CN113142314A - Zanthoxylum oil cake meal resin microcapsule and preparation method thereof - Google Patents
Zanthoxylum oil cake meal resin microcapsule and preparation method thereof Download PDFInfo
- Publication number
- CN113142314A CN113142314A CN202110244823.9A CN202110244823A CN113142314A CN 113142314 A CN113142314 A CN 113142314A CN 202110244823 A CN202110244823 A CN 202110244823A CN 113142314 A CN113142314 A CN 113142314A
- Authority
- CN
- China
- Prior art keywords
- oil cake
- resin
- zanthoxylum
- ultrasonic
- pepper
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000011347 resin Substances 0.000 title claims abstract description 133
- 229920005989 resin Polymers 0.000 title claims abstract description 133
- 241000949456 Zanthoxylum Species 0.000 title claims abstract description 109
- 239000003094 microcapsule Substances 0.000 title claims abstract description 89
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 235000012054 meals Nutrition 0.000 title claims abstract description 20
- 235000002566 Capsicum Nutrition 0.000 claims abstract description 99
- 239000006002 Pepper Substances 0.000 claims abstract description 99
- 241000722363 Piper Species 0.000 claims abstract description 99
- 235000016761 Piper aduncum Nutrition 0.000 claims abstract description 99
- 235000017804 Piper guineense Nutrition 0.000 claims abstract description 99
- 235000008184 Piper nigrum Nutrition 0.000 claims abstract description 99
- 238000000034 method Methods 0.000 claims abstract description 56
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 29
- 239000001116 FEMA 4028 Substances 0.000 claims abstract description 27
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims abstract description 27
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims abstract description 27
- 229960004853 betadex Drugs 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 24
- 239000006227 byproduct Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 238000012545 processing Methods 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 37
- 244000089698 Zanthoxylum simulans Species 0.000 claims description 19
- 239000000126 substance Substances 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 15
- 238000002386 leaching Methods 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 13
- 239000011162 core material Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 239000000284 extract Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000004108 freeze drying Methods 0.000 claims description 7
- 238000002137 ultrasound extraction Methods 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 13
- 239000002245 particle Substances 0.000 abstract description 12
- 239000008601 oleoresin Substances 0.000 abstract description 11
- 230000008901 benefit Effects 0.000 abstract description 6
- 238000000605 extraction Methods 0.000 abstract description 5
- 238000004064 recycling Methods 0.000 abstract description 5
- 238000000638 solvent extraction Methods 0.000 abstract description 4
- 238000011112 process operation Methods 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 164
- 235000019198 oils Nutrition 0.000 description 164
- 239000000047 product Substances 0.000 description 14
- 238000012360 testing method Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 230000008569 process Effects 0.000 description 9
- 235000007650 Aralia spinosa Nutrition 0.000 description 7
- 238000009826 distribution Methods 0.000 description 7
- 238000001694 spray drying Methods 0.000 description 6
- 235000015112 vegetable and seed oil Nutrition 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 230000004044 response Effects 0.000 description 5
- 230000001953 sensory effect Effects 0.000 description 5
- 238000009210 therapy by ultrasound Methods 0.000 description 5
- 235000019658 bitter taste Nutrition 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 206010002091 Anaesthesia Diseases 0.000 description 3
- 244000000231 Sesamum indicum Species 0.000 description 3
- 235000003434 Sesamum indicum Nutrition 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 description 3
- 230000037005 anaesthesia Effects 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 238000005457 optimization Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000008213 purified water Substances 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 238000005211 surface analysis Methods 0.000 description 3
- 239000005913 Maltodextrin Substances 0.000 description 2
- 229920002774 Maltodextrin Polymers 0.000 description 2
- 235000019484 Rapeseed oil Nutrition 0.000 description 2
- 235000010489 acacia gum Nutrition 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 150000001408 amides Chemical class 0.000 description 2
- 238000000540 analysis of variance Methods 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 239000000796 flavoring agent Substances 0.000 description 2
- 235000019634 flavors Nutrition 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 239000010647 garlic oil Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- CDOSHBSSFJOMGT-UHFFFAOYSA-N linalool Chemical compound CC(C)=CCCC(C)(O)C=C CDOSHBSSFJOMGT-UHFFFAOYSA-N 0.000 description 2
- UWKAYLJWKGQEPM-LBPRGKRZSA-N linalyl acetate Chemical compound CC(C)=CCC[C@](C)(C=C)OC(C)=O UWKAYLJWKGQEPM-LBPRGKRZSA-N 0.000 description 2
- 229940035034 maltodextrin Drugs 0.000 description 2
- 230000000873 masking effect Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 description 2
- 235000019640 taste Nutrition 0.000 description 2
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 2
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 2
- 239000001490 (3R)-3,7-dimethylocta-1,6-dien-3-ol Substances 0.000 description 1
- CDOSHBSSFJOMGT-JTQLQIEISA-N (R)-linalool Natural products CC(C)=CCC[C@@](C)(O)C=C CDOSHBSSFJOMGT-JTQLQIEISA-N 0.000 description 1
- 244000215068 Acacia senegal Species 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 description 1
