CN1806672A - Method for preparing zanthoxylum oil microcapsule by coupled supercritical extraction and atomized drying - Google Patents
Method for preparing zanthoxylum oil microcapsule by coupled supercritical extraction and atomized drying Download PDFInfo
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- CN1806672A CN1806672A CNA2005101117441A CN200510111744A CN1806672A CN 1806672 A CN1806672 A CN 1806672A CN A2005101117441 A CNA2005101117441 A CN A2005101117441A CN 200510111744 A CN200510111744 A CN 200510111744A CN 1806672 A CN1806672 A CN 1806672A
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- emulsion
- zanthoxylum oil
- spray
- extract
- chinese prickly
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 16
- 241000949456 Zanthoxylum Species 0.000 title claims abstract description 14
- 238000000194 supercritical-fluid extraction Methods 0.000 title claims abstract description 6
- 238000001035 drying Methods 0.000 title claims description 5
- 239000000839 emulsion Substances 0.000 claims abstract description 18
- 238000001694 spray drying Methods 0.000 claims abstract description 12
- 238000007592 spray painting technique Methods 0.000 claims abstract description 9
- 230000008878 coupling Effects 0.000 claims abstract description 5
- 238000010168 coupling process Methods 0.000 claims abstract description 5
- 238000005859 coupling reaction Methods 0.000 claims abstract description 5
- 244000089698 Zanthoxylum simulans Species 0.000 claims description 25
- 239000003995 emulsifying agent Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 244000215068 Acacia senegal Species 0.000 claims description 6
- 229920000084 Gum arabic Polymers 0.000 claims description 6
- 239000005913 Maltodextrin Substances 0.000 claims description 6
- 229920002774 Maltodextrin Polymers 0.000 claims description 6
- 239000000205 acacia gum Substances 0.000 claims description 6
- 235000010489 acacia gum Nutrition 0.000 claims description 6
- 229940035034 maltodextrin Drugs 0.000 claims description 6
- 238000004945 emulsification Methods 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 claims description 3
- 108010073771 Soybean Proteins Proteins 0.000 claims description 3
- 235000019710 soybean protein Nutrition 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 235000008496 Drimys aromatica Nutrition 0.000 abstract 1
- 240000008202 Schinus molle Species 0.000 abstract 1
- 235000005151 Schinus molle Nutrition 0.000 abstract 1
- 235000013880 Schinus terebinthifolius var. raddianus Nutrition 0.000 abstract 1
- 230000001804 emulsifying effect Effects 0.000 abstract 1
- 238000005507 spraying Methods 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 16
- 239000000341 volatile oil Substances 0.000 description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 238000000605 extraction Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000012530 fluid Substances 0.000 description 4
- 235000002566 Capsicum Nutrition 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 3
- 239000006002 Pepper Substances 0.000 description 3
- 241000722363 Piper Species 0.000 description 3
- 235000016761 Piper aduncum Nutrition 0.000 description 3
- 235000017804 Piper guineense Nutrition 0.000 description 3
- 235000008184 Piper nigrum Nutrition 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 241001093501 Rutaceae Species 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 241000282326 Felis catus Species 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- ZYGHJZDHTFUPRJ-UHFFFAOYSA-N benzo-alpha-pyrone Natural products C1=CC=C2OC(=O)C=CC2=C1 ZYGHJZDHTFUPRJ-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 235000001671 coumarin Nutrition 0.000 description 1
- 150000004775 coumarins Chemical class 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229960004488 linolenic acid Drugs 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 235000021264 seasoned food Nutrition 0.000 description 1
- 210000000697 sensory organ Anatomy 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention discloses a method of preparing zanthoxylum oil microcapsule with supercritical extraction and spray drying coupling, comprising the following steps: 1 putting the peppertree into extractor, extracting at the condition of CO2, 2 sending the extractant and emulsion into coaxial nozzle on the top of spray drying tower, at the export of coaxial nozzle, emulsifying the zanthoxylum oil in extractant and emulsion, then spraying, spray painting, drying and getting the zanthoxylum oil microcapsule. The invention has the advantages of simple operation, short preparing time, realizing the one-step preparing method, avoiding the problems of zanthoxylum oil oxidation and metamorphism in the course of middle treatment. The direct embed rate of zanthoxylum oil is up to 55%, and the zanthoxylum oil which is not embed can be reclaimed.
Description
Technical field
The present invention relates to wrap up the preparation method of the microcapsules of plant volatile oil, relate in particular to the preparation method of the microcapsules of Chinese prickly ash oil.
