soluble rear lysate clear of product, good fluidity.
The weight yield of product is 9.41%;Total chlorogenic acid content is 56.7%;5-CQA contents are that 34.8%, 3-CQA contents are that 2.55%, 4-CQA contents are that 4.37%, 3,4-diCQA contents are that 1.3%, 3,5-diCQA contents are that 3.89%, 4,5-diCQA contents are 1.59%, and other related isomer contents are 8.2%;Content of caffeine is 1.25%;The residues of pesticides of isofenphos, Hostathion and Rogor are 0.005 ppm in product, and dissolvent residual is 26.8 ppm.
It can be seen that by this comparative example：During first supercritical processing, if the extraction temperature of quiet dynamic extraction is higher, the removal effect to caffeine, agricultural chemicals in coffee bean can be reached, but the weight yield of product reduces more.
Comparative example 2
The green coffee beans of 120 kg are weighed, detection raw material total acid content is 6.7%, sets water to account for the 30% of material quality, and roller sheet after humidifying sofening treatment 15min through water under the conditions of 50 °C, flaking machine sets piece thickness to be 0.3 mm.
The technique that raw material after roller sheet is combined using static and dynamic extraction carries out first supercritical processing：Static extracting pressure is 12 MPa, and extraction time is 30min;Dynamic extraction pressure is 30 MPa, and extraction time is 3h;The extraction temperature of quiet dynamic extraction is 26 °C;During dynamic extraction, solvent C02Mass ratio with green coffee bean after roller sheet is 10:1 ;CO 2 supercritical processing, is parsed using two-stage：One-level parsing pressure is 10 MPa, and two grades of parsing pressure are 6 MPa, and two-stage resolution temperature is 35 °C.Carbon dioxide flow is 1200 L/h.
Green coffee bean roller sheet raw material after first supercritical processing, with 70% (mass fraction）Ethanol extraction, feed liquid mass volume ratio be 1:4,50 °C of temperature;Extraction 4 times, extract every time when
Between be 1.5h.
The extract that will be obtained by extraction using ethanol, be concentrated under reduced pressure it is solvent-free after be diluted, dilution filtering accuracy is 30 KDa ceramic membrane filter, and temperature during filtering is 35 °C;After filtering is refined, filtrate is concentrated under reduced pressure to give paste under conditions of 55 °C of gas phase temperature, the MPa of vacuum -0.096；Paste obtains the green kg of coffee bean extract product 16.1 under 50 °C, the MPa of vacuum -0.096 by being dried in vacuo and being crushed to after 80 mesh, allotment;The water-soluble rear lysate clear of product, good fluidity.
The weight yield of product is 13.4%;Total chlorogenic acid content is 43.7%;5-CQA contents are that 26.6%, 3-CQA contents are that 1.97%, 4-CQA contents are that 3.36%, 3,4-diCQA contents are that 1.01%, 3,5-diCQA contents are that 3.0%, 4,5-diCQA contents are 1.22%, and other related isomer contents are 6.54%;Content of caffeine is 8.69%;The residues of pesticides of isofenphos, Hostathion and Rogor are 4.2 ppm in product, and dissolvent residual is 35.6 ppm.
It can be seen that by this comparative example：During first supercritical processing, if the extraction temperature of quiet dynamic extraction is relatively low, the effect for removing caffeine and agricultural chemicals is poor, causes caffeine in product, residues of pesticides higher；Though the yield of product does not have much affect, the content of active ingredient decreases in product.
Comparative example 3
The green coffee beans of 120 kg are weighed, detection raw material total acid content is 6.7%, sets water to account for the 30% of material quality, and roller sheet after humidifying sofening treatment 17min through water under the conditions of 55 °C, flaking machine sets piece thickness to be 0.2mm.
The technique that raw material after roller sheet is combined using static and dynamic extraction carries out first supercritical processing：Static extracting pressure is 12 MPa, and extraction time is 30min;Dynamic extraction pressure is 30 MPa, and extraction time is 3h;The extraction temperature of quiet dynamic extraction is 100 °C;During dynamic extraction, solvent C02Mass ratio with green coffee bean after roller sheet is 20:1 ;CO 2 supercritical processing, is parsed using two-stage：One-level parsing pressure is 10 MPa, and-level resolution temperature is 85 °C;Two grades of parsing pressure are 6 MPa, and two grades of resolution temperatures are 70 °C.Carbon dioxide flow is 1300 L/h.