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229920001661 Chitosan Polymers 0.000 description 1
- 229920000084 Gum arabic Polymers 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 241001093501 Rutaceae Species 0.000 description 1
- 108010073771 Soybean Proteins Proteins 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 241000032846 Zanthoxylum bungeanum Species 0.000 description 1
- 239000000205 acacia gum Substances 0.000 description 1
- 239000001785 acacia senegal l. willd gum Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 235000009120 camo Nutrition 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 239000000679 carrageenan Substances 0.000 description 1
- 235000010418 carrageenan Nutrition 0.000 description 1
- 229920001525 carrageenan Polymers 0.000 description 1
- 229940113118 carrageenan Drugs 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 235000005607 chanvre indien Nutrition 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000011487 hemp Substances 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229930007744 linalool Natural products 0.000 description 1
- UWKAYLJWKGQEPM-UHFFFAOYSA-N linalool acetate Natural products CC(C)=CCCC(C)(C=C)OC(C)=O UWKAYLJWKGQEPM-UHFFFAOYSA-N 0.000 description 1
- 238000013178 mathematical model Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000862 numbness Toxicity 0.000 description 1
- 238000003921 particle size analysis Methods 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 235000019710 soybean protein Nutrition 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 1
Images
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
- A23D9/04—Working-up
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
- A23P10/30—Encapsulation of particles, e.g. foodstuff additives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09F—NATURAL RESINS; FRENCH POLISH; DRYING-OILS; OIL DRYING AGENTS, i.e. SICCATIVES; TURPENTINE
- C09F1/00—Obtaining purification, or chemical modification of natural resins, e.g. oleo-resins
- C09F1/02—Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention provides a pepper oil cake pulp resin microcapsule and a preparation method thereof, wherein pepper oil cake pulp raw materials are prepared into pepper oil cake pulp resin and the pepper oil cake pulp resin is microencapsulated. The method utilizes the raw material as a processing byproduct after hot oil extraction and squeezing production of zanthoxylum oil, namely zanthoxylum oil cake meal, and mainly comprises the following steps: crushing the cake, extracting residual zanthoxylum oleoresin in the cake by an ultrasonic-assisted solvent extraction method, and microencapsulating the obtained resin by an ultrasonic-assisted molecular embedding method by taking beta-cyclodextrin as a wall material. The prepared pepper oil cake resin microcapsule has uniform particle size, is spherical and ellipsoidal, has smooth and continuous surface, reduces the contact area with the outside, and improves the thermal stability. The invention provides a new method for recycling cake resources which are byproducts in the production of pepper oil, and the method has the advantages of simple process operation and good microencapsulation effect.
Description
Technical Field
The invention belongs to the technical field of recycling of byproducts generated after production of zanthoxylum oil, and particularly relates to a zanthoxylum oil cake meal resin microcapsule and a preparation method thereof.
Background
Zanthoxylum bungeanum (Zanthoxylum bungeanum Maxim.) is the mature pericarp of Zanthoxylum bungeanum of Rutaceae, and is known as one of eight major flavors. The pepper is used as an important economic crop and is widely planted in China, and the planting area and the yield are the top of the world. The zanthoxylum oil is used as a main processing product of zanthoxylum, and a byproduct, namely zanthoxylum oil cake (or called cake residue and waste residue), is generated in the production process. Researches show that a large amount of usable substances such as numb-taste substances, polysaccharides, proteins, grease, cellulose and the like still remain in the zanthoxylum oil cake, but the by-products are not fully utilized for a long time, even environmental pollution is caused, and the by-products become burdens of zanthoxylum oil production enterprises. How to effectively extract the main substance, namely the numb-taste substance, remained in the pepper oil cake meal and further process the extracted substance into a pepper deep-processed product, and the improvement of the pepper deep-processing level and the enterprise economic benefit becomes a big problem to be solved.
In order to improve the economic value of the zanthoxylum bungeanum and enrich the category of the zanthoxylum bungeanum fine and deep processing products, in recent years, the deep processing technology of the zanthoxylum bungeanum gradually rises, and the zanthoxylum oil resin is a multi-component mixed extract which is prepared by adopting a solvent extraction method and has the numb taste and the fragrance of the zanthoxylum bungeanum, and has the advantages of standardization and consistent flavor. However, the zanthoxylum oil resin is inconvenient to use in a water-soluble environment as a fat-soluble product. Thus, chinese patent document CN 104381953a discloses a process capable of mass production of water-soluble zanthoxylum oil resin. The inventor of the patent also researches and extracts the pepper oil cake resin from the pepper oil cake, and the pepper oil cake resin extracted by the optimal process has higher tingling degree, stronger bitter taste and unstable under the environment with higher temperature, oxygen, illumination and humidity, so that the application of the pepper oil cake resin is limited and the economic value of the byproduct of the pepper oil cake cannot be fully improved. Therefore, the problems of stable storage and convenient use of the zanthoxylum oil cake resin are urgently needed to be solved.
