CN104083900A - Method for extracting volatile components from Pandanus amaryllifolius Roxb leaves - Google Patents
Method for extracting volatile components from Pandanus amaryllifolius Roxb leaves Download PDFInfo
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- CN104083900A CN104083900A CN201410336061.5A CN201410336061A CN104083900A CN 104083900 A CN104083900 A CN 104083900A CN 201410336061 A CN201410336061 A CN 201410336061A CN 104083900 A CN104083900 A CN 104083900A
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- 238000000034 method Methods 0.000 title claims abstract description 50
- 240000006353 Pandanus amaryllifolius Species 0.000 title abstract description 5
- 235000012110 Pandanus odorus Nutrition 0.000 title abstract description 5
- 238000000605 extraction Methods 0.000 claims abstract description 88
- 239000004615 ingredient Substances 0.000 claims description 34
- 239000002304 perfume Substances 0.000 claims description 30
- 235000013599 spices Nutrition 0.000 claims description 29
- 239000000284 extract Substances 0.000 claims description 19
- 238000000926 separation method Methods 0.000 claims description 6
- 239000000498 cooling water Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 238000005057 refrigeration Methods 0.000 claims description 5
- 230000001351 cycling effect Effects 0.000 claims description 4
- 238000001256 steam distillation Methods 0.000 abstract description 27
- BHEOSNUKNHRBNM-UHFFFAOYSA-N Tetramethylsqualene Natural products CC(=C)C(C)CCC(=C)C(C)CCC(C)=CCCC=C(C)CCC(C)C(=C)CCC(C)C(C)=C BHEOSNUKNHRBNM-UHFFFAOYSA-N 0.000 abstract description 19
- PRAKJMSDJKAYCZ-UHFFFAOYSA-N dodecahydrosqualene Natural products CC(C)CCCC(C)CCCC(C)CCCCC(C)CCCC(C)CCCC(C)C PRAKJMSDJKAYCZ-UHFFFAOYSA-N 0.000 abstract description 19
- 229940031439 squalene Drugs 0.000 abstract description 19
- TUHBEKDERLKLEC-UHFFFAOYSA-N squalene Natural products CC(=CCCC(=CCCC(=CCCC=C(/C)CCC=C(/C)CC=C(C)C)C)C)C TUHBEKDERLKLEC-UHFFFAOYSA-N 0.000 abstract description 19
- YYGNTYWPHWGJRM-UHFFFAOYSA-N (6E,10E,14E,18E)-2,6,10,15,19,23-hexamethyltetracosa-2,6,10,14,18,22-hexaene Chemical compound CC(C)=CCCC(C)=CCCC(C)=CCCC=C(C)CCC=C(C)CCC=C(C)C YYGNTYWPHWGJRM-UHFFFAOYSA-N 0.000 abstract description 18
- 239000000203 mixture Substances 0.000 abstract description 16
- 150000001875 compounds Chemical class 0.000 abstract description 14
- 239000000126 substance Substances 0.000 abstract description 10
- 239000001149 (9Z,12Z)-octadeca-9,12-dienoate Substances 0.000 abstract description 3
- DVWSXZIHSUZZKJ-UHFFFAOYSA-N 18:3n-3 Natural products CCC=CCC=CCC=CCCCCCCCC(=O)OC DVWSXZIHSUZZKJ-UHFFFAOYSA-N 0.000 abstract description 3
- IMKHDCBNRDRUEB-UHFFFAOYSA-N Dihydroactinidiolide Natural products C1CCC(C)(C)C2=CC(=O)OC21C IMKHDCBNRDRUEB-UHFFFAOYSA-N 0.000 abstract description 3
- IMKHDCBNRDRUEB-LLVKDONJSA-N dihydroactinidiolide Chemical compound C1CCC(C)(C)C2=CC(=O)O[C@@]21C IMKHDCBNRDRUEB-LLVKDONJSA-N 0.000 abstract description 3
- RUDATBOHQWOJDD-UHFFFAOYSA-N (3beta,5beta,7alpha)-3,7-Dihydroxycholan-24-oic acid Natural products OC1CC2CC(O)CCC2(C)C2C1C1CCC(C(CCC(O)=O)C)C1(C)CC2 RUDATBOHQWOJDD-UHFFFAOYSA-N 0.000 abstract 1
- JIGCTXHIECXYRJ-ILWBRPEASA-N [(e,7r,11r)-3,7,11,15-tetramethylhexadec-2-enyl] acetate Chemical compound CC(C)CCC[C@@H](C)CCC[C@@H](C)CCC\C(C)=C\COC(C)=O JIGCTXHIECXYRJ-ILWBRPEASA-N 0.000 abstract 1