Green coffee bean roller sheet raw material after first supercritical processing, with 70% (mass fraction）Ethanol extraction, feed liquid mass volume ratio be 1:4,50 °C of temperature;Extraction 4 times, the time extracted every time is 1.5h.
The extract that will be obtained by extraction using ethanol, be concentrated under reduced pressure it is solvent-free after be diluted, dilution filtering accuracy is 30 KDa ceramic membrane filter, and temperature during filtering is 35 °C;After filtering is refined, filtrate is concentrated under reduced pressure to give paste under conditions of 55 °C of gas phase temperature, the MPa of vacuum -0.096；Paste obtains the green kg of coffee bean extract product 15.9 under 50 °C, the MPa of vacuum -0.096 by being dried in vacuo and being crushed to after 80 mesh, allotment;The water-soluble rear lysate clear of product, good fluidity.
The weight yield of product is 13.25%;Total chlorogenic acid content is 40.8%;5-CQA contents are that 25.3%, 3-CQA contents are that 1.84%, 4-CQA contents are that 3.14%, 3,4-diCQA contents are that 0.94%, 3,5-diCQA contents are that 2.8%, 4,5-diCQA contents are 1.14%, and other related isomer contents are 5.64%;Content of caffeine is 1.32%;The residues of pesticides of isofenphos, Hostathion and Rogor are 0.008 ppm in product, and dissolvent residual is 45.8 ppm.
It can be seen that by this comparative example：During first supercritical processing, if the extraction temperature of quiet dynamic extraction is higher, and resolution temperature it is also higher when, the content loss of active ingredient is larger, i.e., active constituent content is relatively low.
Although above the present invention is described in detail with a general description of the specific embodiments, on the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to the scope of protection of present invention.Industrial applicibility
The present invention provides a kind of method for producing green coffee bean extract, including：Green coffee bean is subjected to CO 2 supercritical processing, is then extracted, produced using organic solvent.Obtained green coffee bean extract product is produced, 5-CQA 28 ~ 37%, total chlorogenic acid 45 ~ 60%, with pharmacological activity such as anti-oxidant, antiviral, anticancer, the antibacterial or fat that disappears is mainly contained.
Claims (6)
- Claims1st, a kind of method for producing green coffee bean extract, including：Green coffee bean is subjected to CO 2 supercritical processing, is then extracted, produced using organic solvent.2nd, method for producing green coffee bean extract according to claim 1, it is characterised in that the CO 2 supercritical processing, including static extracting, dynamic extraction and two-stage parsing；The extraction temperature of static extracting and dynamic extraction is 30 ~ 60 °C;Preferably 30 ~ 50 °C of the extraction temperature of static extracting, preferably 45 ~ 60 °C of the extraction temperature of dynamic extraction；The resolution temperature of two-stage parsing is 30 ~ 50 °C;When the temperature that two-stage is parsed is differed, preferably 40 ~ 50 °C of one-level resolution temperature, preferably 30 ~ 35 °C of two grades of resolution temperatures;When the temperature that two-stage is parsed is identical, preferably 35 ~ 45 °C of resolution temperature.3rd, method for producing green coffee bean extract according to claim 2, it is characterised in that in the static extracting, extracting pressure is 8 ~ 12 MPa, and extraction time is 20 ~ 30 minutes；In the dynamic extraction, extracting pressure is 21 ~ 30 MPa, and extraction time is 3 ~ 7 hours, and the mass ratio of carbon dioxide and green coffee bean is 10: 1~70: 1；In the two-stage parsing, one-level parsing pressure is 7.5 ~ 10 MPa, and two grades of parsing pressure are 4-6 MPa.4th, the method for producing green coffee bean extract according to claim 1 ~ 3 any one, it is characterised in that the CO 2 supercritical processing, wherein carbon dioxide flow are 1000-1500 L/h.5th, the method for producing green coffee bean extract according to claim 1 ~ 4 any one, it is characterised in that using organic solvent extraction, condition includes：The mass volume ratio of green coffee bean and organic solvent is 1:3~1 :5, extraction temperature is 40 ~ 60 °C, preferably 45 ~ 50 °C;Extraction 2 ~ 5 times, is extracted 1 ~ 2 hour every time；It is preferred that extracting 4 times, extract 1.5 hours every time.6th, method for producing green coffee bean extract according to claim 1 or 5, it is characterised in that the organic solvent is alcohols or ketones solvent；The water content of the organic solvent is 20 ~ 50%. 