Microencapsulation is a commonly used encapsulation technique to protect labile sensitive compounds from environmental elements and to mask the unpleasant odor of the core material. Chinese patent document CN 107041549a discloses a method for preparing garlic oil microcapsule powder, which can store garlic oil at normal temperature after microencapsulation treatment, and has prolonged storage time and better storage effect. Chinese patent document CN 109907123 a discloses a method for preparing zanthoxylum oil resin microcapsules by using gum arabic and chitosan as wall materials and adopting a spray drying method, the microcapsules prepared by the method are spherical, have good fluidity, and reduce the chance of contacting with the outside, but the above patent methods have the following disadvantages: the inlet temperature during spray drying is as high as 180 ℃, and the loss of heat-sensitive Zanthoxylum amide substances and volatile Zanthoxylum aroma components is huge. Chinese patent document CN 104757531a discloses a microcapsule of zanthoxylum seed oil and a preparation method thereof, the microcapsule is composed of a core material and a wall material, the wall material is a mixture of arabic gum and maltodextrin, and the core material is zanthoxylum seed oil; the microcapsule is prepared by heating wall material, dissolving in water to obtain emulsion, mixing the emulsion with heated core material, homogenizing, and spray drying. The air inlet temperature is required to be strictly controlled to be 170-190 ℃ and the air outlet temperature is required to be 80-90 ℃ during spray drying, although the method obtains good embedding rate for the zanthoxylum seed oil, the method is still difficult to apply to the zanthoxylum oil cake, so that the components in the zanthoxylum oil cake are unstable, and the amide substances and volatile zanthoxylum aroma components are easy to lose.
Compared with a spray drying method, the molecular embedding method is a microencapsulation method which is generated on a molecular level, and mainly utilizes the structural characteristics of beta-cyclodextrin that the beta-cyclodextrin is hollow, hydrophobic inside and hydrophilic outside, hydrophobic core materials can be selectively combined in an aqueous solution, and some core materials with proper size and shape are embedded in a ring structure by virtue of Van der Waals force to form a stable inclusion complex. However, although the preparation of the microcapsule by the molecular embedding method is simple and easy, the direct embedding rate of the zanthoxylum seed oil is low. For example, in the Xuhuaide et al, published in the study on the preparation of unsaturated fatty acid beta-cyclodextrin inclusion compound of Zanthoxylum bungeanum seed oil, the inclusion of unsaturated fatty acid of Zanthoxylum bungeanum seed oil is studied by molecular embedding method, and the embedding rate after optimization is only 47.3%. The results show that the beta-cyclodextrin as the wall material is not fully utilized by the simple microencapsulation by the molecular embedding method. Beta-cyclodextrin is used as the most commonly used food additive and auxiliary agent, has low cost and wide application range, can be used as an ideal embedding wall material of a fat-soluble core material, and needs to optimize an embedding mode and conditions to improve the embedding rate.
Because the prickly ash oil cake pulp resin has the problem of instability in the environment with high temperature, oxygen, illumination and humidity, unstable substances in prickly ash oil cake pulp are easy to go bad, the bitter taste of the prickly ash oil cake pulp resin is strong, the stability of the spicy substances is poor, the effect of the existing process for embedding prickly ash oil resin on the prickly ash oil cake pulp resin is poor, the embedding rate of microencapsulation is only less than 50%, and therefore, methods for preparing prickly ash oil cake pulp resin and microencapsulating by adopting prickly ash oil cake are not seen, and the field is urgent to be developed and researched.
Therefore, how to use cyclodextrin as a wall material and combine a molecular embedding method to develop a microencapsulation technology for improving the embedding effect of the zanthoxylum oil cake, and how to develop a deep processing product for recycling the zanthoxylum oil cake become technical problems to be solved by the invention.
Disclosure of Invention
The invention aims to solve the technical problems and provides a pepper oil cake dreg resin microcapsule and a preparation method thereof. The method provided by the invention is used for embedding the zanthoxylum oil cake resin extracted from the zanthoxylum oil cake by using an ultrasonic-assisted molecular embedding method, masking the bitter taste of the zanthoxylum oil cake resin, enhancing the stability of the numb taste and improving the embedding rate of microencapsulation, and by-product zanthoxylum oil cake in the zanthoxylum oil production process is used as a raw material to obtain a zanthoxylum oil deep-processed product, thereby well achieving the purpose of recycling the zanthoxylum oil processing by-product.