Background technology
Chinese prickly ash (Zanthoxylum Bungeanum Maxim), the annual herb plant that belongs to Rutaceae (rutaceae), be not only Chinese medicine commonly used, the consumption spices that liked by the common people, its resource distributes very wide in China, except all there is distribution the later each department in northeast and Xinjiang, is worth and is familiar with by people day by day.The chemical analysis of Chinese prickly ash mainly contains volatile oil, alkaloid, flavonoids, Coumarins, and wherein the volatile oil content height has important pharmacological action.
At present, still based on Chinese prickly ash seed or traditional Powdered, there are many shortcomings in the main type of service of Chinese prickly ash, and at first the cell tissue of Chinese prickly ash can not fully be destroyed, and effectively being the composition of distinguishing the flavor of like this in the Chinese prickly ash can not fully discharge, and causes waste; Secondly,, influence the sense organ form, food or dish quality are descended because coarse Chinese prickly ash particle is dispersed in unevenly by in the seasoned food or on the dish.
Supercritical CO
2Fluid extraction technology (SFE-CO
2) be to develop more a kind of high-new extraction and separation technology in recent ten years, compare with traditional extraction process, it is strong to have extracting power, the yield height, with short production cycle, active ingredient is not destroyed, and technology is simple, operating parameter is controlled easily, does not have dissolvent residual, advantages such as constant product quality.Volatile oil component molecules amount is less, has lipophilicity and lower boiling character, the fine solubility energy is arranged in supercritical carbon dioxide fluid, the all available pure carbon dioxide of great majority directly extraction obtains, required operating temperature is generally lower, avoided the destruction and the decomposition of active ingredient, and yield being also higher, is the composition that a class is suitable for supercritical carbon dioxide extracting most.
But, supercritical CO
2The pepper volatile oil that fluid extraction obtained also can't directly be used, and as it being adopted conventional method, preparation becomes microcapsules, owing to there is an intermediate link, must cause the loss of pepper volatile oil, the efficient of influence preparation.
How with supercritical CO
2The pepper volatile oil of fluid extraction is prepared into the microcapsules easy to use into people, be relevant department the problem very paid close attention to.
Summary of the invention
The technical issues that need to address of the present invention are to disclose the method that the coupling of a kind of means of supercritical extraction and spray-drying prepares zanthoxylum oil microcapsule, to overcome the above-mentioned defective that prior art exists, satisfy the needs of relevant department.
Method of the present invention comprises the steps:
(1) with CO
2Continuous feeding is equipped with the extractor of Chinese prickly ash, at CO
2Super critical condition under, extract preferred CO
2Super critical condition be: CO
2Temperature be 40～45 ℃, pressure is 150～250bar, CO
2Flow velocity in the extractor outlet is 1.5～2.5Lmin
-1, CO
2Flow be 900～1500L/kg Chinese prickly ash hour;
Said CO
2Super critical condition refer to, temperature is greater than 31 ℃, pressure is higher than 72bar;
(2) CO that extractor is exported
2Extract and emulsion are delivered to the coaxial nozzle that is arranged on the spray-drying top of tower, and in the outlet of coaxial nozzle, Chinese prickly ash in extract oil and emulsion emulsification spray then and descend spray painting drying, acquisition zanthoxylum oil microcapsule;
The CO that discharges
2Discharge from the spray-drying cat head, reclaim, reuse after the compression.
Said emulsion is the aqueous solution of gum arabic, maltodextrin and emulsifying agent, and wherein, the gum arabic weight content is 15～20%, and the maltodextrin weight content is 15～20%, and the emulsifying agent weight content is 0.2～0.4%.
Said emulsifying agent is selected from a kind of or its mixture in monoglyceride or the soybean protein isolate;
The volumetric usage of emulsion is 25～30 times of extract;
The linear velocity of the mixture of coaxial nozzle outlet is 0.8～1Lmin
-1
The spray painting baking temperature is 80～100 ℃.
Nozzle exit pressure is 0.15～0.25Mpa, and the atomization gas flow velocity is CO
2Exit velocity is 2～3Lmin
-1
Adopt said method, the direct embedding rate of Chinese prickly ash oil can reach more than 55%.
Embedding rate is an important indicator of weighing the microcapsules quality.Measuring method is as follows: the sample dissolution of products obtained therefrom is in deionized water, with the laggard promoting the circulation of qi analysis of hplc of Fructus Zanthoxyli oil esterification that discharges.The alpha-linolenic acid content that obtains discharging.