7th, method for producing green coffee bean extract according to claim 6, it is characterised in that the alcohols solvent is ethanol or isopropanol, the ketones solvent is acetone.8th, the method for producing green coffee bean extract according to claim 1 ~ 7 any one, it is characterised in that before green coffee bean is carried out into CO 2 supercritical processing, in addition to：By green coffee bean roller sheet.9th, method for producing green coffee bean extract according to claim 8, it is characterised in that described by green coffee bean roller sheet, including：Green coffee bean is under the conditions of 50 ~ 60 °C through roller sheet after water process 10 ~ 20 minutes；Water accounts for the 10 ~ 30% of green coffee bean quality, and the piece thickness of roller sheet is 0.1 ~ 0.3 mm.10th, the method for producing green coffee bean extract according to claim 1 ~ 9 any one, it is characterised in that after using organic solvent extraction, in addition to：Extract is subjected to refinement treatment with ceramic membrane.11st, method for producing green coffee bean extract according to claim 10, it is characterised in that extract is subjected to refinement treatment with ceramic membrane, including：By the ceramic membrane filter that extract filtering accuracy is 10 ~ 50 KDa, temperature during filtering is 25 ~ 35 °C.12nd, the method for producing green coffee bean extract according to claim 10 or 11, it is characterised in that extract is carried out after refinement treatment with ceramic membrane, then is concentrated under reduced pressure to give paste；Paste by being dried in vacuo and crushing, obtains green coffee bean extract product again；The condition being concentrated under reduced pressure includes：Gas phase temperature is 55 ~ 65 °C, and vacuum is -0.08-0.1 MPa;The vacuum drying temperature of paste is 50 ~ 60 °C, and vacuum is -0.08-0.1 MPa;Paste is crushed to 80-100 mesh.13rd, a kind of green coffee bean extract, the method for producing green coffee bean extract production as described in claim 1 ~ 12 any one is obtained, wherein the composition containing following weight/mass percentage composition：5-CQA is 28 ~ 37%, and 3-caffeoylquinic acid is 2 ~ 7%, and 4-CQ is that 2 ~ 6%, 3,4- dicaffeoylquinic acids are that 0.2 ~ 4%, 3,5- dicaffeoylquinic acids are that 0.2 ~ 4%, 4,5- dicaffeoylquinic acids are 0.15 ~ 2%；The 5-CQA is preferably 34 ~ 37%. 14th, a kind of green coffee bean extract, the composition containing following weight/mass percentage composition：5- caffeoylquinic acids are 28 ~ 37%, and 3-caffeoylquinic acid is 2 ~ 7%, and 4-CQ is 2 ~ 6%, 3,4- dicaffeoylquinic acids are 0.2 ~ 4%, 3,5- dicaffeoylquinic acids are 0.2-4%, and 4,5- dicaffeoylquinic acids are 0.15 ~ 2%；The 5-CQA is preferably 34 ~ 37%.15th, the green coffee bean extract according to claim 13 or 14, it is characterised in that the weight/mass percentage composition of total chlorogenic acid is 45 ~ 60%, preferably 54 ~ 60%.16th, the green coffee bean extract according to claim 13 ~ 15 any one, it is characterised in that the weight/mass percentage composition of caffeine is less than 1.5%.
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| CN113304504A (en) * | 2021-06-08 | 2021-08-27 | 晨光生物科技集团股份有限公司 | Industrial technology for preparing green coffee bean extract |
| CN115155100A (en) * | 2022-06-02 | 2022-10-11 | 贵阳晨光生物科技有限公司 | Automatic supercritical extraction method |
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| JP2011057562A (en) * | 2009-09-05 | 2011-03-24 | Ucc Ueshima Coffee Co Ltd | Coffee bean extract having antiallergic activity and method for producing the same |
| JP2011057561A (en) * | 2009-09-05 | 2011-03-24 | Ucc Ueshima Coffee Co Ltd | Preventive against metabolic syndrome |
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| CN103232346B (en) * | 2013-04-06 | 2016-06-08 | 西安宏冠生物科技有限公司 | A kind of production technology of green coffee bean chlorogenic acid extracting |
| CN103251053B (en) * | 2013-05-23 | 2014-10-08 | 晨光生物科技集团天津有限公司 | Weight-reducing and beautifying composite and preparation method |
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| JP2011057561A (en) * | 2009-09-05 | 2011-03-24 | Ucc Ueshima Coffee Co Ltd | Preventive against metabolic syndrome |
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| CN115155100A (en) * | 2022-06-02 | 2022-10-11 | 贵阳晨光生物科技有限公司 | Automatic supercritical extraction method |
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