One of the purposes of the invention is to provide a preparation method of a pepper oil cake resin microcapsule, which comprises the steps of preparing a pepper oil cake raw material into pepper oil cake resin and microencapsulating the pepper oil cake resin; wherein the content of the first and second substances,
the preparation method of the zanthoxylum oil cake resin comprises the following steps:
(1) selecting a pepper oil cake raw material, drying, crushing and sieving;
(2) ethanol leaching: adding an ethanol solution into the pepper oil cake crushed in the step (1) for leaching;
(3) ultrasonic extraction: performing ultrasonic-assisted extraction on the extract obtained in the step (2), wherein the ultrasonic temperature is 30 ℃, the ultrasonic time is 30min, the ultrasonic power is 180W, filtering the extract, and distilling the filtrate under reduced pressure to remove ethanol to obtain the zanthoxylum oil cake resin;
the microencapsulation of the zanthoxylum oil cake resin comprises the following steps:
s1: dissolving wall materials and core materials: dissolving beta-cyclodextrin in hot water at 40 ℃ according to the proportion of 1:3g/mL, stirring for 10min, preparing into uniform slurry, slowly adding pepper oil cake resin, wherein the mass ratio of the pepper oil cake resin to the beta-cyclodextrin is 1:3-4g/g, and uniformly stirring to obtain O/W type mixed solution;
s2: ultrasonic: putting the O/W type mixed solution of the wall material and the core material obtained in the step S1 into an ultrasonic environment for ultrasonic-assisted embedding, wherein the conditions of the ultrasonic-assisted embedding are as follows: the ultrasonic temperature is 35-40 ℃, the ultrasonic time is 5-15min, and the ultrasonic power is 180-;
s3: embedding: embedding the prepared O/W type mixed solution under magnetic stirring;
s4: and centrifuging the O/W type mixed solution, freeze-drying the obtained precipitate, and grinding to obtain the zanthoxylum oil cake resin microcapsule.
The raw material utilized by the method is a processing byproduct, namely the pepper oil cake meal, after hot oil extraction and squeezing production of pepper oil, the pepper oil cake meal is crushed, residual pepper oleoresin in the cake meal is extracted by an ultrasonic-assisted solvent extraction method, and the obtained resin is microencapsulated by an ultrasonic-assisted molecular embedding method with beta-cyclodextrin as a wall material. The prepared pepper oil cake resin microcapsule has uniform particle size, is spherical and ellipsoidal, has smooth and continuous surface, reduces the contact area with the outside, and improves the thermal stability. The invention provides a new method for recycling cake resources which are byproducts in the production of pepper oil, and the method has the advantages of simple process operation and good microencapsulation effect.
Further, the zanthoxylum oil cake in the step (1) is a processing by-product after the zanthoxylum oil is produced by leaching and pressing with hot oil.
Further, the crushing in the step (1) is carried out by adopting a high-speed universal crusher, and the sieving is carried out by sieving with an 80-mesh sieve.
Further, the volume concentration of the ethanol solution added in the step (2) is 50%, and the mass-volume ratio of the pepper oil cake and the ethanol solution is 1:12 g/mL.
Further, the ethanol solution in the step (2) is leached for 20 min.
Further, the conditions of the ultrasound-assisted embedding in step S2 are as follows: the ultrasonic temperature is 35 ℃, the ultrasonic time is 10min, and the ultrasonic power is 240W.
Further, the temperature for embedding under magnetic stirring in step S3 was 35 ℃ and the embedding time was 90 min.
Further, the conditions of the centrifugation in step S4 are: the rotation speed is 6000rpm, and the centrifugation time is 12 min.
Further, the freeze-drying time in step S4 was 48 hours.
The invention also aims to provide a pepper oil cake resin microcapsule which is prepared by the method.
Compared with the prior art, the invention has the technical progress that:
1. at present, no report about the reuse of the resin of the pepper oil cake extracted from the pepper oil cake is found, and the invention provides a new scheme for the reuse of pepper oil cake resources.
2. The invention solves the problem that the pepper oil cake pulp resin is unstable in the environment with high temperature, oxygen, illumination and humidity, adopts beta-cyclodextrin as a wall material, and microencapsulates the pepper oil cake pulp resin by using an ultrasonic-assisted molecular embedding method, thereby greatly improving the adverse phenomenon of the pepper oil cake pulp resin in the using process.
3. Compared with the common spray drying method for preparing the microcapsule, the invention has mild conditions during the preparation of the microcapsule, is more beneficial to preventing the unstable substances from deteriorating, and has simple preparation process and low equipment requirement. In addition, compared with the zanthoxylum oil cake resin microcapsule obtained without ultrasonic treatment, the zanthoxylum oil cake resin microcapsule obtained by ultrasonic-assisted embedding has the advantages that the embedding rate is remarkably improved, and the embedding efficiency is close to or even exceeds the embedding rate of the zanthoxylum oil cake resin microcapsule obtained by directly extracting zanthoxylum peel. The masking effect on the bitterness of the pepper oil cake pulp resin is better, the tingling degree of the obtained microcapsule product is not much different from the tingling degree of pepper blended oil sold in the market, and the microcapsule product has the condition of serving as a novel tingling seasoning product.
4. The particle size distribution of the prepared zanthoxylum oil cake resin microcapsule after process optimization is uniform, the microcapsule is spherical and ellipsoidal, the surface is smooth and continuous, the cracks are few, and the embedding effect is proved to be ideal. And the microcapsule is protected by wall materials, so that the thermal stability of the microcapsule is better than that of the pepper oil cake resin. The synthesis of the above description shows that the pepper oil cake resin microcapsule prepared by the method has better application prospect.
Drawings
Fig. 1 is a particle size distribution diagram of the pepper oil cake resin microcapsule provided by the invention.