The characteristics that the present invention gives prominence to are with the microcapsules technology of preparing of advanced person's supercritical extraction technique and extensive use-spray drying technology coupling, easy and simple to handle, preparation time is short, the realization heat-sensitive material is finished from extracting one step of microcapsules preparation, the product that is obtained is suitable directly to eat or storage, has prevented oxidation, the spoilage problems of Chinese prickly ash oil intermediate treatment greatly.The direct embedding rate of Chinese prickly ash oil can reach more than 55%, and the Chinese prickly ash oil that does not obtain coating can reclaim handy, reduces the loss of natural plant volatile oil.
Description of drawings
Fig. 1 is the device schematic diagram.
Fig. 2 is the nozzle arrangements schematic diagram.
The specific embodiment
Fig. 2 is coaxial nozzle that following examples adopted, comprise outer tube 10, with coaxial being arranged on the interior pipe 11 in the outer tube 10 and the spout 12 of outer tube 10 ends be set of outer tube 10.
Embodiment 1
Adopt the device of Fig. 1 and the nozzle of Fig. 2.
100 gram Chinese prickly ashes are got the raw materials ready and are loaded in the extractor 1, at CO
2Temperature be 45 ℃, pressure is at 250bar, CO
2Exit velocity 2.5Lmin
-1, CO
2Flow be 150L/ hour, extract;
The extract and the emulsion of extractor 1 outlet are delivered to the coaxial nozzle 4 that is arranged on spray drying tower 3 tops by pump defeated 2, in the outlet of coaxial nozzle 4, Chinese prickly ash in extract oil and emulsion emulsification spray then and descend, the spray painting drying obtains zanthoxylum oil microcapsule;
In the said emulsion, the gum arabic weight content is 15%, maltodextrin 15%, monoglyceride 0.2%;
The volumetric usage of emulsion is 25 times of extract;
The linear velocity of the mixture of coaxial nozzle outlet is 0.8Lmin
-1
The spray painting baking temperature is 80 ℃.
The direct embedding rate of Chinese prickly ash oil is 55%.
Adopt the device of Fig. 1 and the nozzle of Fig. 2.
100 gram Chinese prickly ashes are got the raw materials ready and are loaded in the extractor 1, at CO
2Temperature be 40 ℃, pressure is at 150bar, CO
2Exit velocity 1.5Lmin
-1, CO
2Consumption be 90L/ hour, extract;
The extract and the emulsion of extractor 1 outlet are delivered to the coaxial nozzle 4 that is arranged on spray drying tower 3 tops by pump defeated 2, in the outlet of coaxial nozzle 4, Chinese prickly ash in extract oil and emulsion emulsification spray then and descend, the spray painting drying obtains zanthoxylum oil microcapsule;
In the said emulsion, the weight content of gum arabic is 17%, maltodextrin 17%, emulsifying agent 0.2%)
Said emulsifying agent is selected from soybean protein isolate;
The volumetric usage of emulsion is 27 times of extract;
The linear velocity of the mixture of coaxial nozzle outlet is 0.9Lmin
-1
The spray painting baking temperature is 80 ℃.
The direct embedding rate of Chinese prickly ash oil is 56.5%.
Claims (7)
1. the coupling of means of supercritical extraction and spray-drying prepares the method for zanthoxylum oil microcapsule, it is characterized in that, comprises the steps:
(1) with CO
2Continuous feeding is equipped with the extractor of Chinese prickly ash, at CO
2Super critical condition under, extract,
(2) extract and the emulsion of extractor outlet are delivered to the coaxial nozzle that is arranged on the spray-drying top of tower, in the outlet of coaxial nozzle, Chinese prickly ash oil and emulsion emulsification in the extract spray then and descend spray painting drying, acquisition zanthoxylum oil microcapsule.
2. method according to claim 1 is characterized in that CO
2Super critical condition be: CO
2Temperature be 40～45 ℃, pressure is 150～250bar, CO
2Flow velocity in the extractor outlet is 1.5～2.5Lmin
-1, CO
2Flow be 900～1500L/kg Chinese prickly ash hour.
3. method according to claim 1 is characterized in that, said emulsion is the aqueous solution of gum arabic, maltodextrin and emulsifying agent, wherein, the gum arabic weight content is 15～20%, and the maltodextrin weight content is 15～20%, and the emulsifying agent weight content is 0.2～0.4%.