- JIGCTXHIECXYRJ-UHFFFAOYSA-N trans-phytol acetate Natural products CC(C)CCCC(C)CCCC(C)CCCC(C)=CCOC(C)=O JIGCTXHIECXYRJ-UHFFFAOYSA-N 0.000 abstract 1
- RUDATBOHQWOJDD-UZVSRGJWSA-N ursodeoxycholic acid Chemical compound C([C@H]1C[C@@H]2O)[C@H](O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@H]([C@@H](CCC(O)=O)C)[C@@]2(C)CC1 RUDATBOHQWOJDD-UZVSRGJWSA-N 0.000 abstract 1
- 229960001661 ursodiol Drugs 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- 239000000243 solution Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 239000013558 reference substance Substances 0.000 description 6
- 239000000341 volatile oil Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 241000196324 Embryophyta Species 0.000 description 4
- 150000001298 alcohols Chemical class 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- -1 squalene compound Chemical class 0.000 description 4
- 150000001299 aldehydes Chemical class 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 235000013399 edible fruits Nutrition 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 150000007524 organic acids Chemical class 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 2
- 240000002390 Pandanus odoratissimus Species 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- RPKLZQLYODPWTM-KBMWBBLPSA-N cholanoic acid Chemical compound C1CC2CCCC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@@H](CCC(O)=O)C)[C@@]1(C)CC2 RPKLZQLYODPWTM-KBMWBBLPSA-N 0.000 description 2
- 238000010835 comparative analysis Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- GOQYKNQRPGWPLP-UHFFFAOYSA-N heptadecan-1-ol Chemical class CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- DVWSXZIHSUZZKJ-YSTUJMKBSA-N methyl linolenate Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(=O)OC DVWSXZIHSUZZKJ-YSTUJMKBSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 description 2
- 239000008158 vegetable oil Substances 0.000 description 2
- XBZYWSMVVKYHQN-MYPRUECHSA-N (4as,6as,6br,8ar,9r,10s,12ar,12br,14bs)-10-hydroxy-2,2,6a,6b,9,12a-hexamethyl-9-[(sulfooxy)methyl]-1,2,3,4,4a,5,6,6a,6b,7,8,8a,9,10,11,12,12a,12b,13,14b-icosahydropicene-4a-carboxylic acid Chemical compound C1C[C@H](O)[C@@](C)(COS(O)(=O)=O)[C@@H]2CC[C@@]3(C)[C@]4(C)CC[C@@]5(C(O)=O)CCC(C)(C)C[C@H]5C4=CC[C@@H]3[C@]21C XBZYWSMVVKYHQN-MYPRUECHSA-N 0.000 description 1
- 239000001707 (E,7R,11R)-3,7,11,15-tetramethylhexadec-2-en-1-ol Substances 0.000 description 1
- OJISWRZIEWCUBN-QIRCYJPOSA-N (E,E,E)-geranylgeraniol Chemical compound CC(C)=CCC\C(C)=C\CC\C(C)=C\CC\C(C)=C\CO OJISWRZIEWCUBN-QIRCYJPOSA-N 0.000 description 1
- XFDUHJPVQKIXHO-UHFFFAOYSA-N 3-aminobenzoic acid Chemical compound NC1=CC=CC(C(O)=O)=C1 XFDUHJPVQKIXHO-UHFFFAOYSA-N 0.000 description 1
- 241000989747 Maba Species 0.000 description 1
- 240000007817 Olea europaea Species 0.000 description 1
- 241000233929 Pandanaceae Species 0.000 description 1
- 235000005311 Pandanus odoratissimus Nutrition 0.000 description 1
- BLUHKGOSFDHHGX-UHFFFAOYSA-N Phytol Natural products CC(C)CCCC(C)CCCC(C)CCCC(C)C=CO BLUHKGOSFDHHGX-UHFFFAOYSA-N 0.000 description 1
- 241001529246 Platymiscium Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- HNZBNQYXWOLKBA-UHFFFAOYSA-N Tetrahydrofarnesol Natural products CC(C)CCCC(C)CCCC(C)=CCO HNZBNQYXWOLKBA-UHFFFAOYSA-N 0.000 description 1
- 241001482311 Trionychidae Species 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- BOTWFXYSPFMFNR-OALUTQOASA-N all-rac-phytol Natural products CC(C)CCC[C@H](C)CCC[C@H](C)CCCC(C)=CCO BOTWFXYSPFMFNR-OALUTQOASA-N 0.000 description 1