FIG. 2 is a microscope image and a scanning electron microscope image of a pepper oil cake resin microcapsule provided by the invention; wherein: a is a microscope picture of the pepper oil cake resin microcapsule; and b is an electron microscope image of the zanthoxylum oil cake resin microcapsule under the condition of 5000 times.
FIG. 3 is a differential scanning calorimetry curve diagram of a pepper oil cake resin microcapsule provided by the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the present invention is described in detail below with reference to the following embodiments, and it should be noted that the following embodiments are only for explaining and illustrating the present invention and are not intended to limit the present invention. The invention is not limited to the embodiments described above, but rather, may be modified within the scope of the invention.
Example 1
The preparation method comprises the following steps of (A) preparing raw materials of pepper oil cake pulp, wherein the preparation operation steps of pepper oil cake pulp resin are as follows:
firstly, crushing dried pepper oil cake meal by using a high-speed universal crusher, screening by using a stainless steel mesh screen of 80 meshes, adding 600mL of ethanol with the volume concentration of 50% into 50g of the crushed and screened pepper oil cake meal, and leaching for 20 min; then putting the zanthoxylum oil cake meal and the leaching solution into an environment with the ultrasonic temperature of 30 ℃ and the ultrasonic power of 180W for ultrasonic treatment for 30 min; after the ultrasonic-assisted extraction is finished, filtering the extract for later use; and distilling the filtrate under reduced pressure until no ethanol exists, thus obtaining the zanthoxylum oil cake resin.
The microencapsulation of the (II) zanthoxylum oil cake resin comprises the following steps:
A. dissolving wall material beta-cyclodextrin in purified water at 40 ℃ according to the proportion of 1:3g/mL, stirring for 10min, preparing into uniform slurry, slowly adding pepper oil cake resin with the wall material proportion of 1:4g/g, and uniformly stirring by a magnetic stirrer to form O/W type mixed solution;
B. placing the O/W mixed solution into an environment with the ultrasonic temperature of 35 ℃ and the ultrasonic power of 200W for auxiliary embedding for 15 min; after the ultrasound is finished, the magnetic stirring embedding is carried out for 90min at the temperature of 35 ℃;
C. centrifuging the microcapsule mixed solution at 6000rpm for 12min to obtain precipitate, freeze drying for 48 hr, and grinding to obtain fructus Zanthoxyli oil cake resin microcapsule.
Test example 1
The components and contents of the zanthoxylum oil cake resin prepared in example 1 were measured, the degree of hemp of the zanthoxylum oil cake resin prepared under the conditions was 115.10, and the obtained zanthoxylum oil cake resin was subjected to GC-MS analysis. A search was performed using NIST.11 standard database, 53 chromatographic peaks were detected in total, and fractions having a degree of matching of not less than 80% were selected (Table 1). From table 1, a total of 12 compounds were identified, including 7 esters and 1 phenol, and others were alkanes. The research at present shows that the types of the aroma components of the pepper are as many as 120, and the pepper mainly contains hydrocarbon, ester, alcohol and other substances, but the aroma components in the pepper resin extracted under the optimal condition are not only few in types, but also not high in content, such as linalyl acetate (0.5017%). This is because the hot oil extraction of zanthoxylum oil in the early stage causes more volatilization of the peculiar aroma substances of zanthoxylum, so the later stage microencapsulation emphasizes the optimization of the degree of anesthesia.
TABLE 1 major components of Zanthoxylum bungeanum oil cake resin and their relative percentages
The characterization test of the zanthoxylum oil cake resin microcapsules prepared in example 1 shows that the embedding rate of the obtained zanthoxylum oil cake resin microcapsules is 81.94%, the anesthesia degree is 6.74, the sensory evaluation is 81.33 minutes, and the yield is 79.56%. The embedding rate of the pepper oil cake resin microcapsule prepared by the invention is higher in the same determination method, and the difference between the sesame degree and the sesame degree of pepper blend oil sold in the market is not great.
Comparative example 1
Comparative example 1 is a comparative experiment of example 1, and comparative example 1 zanthoxylum oleoresin microcapsules were prepared using zanthoxylum oleoresin extracted from zanthoxylum bungeanum.
(1) The raw material is pepper peel, and the preparation operation steps of the pepper oleoresin are as follows:
firstly, crushing dried pepper by using a high-speed universal crusher, screening the crushed pepper by using a stainless steel mesh screen of 80 meshes, adding 600mL of 50 volume concentration ethanol into 50g of crushed and screened pepper powder, and leaching for 20 min; then putting the pepper powder and the leaching liquor into an environment with the ultrasonic temperature of 30 ℃ and the ultrasonic power of 180W for ultrasonic treatment for 30 min; after the ultrasonic-assisted extraction is finished, filtering the extract for later use; distilling the filtrate under reduced pressure until no ethanol exists, and obtaining the zanthoxylum oil resin.