4. method according to claim 3 is characterized in that, said emulsifying agent is selected from a kind of or its mixture in monoglyceride or the soybean protein isolate.
5. method according to claim 3 is characterized in that, the volumetric usage of emulsion is 25～30 times of extract.
6. method according to claim 3 is characterized in that, the linear velocity of the mixture of coaxial nozzle outlet is 0.8～1Lmin
-1
7. method according to claim 6 is characterized in that, the spray painting baking temperature is 80～100 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101117441A CN100402633C (en) | 2005-12-20 | 2005-12-20 | Method for preparing zanthoxylum oil microcapsule by coupled supercritical extraction and atomized drying |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101117441A CN100402633C (en) | 2005-12-20 | 2005-12-20 | Method for preparing zanthoxylum oil microcapsule by coupled supercritical extraction and atomized drying |
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| Publication Number | Publication Date |
|---|---|
| CN1806672A true CN1806672A (en) | 2006-07-26 |
| CN100402633C CN100402633C (en) | 2008-07-16 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005101117441A Active CN100402633C (en) | 2005-12-20 | 2005-12-20 | Method for preparing zanthoxylum oil microcapsule by coupled supercritical extraction and atomized drying |
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|---|---|
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100453628C (en) * | 2006-08-24 | 2009-01-21 | 保靖县武陵山花椒科技开发有限公司 | Linolenic oil and wild pepper seeds dregs, and prodn, method therefor |
| CN101606676B (en) * | 2009-07-13 | 2012-07-04 | 周大甫 | Production technology of fresh zanthoxylum oil |
| CN104026538A (en) * | 2014-05-19 | 2014-09-10 | 郑州雪麦龙食品香料有限公司 | Preparing method for high-purity sanshoamides |
| CN105831687A (en) * | 2016-03-29 | 2016-08-10 | 苏州美嘉汇食品科技有限公司 | Chilli particle and chilli oil employing the chilli particle |
| CN109007954A (en) * | 2018-09-11 | 2018-12-18 | 鹰潭华宝香精有限公司 | A kind of method of supercritical fluid preparation tobacco extractive microcapsule |
| CN109430428A (en) * | 2018-10-23 | 2019-03-08 | 东北农业大学 | A kind of preparation method of structured lipid OPO nanoemulsions |
| WO2021255943A1 (en) * | 2020-06-15 | 2021-12-23 | 山本 芳栄 | Method for stabilizing sanshools |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1212079C (en) * | 2003-08-20 | 2005-07-27 | 大连理工大学 | Method for producing condiment seasoning oil resin micro capsule |
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2005
- 2005-12-20 CN CNB2005101117441A patent/CN100402633C/en active Active
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100453628C (en) * | 2006-08-24 | 2009-01-21 | 保靖县武陵山花椒科技开发有限公司 | Linolenic oil and wild pepper seeds dregs, and prodn, method therefor |
| CN101606676B (en) * | 2009-07-13 | 2012-07-04 | 周大甫 | Production technology of fresh zanthoxylum oil |
| CN104026538A (en) * | 2014-05-19 | 2014-09-10 | 郑州雪麦龙食品香料有限公司 | Preparing method for high-purity sanshoamides |
| CN104026538B (en) * | 2014-05-19 | 2016-02-24 | 郑州雪麦龙食品香料有限公司 | A kind of preparation method of high-purity numb-taste component of zanthoxylum |
| CN105831687A (en) * | 2016-03-29 | 2016-08-10 | 苏州美嘉汇食品科技有限公司 | Chilli particle and chilli oil employing the chilli particle |
| CN105831687B (en) * | 2016-03-29 | 2018-11-09 | 苏州美嘉汇食品科技有限公司 | Capsicum particle and the chilli oil for using the capsicum particle |
| CN109007954A (en) * | 2018-09-11 | 2018-12-18 | 鹰潭华宝香精有限公司 | A kind of method of supercritical fluid preparation tobacco extractive microcapsule |
| CN109430428A (en) * | 2018-10-23 | 2019-03-08 | 东北农业大学 | A kind of preparation method of structured lipid OPO nanoemulsions |
| WO2021255943A1 (en) * | 2020-06-15 | 2021-12-23 | 山本 芳栄 | Method for stabilizing sanshools |
| EP4166535A4 (en) * | 2020-06-15 | 2024-03-13 | Yamamoto, Yoshie | Method for stabilizing sanshools |
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| Publication number | Publication date |
|---|---|
| CN100402633C (en) | 2008-07-16 |
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