- UZFLPKAIBPNNCA-BQYQJAHWSA-N alpha-ionone Chemical compound CC(=O)\C=C\C1C(C)=CCCC1(C)C UZFLPKAIBPNNCA-BQYQJAHWSA-N 0.000 description 1
- UZFLPKAIBPNNCA-UHFFFAOYSA-N alpha-ionone Natural products CC(=O)C=CC1C(C)=CCCC1(C)C UZFLPKAIBPNNCA-UHFFFAOYSA-N 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
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- 239000012159 carrier gas Substances 0.000 description 1
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- 239000005350 fused silica glass Substances 0.000 description 1
- HNZUNIKWNYHEJJ-FMIVXFBMSA-N geranyl acetone Chemical compound CC(C)=CCC\C(C)=C\CCC(C)=O HNZUNIKWNYHEJJ-FMIVXFBMSA-N 0.000 description 1
- HNZUNIKWNYHEJJ-UHFFFAOYSA-N geranyl acetone Natural products CC(C)=CCCC(C)=CCCC(C)=O HNZUNIKWNYHEJJ-UHFFFAOYSA-N 0.000 description 1
- CCCXGQLQJHWTLZ-UHFFFAOYSA-N geranyl linalool Natural products CC(=CCCC(=CCCCC(C)(O)CCC=C(C)C)C)C CCCXGQLQJHWTLZ-UHFFFAOYSA-N 0.000 description 1
- IQDXAJNQKSIPGB-HQSZAHFGSA-N geranyllinalool Chemical compound CC(C)=CCC\C(C)=C\CC\C(C)=C\CCC(C)(O)C=C IQDXAJNQKSIPGB-HQSZAHFGSA-N 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- BOTWFXYSPFMFNR-PYDDKJGSSA-N phytol Chemical compound CC(C)CCC[C@@H](C)CCC[C@@H](C)CCC\C(C)=C\CO BOTWFXYSPFMFNR-PYDDKJGSSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
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- 239000013557 residual solvent Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 201000008827 tuberculosis Diseases 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a method for extracting volatile components from Pandanus amaryllifolius Roxb leaves by use of a supercritical CO2 extraction method. The method can obtain 151 compounds from the volatile components of Pandanus amaryllifolius Roxb, but a steam distillation method only can obtain 95 compounds, and extra 56 compounds, such as n-heptatriacontanyl alcohol, methyl linolenate, phytyl acetate, 3-hydroxyl-7 (isonitroso) ursodeoxycholic acid and dihydroactinidiolide, which cannot be obtained by the steam distillation method, are obtained by the method provided by the invention. The method for extracting the volatile components from Pandanus amaryllifolius Roxb leaves is superior to the steam distillation method in the aspects of smell, yield, chemical composition, squalene yield and extracting efficiency.
Description
Technical field
The present invention relates to extraction and separation technology field, relate in particular to a kind of method of extracting fragrant dew pocket volatile ingredient from perfume (or spice) dew pocket leaf.
Background technology
The fragrant pocket leaf system Pandanaceae of revealing is revealed the fragrant fresh blade (another name: Pandan Leaves, the blue perfume of plate, spot Lan Ye etc.) that reveals pocket (Pandanus amaryllifolius Roxb) of pocket genus.Fragrant dew pocket is evergreen draft, and leaf is about 30cm, wide about 1.5cm, and the accidental aculea of leaf margin, blade tip thorn is slightly close, and leaf back tip has aculea, and leaf sheath has narrow tunica albuginea, and flowers and fruits have no.Original producton location is Indonesia Ma Gulu archipelago.Research is found, the acid red earth of fragrant dew pocket adaptation south China, but because being subject to temperature limiting, being only adapted at Subtropic of China south edge to tropical area and growing.