(2) The microencapsulation of the zanthoxylum oil resin comprises the following steps:
A. dissolving wall material beta-cyclodextrin in purified water at 40 ℃ according to the proportion of 1:3g/mL, stirring for 10min, preparing into uniform slurry, slowly adding pepper oleoresin with the wall material proportion of 1:4g/g, uniformly stirring by a magnetic stirrer to form O/W type mixed solution, and then continuing to magnetically stir and embed for 90min at 35 ℃;
B. centrifuging the microcapsule mixed solution for 12min under 6000rmp, freeze drying the obtained precipitate for 48h, and grinding to obtain oleum Zanthoxyli Bungeani microcapsule.
The tingling degree of the pepper oleoresin is 343.85 through testing, and GC-MS analysis is carried out on the pepper oleoresin. The components were selected to have a degree of matching of not less than 80% by searching through NIST.11 standard database, detecting 43 chromatographic peaks in total (Table 2). From table 2, 12 compounds were identified, including 4 alkenes and 3 alcohols, and the rest being ketones, esters and alkanes, wherein the linalool content was 1.9569%. The GC-MS analysis of the zanthoxylum oil resin in the Zanthoxylum oil resin microcapsule product preparation technology and process research of Zhengxingyi shows that: 51 chemical components are detected from the zanthoxylum oil resin, 47 compounds with the matching degree of more than 80 percent are identified, wherein 29 types of alkenes, 12 types of alcohols, 6 types of esters and the balance of ketone, aldehyde, alkane and the like. Compared with the research, the extracted zanthoxylum oil resin has insufficient aroma components. The raw materials used in the invention are residual byproducts after the zanthoxylum oil is extracted and prepared, wherein the aroma components and the numb components are greatly reduced, but the zanthoxylum oleoresin still has more residual chemical components and certain utilization space, and the numb degree of the zanthoxylum oleoresin after microencapsulation is better.
TABLE 2 Zanthoxylum oil resin extracted from Zanthoxylum bungeanum husk and its relative percentage content
As can be seen from the comparison between example 1 and comparative example 1, the degree of numbness of the Zanthoxylum bungeanum oil cake resin is lower than that of Zanthoxylum bungeanum oil resin, and there is a great difference in the content and kind of aroma components. The reason is that most of the fragrance components of the zanthoxylum oil are extracted and lost after the zanthoxylum oil cake is subjected to the processes of hot extraction, centrifugation, squeezing and the like in the production of the zanthoxylum oil. In addition, through the extraction of the rapeseed oil, the resin aroma of the pepper oil cake also presents the components of rapeseed oil fatty acid.
The embedding rate of the pepper oleoresin microcapsules is 82.57%, the tingling degree is 13.26, the sensory evaluation is 89.79 minutes, and the yield is 78.16%. The result shows that the tingling degree of the pepper oil cake resin microcapsules is lower than that of the pepper oil resin microcapsules, which is expected, but when the pepper oil cake resin microcapsules are used as microcapsule products, the tingling degree of the pepper oil resin microcapsules can be achieved by increasing the using amount of the pepper oil cake resin microcapsules, the sensory evaluation is also improved, and meanwhile, the product cost is obviously lower than that of the pepper oil resin microcapsule products prepared by pepper shells. The difference between the two microcapsules is not great in embedding rate and yield, which indicates that the method is also feasible for preparing the zanthoxylum oil resin microcapsules.
The best zanthoxylum oil resin microcapsule preparation process screened by Zhengxingyi is that the soybean protein isolate, maltodextrin and carrageenan are 1:4:0.1, the core-wall ratio is 1:5, and the embedding rate of the microcapsule is 75.35%, which shows that the zanthoxylum oil resin microcapsule prepared by the invention has better embedding effect.
Comparative example 2
Comparative example 2 is another comparative experiment of example 1 and comparative example 2 is a zanthoxylum oil cake resin microcapsule prepared without sonication.
(1) The raw material is pepper oil cake meal, and the preparation operation steps of the pepper oil cake meal resin are as follows:
firstly, crushing dried pepper oil cake meal by using a high-speed universal crusher, screening by using a stainless steel mesh screen of 80 meshes, adding 600mL of ethanol with the volume concentration of 50% into 50g of the crushed and screened pepper oil cake meal, and leaching for 20 min; then putting the zanthoxylum oil cake meal and the leaching solution into an environment with the ultrasonic temperature of 30 ℃ and the ultrasonic power of 180W for ultrasonic treatment for 30min, and filtering the leaching solution for later use after the ultrasonic-assisted leaching is finished; and distilling the filtrate under reduced pressure until no ethanol exists, thus obtaining the zanthoxylum oil cake resin.
(2) The microencapsulation of the zanthoxylum oil cake resin comprises the following steps:
A. dissolving wall material beta-cyclodextrin in purified water at 40 ℃ according to the proportion of 1:3g/mL, stirring for 10min, preparing into uniform slurry, slowly adding pepper oil cake resin with the wall material proportion of 1:4g/g, uniformly stirring by a magnetic stirrer to form O/W type mixed solution, and then continuing to magnetically stir and embed for 90min at 35 ℃;
B. centrifuging the microcapsule mixed solution for 12min under 6000rmp, freeze drying the obtained precipitate for 48h, and grinding to obtain the resin microcapsule of fructus Zanthoxyli oil cake.