Reveal at present the research of pocket chemical composition about perfume (or spice), less both at home and abroad.Mainly contain according to the literature the chemical compositions such as volatile oil, phytosterol, aliphatic acid, phenols and alkaloids.
Angle soft-shelled turtle alkene is natural chain triterpenoid, is important natural active matter, and main source is still abyssal fishes, and the distribution in plant is also very extensive, but content is not high.As relatively high in content in the vegetable oil of olive fruits, palm fruit, and also can detect at other vegetable oil, but content is generally all very low.
Employing steam distillation (SD) methods such as Ren Zhujun, Yin Gui person of outstanding talent decile adopt supercritical CO simply
2extraction (SFE-CO
2) method extracts, and by gaschromatographic mass spectrometry (GC-MS) combination analysis method, perfume (or spice) revealed to pocket leaf volatile oil chemical constitution study, result qualification composition negligible amounts, but all contain squalene.Described supercritical CO
2extraction process is very simple.
Tan M.A. etc. extract to separate and have obtained squalene compound in equal platymiscium aggag (Pandanus tectorius Soland.var.laevis) leaf, and are tested and shown that it has the biologically active for the treatment of tuberculosis effect by MABA.
The fragrant traditional extraction technique that reveals pocket volatile ingredient of bibliographical information mainly adopts steam distillation to follow the example of, but this extracting method exists deficiencies such as extraction efficiency is low, heat-sensitive substance easily decomposes, poor selectivity, and supercritical CO
2extract this novel green Chemical Engineering Technology and can overcome to a certain extent above-mentioned deficiency, not only in product, do not contain residual solvent, extraction process environmentally safe, and the composition of can remaining valid is not destroyed, extraction yield is compared with advantages of higher, and the especially suitable Effective Component of Chinese Medicine that is applied to fat-soluble, rudimentary property extracts.
Summary of the invention
The invention provides a kind of method of extracting fragrant dew pocket volatile ingredient from perfume (or spice) dew pocket leaf.
The present invention adopts following technical scheme:
The concrete steps of the method for extracting fragrant dew pocket volatile ingredient from perfume (or spice) dew pocket leaf of the present invention are as follows:
(1) perfume (or spice) is revealed to pocket cured leaf and be crushed to 20-100 order, for subsequent use;
(2) perfume (or spice) after step (1) pulverizing is revealed to pocket leaf and put into supercritical CO
2in the extraction kettle of extraction equipment;
(3) tighten extraction kettle cover, and check that whether separation kettle cover and valve are in closed condition;
(4) start power supply, connect cooling water, start refrigeration machine switch, and open the heater switch of extraction kettle, separating still I, separating still II and separating still III, and the temperature of setting extraction kettle is 35-55 DEG C, separating still I temperature is 35-50 DEG C, and separating still II temperature is 30-50 DEG C, and separating still III temperature is 30-50 DEG C;
(5) drop to 5-6 DEG C at refrigerator temps, and the temperature of extraction kettle, separating stills at different levels reaches the temperature of setting and when stable, open gas cylinder, air-source inflow valve, first discharge and catch up with the intrasystem air of extract and separate, in the time that extraction kettle pressure is consistent with sump pressure, start high-pressure pump, make extraction kettle pressure rise to gradually 15-27MPa;
(6) control valve of adjusting separating still, separating still I pressure is 9-18MPa, and separating still II pressure is 8-14MPa, and separating still III pressure is 4-8MPa, CO
2flow is 20-40Kg/h, and extraction time is 30-120min;
(7) extraction cycle finishes, and collection material from separating still obtains the fragrant pocket volatile ingredient that reveals.
In step (1), the fragrant pocket leaf that reveals is crushed to 60 orders.
In step (3), the temperature that preferably sets extraction kettle is 45 DEG C, and separating still I temperature is 45 DEG C, and separating still II temperature is 40 DEG C, and separating still III temperature is 40 DEG C.
In step (5), preferably extraction kettle pressure rises to 20MPa.
In step (6), preferable separate still I pressure is 12MPa, and separating still II pressure is 12MPa, and separating still III pressure is 6MPa.
In step (6), preferably CO
2flow is 30Kg/h.
In step (6), preferably extraction time is 60min.
In the perfume (or spice) dew pocket volatile ingredient that method of the present invention obtains, obtain 151 kinds of compounds, and steam distillation obtains 95 kinds, 56 kinds of compounds such as the inventive method method has more positive three heptadecanols, methyl linolenate, plants acetic acid, 3-hydroxyl-7 (isonitroso) cholanic acid, dihydroactinidiolide.
No matter the fragrant dew of the method gained pocket volatile ingredient that extracts fragrant dew pocket volatile ingredient of the present invention from perfume (or spice) dew pocket leaf is all excellent compared with steam distillation far away from yield or the extraction efficiency of the composition of smell, yield, chemical composition, squalene.
Brief description of the drawings
Fig. 1 is supercritical CO of the present invention
2extraction equipment schematic flow sheet.
In figure: 1-extraction kettle, 2-separating still I, 3-separating still II, 4-splitter, 5-heat exchanger, 6-high-pressure pump, 7-CO
2gas cylinder, the cold machine storage tank of 8-, 9-flowmeter, 10-separating still III.
Detailed description of the invention
The following examples are to describe in further detail of the present invention.
Embodiment 1
(1) perfume (or spice) is revealed to pocket cured leaf and be crushed to 20 orders, for subsequent use;
(2) perfume (or spice) after step (1) pulverizing is revealed to pocket leaf and put into supercritical CO
2in the extraction kettle of extraction equipment;
(3) tighten extraction kettle cover, and check that whether separation kettle cover and valve are in closed condition;
(4) start power supply, connect cooling water, start refrigeration machine switch, and open the heater switch of extraction kettle, separating still I, separating still II and separating still III, and the temperature of setting extraction kettle is 35 DEG C, separating still I temperature is 35 DEG C, and separating still II temperature is 30 DEG C, and separating still III temperature is 30 DEG C;
(5) drop to 5 DEG C at refrigerator temps, and the temperature of extraction kettle, separating stills at different levels reaches the temperature of setting and when stable, open gas cylinder, air-source inflow valve, first discharge and catch up with the intrasystem air of extract and separate, in the time that extraction kettle pressure is consistent with sump pressure, start high-pressure pump, make extraction kettle pressure rise to gradually 15MPa;
(6) control valve of adjusting separating still, separating still I pressure is 9MPa, and separating still II pressure is 8MPa, and separating still III pressure is 4MPa, starts cycling extraction, CO
2flow is 20Kg/h, and extraction time is 120min;
(7) extraction cycle finishes, and collection material from separating still obtains the fragrant pocket volatile ingredient that reveals.
Embodiment 2
(1) perfume (or spice) is revealed to pocket cured leaf and be crushed to 100 orders, for subsequent use;
(2) perfume (or spice) after step (1) pulverizing is revealed to pocket leaf and put into supercritical CO
2in the extraction kettle of extraction equipment;
(3) tighten extraction kettle cover, and check that whether separation kettle cover and valve are in closed condition;
(4) start power supply, connect cooling water, start refrigeration machine switch, and open the heater switch of extraction kettle, separating still I, separating still II and separating still III, and the temperature of setting extraction kettle is 55 DEG C, separating still I temperature is 50 DEG C, and separating still II temperature is 50 DEG C, and separating still III temperature is 50 DEG C;
(5) reach the temperature of setting and when stable in the temperature of extraction kettle, separating stills at different levels, open gas cylinder, air-source inflow valve, first discharge and catch up with the intrasystem air of extract and separate, in the time that extraction kettle pressure is consistent with sump pressure, start high-pressure pump, make extraction kettle pressure rise to gradually 27MPa;
(6) control valve of adjusting separating still, separating still I pressure is 18MPa, and separating still II pressure is 14MPa, and separating still III pressure is 8MPa, starts cycling extraction, CO
2flow is 40Kg/h, and extraction time is 30min;
(7) extraction cycle finishes, and collection material from separating still obtains the fragrant pocket volatile ingredient that reveals.