The embedding rate of the pepper oil cake resin microcapsules under the condition is 57.10%, the sesame degree is 4.32, the sensory evaluation is 68 minutes, and the yield is 69.66%. The results show that the embedding rate, the anesthesia degree, the sensory evaluation and the yield of the zanthoxylum oil cake resin microcapsule which is not embedded with the assistance of ultrasound are all lower than those of the zanthoxylum oil cake resin microcapsule obtained after the ultrasound treatment. One reason is that the embedding effect is not good when beta-cyclodextrin is simply used as a wall material for microencapsulation; because the zanthoxylum oil cake meal resin is obtained by ultrasonic-assisted solvent extraction, the zanthoxylum oil cake meal resin is directly dissolved in a beta-cyclodextrin solution and is difficult to directly enter a cavity of the beta-cyclodextrin, and more of the zanthoxylum oil cake meal resin is adsorbed on the surface of the cyclodextrin. Therefore, the ultrasonic-assisted molecular embedding method adopted by the invention is feasible for improving the embedding effect of the zanthoxylum oil cake resin microcapsules.
Comparative example 3
Comparative example 3 is another comparative experiment of example 1, a Box-Behnken model test design was selected, response surface analysis was performed at a level of 3 factors 3 with the microcapsule embedding rate (Y) as a response value and the ultrasonic time (a), ultrasonic power (B), and core-wall ratio (C) as independent variables, and the range of values of the test factors is shown in table 3.
TABLE 3 response surface analysis factor and horizon
The procedure was the same as in example 1, and the results were as follows:
TABLE 4 response surface analysis test and results
And (3) adopting Design-Expert8.0.6 software to perform fitting analysis on the test data of the table 4, establishing a mathematical model, and obtaining an optimal test formula according to a model equation. The obtained multiple quadratic regression model equation for the embedding rate (Y) is:
Y＝79.70+2.85A+4.53B+6.04C+0.74AB-1.61AC-1.99BC-3.81A2-4.20B2-4.92C2
in the formula: y is the embedding rate in unit%; a is ultrasonic time in unit of min; b is ultrasonic power in W; c is the core-wall ratio in g/g.
Equation analysis is carried out on the regression model with the embedding rate as the target function, and the result of the significance test of the regression equation coefficient is shown in table 5.
TABLE 5 regression equation analysis of variance
As can be seen from Table 5, in the regression equation, the value of the model term P & gtF is less than 0.01, the difference is extremely obvious, the mismatching term 0.1003 is more than 0.05, and the difference is not obvious, which indicates that the established regression model is very obvious and can better fit the influence of the ultrasonic time, the ultrasonic power and the core-wall ratio on the embedding rate of the microcapsules. The regression coefficient R2 of the model is 0.9764, and the correction coefficient R2 of the model is 0.9460, which shows that the model has better fitting degree with an actual test and can be used for theoretical speculation of the embedding rate. Within the range of selected factor levels, the influence of each factor on the embedding rate is different, wherein the influence of the primary term A, B, C, the secondary terms A2, B2 and C2 on the test result is extremely obvious (P is less than 0.01), and the result is the same as that of the single factor significance analysis; the effect of the interaction term BC on the test results was significant (P < 0.05). From the analysis of variance results, the influence of 3 factors on the embedding rate is as follows: core-wall ratio (C) > ultrasonic power (B) > ultrasonic time (A).
The maximum response value, namely the maximum embedding rate, is obtained through further analysis and calculation of software, the corresponding optimal process conditions are that the ultrasonic time is 11.6min, the ultrasonic power is 267.34W, the core-wall ratio is 3.47g/g, and the theoretical embedding rate of the microcapsules under the conditions is 82.60%. In order to conveniently verify the feasibility of the method, the ultrasonic time is 11.6min, the ultrasonic power is 240W and the core-wall ratio is 1:3.47g/g under the adjustment values of the conditions. Three parallel experiments were carried out under these conditions to obtain an average embedding rate of 81.94% for the microcapsules, which is 0.80% different from the theoretical value. The result is similar to the theoretical value obtained by software analysis, and the test model is proved to be reliable in selection, so that the microencapsulation process is feasible.
Experimental results example 1
The results of analyzing the corresponding experimental data of example 1 of the present invention are as follows:
(1) analysis of particle size distribution of pepper oil cake resin microcapsules
The particle size is an important index for evaluating the application potential of the microcapsule, and as can be seen from fig. 1, the particle size distribution of the zanthoxylum oil cake resin microcapsule is normal distribution, has only one peak, has a narrow particle size distribution range from 0.88 μm to 11.02 μm, and shows that the particle size distribution of the zanthoxylum oil cake resin microcapsule is uniform. The smaller particle size is beneficial to human body digestion and absorption, and the average particle size of the optimized pepper oil cake resin microcapsule is 2.85 mu m, so the method is beneficial to human body digestion and absorption.