Embodiment 3
(1) perfume (or spice) is revealed to the fresh cured leaf of pocket and be crushed to 60 orders, for subsequent use;
(2) perfume (or spice) after step (1) pulverizing is revealed to pocket leaf and put into supercritical CO
2in the extraction kettle of extraction equipment;
(3) tighten extraction kettle cover, and check that whether separation kettle cover and valve are in closed condition;
(4) start power supply, connect cooling water, start refrigeration machine switch, and open the heater switch of extraction kettle, separating still I, separating still II and separating still III, and the temperature of setting extraction kettle is 45 DEG C, separating still I temperature is 45 DEG C, and separating still II temperature is 40 DEG C, and separating still III temperature is 40 DEG C;
(5) reach the temperature of setting and when stable in the temperature of extraction kettle, separating stills at different levels, open gas cylinder, air-source inflow valve, first discharge and catch up with the intrasystem air of extract and separate, in the time that extraction kettle pressure is consistent with sump pressure, start high-pressure pump, make extraction kettle pressure rise to gradually 20MPa;
(6) control valve of adjusting separating still, separating still I pressure is 12MPa, and separating still II pressure is 12MPa, and separating still III pressure is 6MPa, starts cycling extraction, CO
2flow is 30Kg/h, and extraction time is 60min;
(7) extraction cycle finishes, and collection material from separating still obtains the fragrant pocket volatile ingredient that reveals.
Comparative example (steam distillation extraction)
According to " Chinese pharmacopoeia " version annex XD determination of volatile oil method in 2010, accurately take the fragrant pocket leaf 150g that reveals, put in 2000ml round-bottomed flask, 1500ml adds water, soak 0.5h, put in electric jacket and be slowly heated to seethe with excitement, and keep micro-about 6h that boils, no longer increase to oil mass in analyzer, stop heating, place a moment, collect the volatile oil in extractor, weigh, calculate the fragrant pocket volatile ingredient yield that reveals, measure squalene content.
Test experience
The yield of 1 volatile ingredient and the content of squalene
The yield of volatile ingredient prepared by embodiment 1-3 and the content of squalene are measured, and result is as shown in table 1:
Squalene content assaying method-HPLC chromatographic condition
Chromatographic column: Agilent Eclipse XDB-C18 (4.6mm × 150mm, 5 μ are m);
Column temperature: 30 DEG C; Mobile phase: methyl alcohol, flow velocity 1.0ml/min; Detect wavelength: 204nm;
Detection time: 30min; Sample size: 10 μ l.
Table 1
2 supercritical COs
2extraction (SFE-CO
2) the extraction effect contrast of method and steam distillation (SD) method
Taking embodiment 3 and comparative example as example, contrast supercritical CO of the present invention
2extraction (SFE-CO
2) extraction effect of method and steam distillation (SD) method.
2.1 experimental technique
2.1.1HPLC chromatographic condition
Chromatographic column: Agilent Eclipse XDB-C
18(4.6mm × 150mm, 5 μ are m);
Column temperature: 30 DEG C; Mobile phase: methyl alcohol, flow velocity 1.0ml/min; Detect wavelength: 204nm;
Detection time: 30min; Sample size: 10 μ l.
2.1.2GC-MS chromatographic condition
GC conditions: (60m × 0.25mm × 0.25 μ m) for TR-5MS fused-silica capillary column, heating schedule: 55 DEG C of initial temperatures, rise to 180 DEG C with 5 DEG C/min of programming rate, rise to 250 DEG C with 2 DEG C/min of programming rate again, finally rise to 280 DEG C with 3 DEG C/min of programming rate, keep 45min after reaching 280 DEG C.Do not shunt 280 DEG C of injector temperatures, flow rate of carrier gas 1.0ml/min, sample size 0.5 μ l.
Mass spectrum condition: ionization mode is electronics bombardment (EI); Electron energy 70eV; 280 DEG C of transmission line temperature, 230 DEG C of ion source temperatures; Full scan 40-450amu, solvent delay 7min.
2.1.3 reference substance solution preparation
Get squalene reference substance 0.01g, accurately weighed, add methyl alcohol ultrasonic dissolution, and be settled in the brown measuring bottle of 5ml, as squalene reference substance stock solution.
Precision pipettes squalene reference substance stock solution 3ml, puts in the brown measuring bottle of 25ml, adds methyl alcohol to be diluted to scale, and with miillpore filter, (0.45 μ m) filters, as squalene reference substance solution.
2.1.4 the preparation of need testing solution
(1) the fragrant pocket steam distillation extract that reveals accurately takes processed perfume (or spice) dew pocket leaf 300g, puts in 5000ml round-bottomed flask, distills by " Chinese pharmacopoeia " version annex XD determination of volatile oil method in 2010, collect sample in extractor, weigh, calculated yield, as sample VII.Precision takes 0.01g, with acetic acid ethyl dissolution, is settled in 10ml measuring bottle, and anhydrous sodium sulfate drying, shakes up, and draws supernatant, and (0.45 μ m) filters miillpore filter, as need testing solution VII, carries out GC-MS analysis.
(2) the fragrant pocket supercritical CO that reveals
2extract is got supercritical CO
2the perfume (or spice) that extraction optimum process makes reveals pocket volatile ingredient 12.0g, accurately weighed, puts in round-bottomed flask, distill by " Chinese pharmacopoeia " version annex XD determination of volatile oil method in 2010, collect sample in extractor, as sample VIII, precision takes 0.01g, with acetic acid ethyl dissolution, is settled in 10ml measuring bottle, anhydrous sodium sulfate drying, shake up, draw supernatant, (0.45 μ m) filters miillpore filter, as need testing solution VIII, carry out GC-MS analysis.
(3) get above-mentioned fragrant pocket volatile extract sample VII, the each 0.02g of VIII of revealing, accurately weighed, add methyl alcohol ultrasonic dissolution, and be settled in the brown measuring bottle of 10ml, with miillpore filter, (0.45 μ m) filters, as need testing solution IX, X.
2.1.5 the fragrant pocket analysis of volatile components that reveals is identified
Precision is enfleuraged and is revealed pocket need testing solution VII, the each 0.5 μ l of VIII, measures by 2.2 GC-MS chromatographic conditions.
2.1.6 squalene assay
Accurate squalene reference substance solution, fragrant pocket need testing solution IX, the each 10 μ l of X of revealing of drawing, measure by 2.1.1 item chromatographic condition, record peak area integrated value, calculate squalene content.
2.2 experimental result
2.2.1 fragrant comparison of revealing pocket volatile ingredient kind
SD method, SFE-CO
2the compound that the perfume (or spice) that method is extracted reveals pocket volatile ingredient has respectively 95 kinds, 151 kinds, kind, the corresponding number of contained compound composition and account for the total percentage composition difference relatively of volatile ingredient as table 1,2.
Perfume (or spice) prepared by table 1 Different Extraction Method reveals pocket volatile ingredient classes of compounds composition number
Perfume (or spice) prepared by table 2 Different Extraction Method reveals all kinds of relative percentage compositions of pocket volatile ingredient
Can be found out by table 1,2 results, the fragrant pocket volatile ingredient that reveals mainly contains 8 large compounds, is respectively ester class, alkanes, aldehydes, ketone, alcohols, olefines, organic acid and other compounds.Wherein, the perfume (or spice) that SD method is extracted reveals pocket volatile ingredient taking alcohols, olefines, organic acid, aldehydes as main, accounts for respectively fragrant 50.52%, 17.27%, 8.22%, 8.03% of the pocket volatile ingredient total amount of revealing; The perfume (or spice) that SFE-CO2 method is extracted reveals pocket volatile ingredient mainly taking organic acid, ester class, alcohols, olefines as main, accounts for respectively fragrant 27.68%, 18.77%, 18.54%, 13.94% of the pocket volatile ingredient total amount of revealing.
2.2.2 fragrant comparative analysis of revealing pocket volatile chemical component
Use GC-MS GC-MS to reveal pocket need testing solution to different preparation methods' perfume (or spice) and detect, measurement result adopts NIST11Libraries spectrum library to retrieve, and in conjunction with artificial spectrum elucidation and check related data analysis, the results are shown in Table 3
The comparison of the fragrant dew of table 3 Different Extraction Method preparation pocket analysis of volatile components
2.2.3 comprehensively compare
Reveal pocket volatile ingredient proterties, yield, chemical composition composition number, squalene yield and extraction time as index evaluation steam distillation, supercritical CO taking perfume (or spice)
2the advantage that extraction extracts is with not enough, and the method that selective extraction efficiency is high, outward appearance good, productive rate is high and squalene yield is high, the results are shown in Table 4.
The fragrant comparison of revealing pocket volatile ingredient Different Extraction Method of table 4
2.3 conclusion
By comparing SD method and SFE-CO
2the chemical composition that method is extracted, can find out, traditional SD method gained low boiling point component as the number of alcohols, aldehydes, ketone compounds and relative amount higher, its reason SD method is mainly to extract some low boilings, volatile compound composition.SFE-CO
2method, except obtaining above compound, also extracts the compound that some boiling points are higher, molecular weight is larger.
By supercritical CO
2the perfume (or spice) of extraction reveals the volatile ingredient information content of pocket volatile ingredient gained after steam distillation and carries out steam distillation gained much larger than direct employing crude drug.Simultaneously the two has 35 identical components, mainly contains squalene, phytol, plants ketone, trans-Geranylgeraniol, geranyl acetone, geranyl linalool, α-ionone etc.Supercritical CO is described
2extract carries out GC-MS detection again and contributes to supercritical CO after steam distillation
2the analysis more comprehensively of extract chemical composition.
Comparative analysis is found, SFE-CO
2method obtains 151 kinds of compounds, and SD method obtains 95 kinds, SFE-CO
2method than SD method have more positive three heptadecanols, methyl linolenate, plant acetic acid, 56 kinds of compounds such as 3-hydroxyl-7 (isonitroso) cholanic acid, dihydroactinidiolide.
By relatively obtaining, supercritical CO
2no matter the fragrant pocket volatile ingredient that reveals of extraction gained is all high compared with steam distillation far away from smell, fragrant yield or the extraction efficiency of revealing pocket volatile ingredient yield, squalene, therefore can think supercritical CO
2extraction extracts the fragrant pocket volatility of revealing and is better than steam distillation.
Although illustrated and described embodiments of the invention, for the ordinary skill in the art, be appreciated that without departing from the principles and spirit of the present invention and can carry out multiple variation, amendment, replacement and modification to these embodiment, scope of the present invention is limited by claims and equivalent thereof.
Claims (7)
1. reveal pocket leaf and extract a fragrant method of revealing pocket volatile ingredient from perfume (or spice), it is characterized in that: the concrete steps of described method are as follows:
(1) perfume (or spice) is revealed to pocket cured leaf and pulverize 20-100 order, for subsequent use;
(2) perfume (or spice) after step (1) pulverizing is revealed to pocket leaf and put into supercritical CO
2in the extraction kettle of extraction equipment;
(3) tighten extraction kettle cover, and check separation kettle cover and whether have closing valve in closed condition;
(4) start power supply, connect cooling water, start refrigeration machine switch, and open the heater switch of extraction kettle, separating still I, separating still II and separating still III, and the temperature of setting extraction kettle is 35-55 DEG C, separating still I temperature is 35-50 DEG C, and separating still II temperature is 30-50 DEG C, and separating still III temperature is 30-50 DEG C;
(5) drop to 5-6 DEG C at refrigerator temps, and the temperature of extraction kettle, separating stills at different levels reaches the temperature of setting and when stable, open gas cylinder, air-source inflow valve, first discharge and catch up with the intrasystem air of extract and separate, in the time that extraction kettle pressure is consistent with sump pressure, start high-pressure pump, make extraction kettle pressure rise to gradually 15-27MPa;
(6) control valve of adjusting separating still, separating still I pressure is 9-18MPa, and separating still II pressure is 8-14MPa, and separating still III pressure is 4-8MPa, starts cycling extraction, CO
2flow is 20-40Kg/h, and extraction time is 30-120min;
(7) extraction cycle finishes, and collection material from separating still obtains the fragrant pocket volatile ingredient that reveals.
2. the method for claim 1, is characterized in that: in step (1), the fragrant pocket leaf that reveals is crushed to 60 orders.
3. the method for claim 1, is characterized in that: in step (3), the temperature of setting extraction kettle is 45 DEG C, and separating still I temperature is 45 DEG C, and separating still II temperature is 40 DEG C, and separating still III temperature is 40 DEG C.
4. the method for claim 1, is characterized in that: in step (5), extraction kettle pressure rises to 20MPa.
5. the method for claim 1, is characterized in that: in step (6), separating still I pressure is 12MPa, and separating still II pressure is 12MPa, and separating still III pressure is 6MPa.
6. the method for claim 1, is characterized in that: in step (6), and CO
2flow is 30Kg/h.
7. the method for claim 1, is characterized in that: in step (6), extraction time is 60min.
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