(2) Morphology observation of pepper oil cake resin microcapsules
The beta-cyclodextrin is generally in a flake shape or other irregular shapes, and most of microcapsules prepared by the beta-cyclodextrin are also in an irregular plate shape. As can be seen from figure 2a, the appearance of the zanthoxylum oil cake resin microcapsule is mostly similar to a sphere, and the particle size is relatively uniform, because the zanthoxylum oil cake resin enters a cavity structure of beta-cyclodextrin, the compactness of the beta-cyclodextrin is reduced. In addition, the capsule wall and the content of the microcapsule can be clearly distinguished, and the inner cavity is filled with the pepper oil cake resin, which shows that the prepared pepper oil cake resin microcapsule has a good embedding effect on the pepper oil cake resin.
From fig. 2b, it can be observed that the zanthoxylum oil cake resin microcapsule is spherical and ellipsoidal, the surface is smooth and continuous, the cracks are less, the embedding effect is proved to be ideal, and the embedding effect is consistent with the observation result of a microscope; the sizes are basically consistent and are about 2-4 mu m, and the sizes are consistent with the particle size analysis result. However, the microcapsules may be stuck together, and the microcapsules may be naturally pushed together along with the evaporation of water during the drying process. The surface of the microcapsule product has a certain degree of wall breaking phenomenon, because the structure of the surface wall material is changed due to unstable heating.
(3) Determination of thermal stability of pepper oil cake resin microcapsule
Fig. 3 is a differential scanning calorimetry curve of zanthoxylum oil cake resin, beta-cyclodextrin and zanthoxylum oil cake resin microcapsule, and it can be seen from the figure that the thermodynamic property of zanthoxylum oil cake resin changes to a certain extent after the zanthoxylum oil cake resin is embedded by the beta-cyclodextrin. The zanthoxylum oil cake pulp resin has two obvious endothermic peaks at 108 ℃ and 158 ℃, wherein 108 ℃ is an endothermic peak reflected by heat absorption when water is evaporated and volatile components of the zanthoxylum oil cake pulp resin volatilize, and 158 ℃ is a boiling point peak of the zanthoxylum oil cake pulp resin; beta-cyclodextrin has an endothermic peak with a boiling point at 153 ℃; the Zanthoxylum bungeanum oil cake resin microcapsule has an endothermic peak similar to beta-cyclodextrin at 144 ℃, and the endothermic peak moves rightwards relative to the first endothermic peak of Zanthoxylum bungeanum oil cake resin, which indicates that Zanthoxylum bungeanum oil cake resin is not only successfully embedded in beta-cyclodextrin, but also the microcapsule has better thermal stability than Zanthoxylum bungeanum oil cake resin because of the protection of wall material.
The invention relates to a preparation method of a pepper oil cake resin microcapsule, which is not only suitable for embedding pepper oil cake resin, but also suitable for embedding pepper oil resin and other fat-soluble core materials. The present invention is not limited to the above-mentioned examples, which only describe the combination conditions of partial microencapsulation of the present invention, and any simple modifications of the above examples, which are based on the technical basis of the present invention, are within the scope of the present invention.
Claims (10)
1. A preparation method of a pepper oil cake pulp resin microcapsule is characterized by comprising the steps of preparing a pepper oil cake pulp raw material into pepper oil cake pulp resin and microencapsulating the pepper oil cake pulp resin; wherein the content of the first and second substances,
the preparation method of the zanthoxylum oil cake resin comprises the following steps:
(1) selecting a pepper oil cake raw material, drying, crushing and sieving;
(2) ethanol leaching: adding an ethanol solution into the pepper oil cake dregs crushed and sieved in the step (1) for leaching;
(3) ultrasonic extraction: performing ultrasonic-assisted extraction on the extract obtained in the step (2), wherein the ultrasonic temperature is 30 ℃, the ultrasonic time is 30min, the ultrasonic power is 180W, filtering the extract, and distilling the filtrate under reduced pressure to remove ethanol to obtain the zanthoxylum oil cake resin;
the microencapsulation of the zanthoxylum oil cake resin comprises the following steps:
s1: dissolving wall materials and core materials: dissolving beta-cyclodextrin in hot water at 40 ℃ according to the proportion of 1:3g/mL, stirring for 10min, preparing into uniform slurry, slowly adding pepper oil cake resin, wherein the mass ratio of the pepper oil cake resin to the beta-cyclodextrin is 1:3-4g/g, and uniformly stirring to obtain O/W type mixed solution;
s2: ultrasonic: putting the O/W type mixed solution of the wall material and the core material obtained in the step S1 into an ultrasonic environment for ultrasonic-assisted embedding, wherein the conditions of the ultrasonic-assisted embedding are as follows: the ultrasonic temperature is 35-40 ℃, the ultrasonic time is 5-15min, and the ultrasonic power is 180-;
s3: embedding: embedding the prepared O/W type mixed solution under magnetic stirring;
s4: and centrifuging the O/W type mixed solution, freeze-drying the obtained precipitate, and grinding to obtain the zanthoxylum oil cake resin microcapsule.
2. The method according to claim 1, wherein the Zanthoxylum bungeanum oil cake in step (1) is a by-product of processing after the production of Zanthoxylum bungeanum oil by leaching with hot oil and pressing.
3. The method according to claim 1, wherein the pulverization in the step (1) is carried out by a high-speed universal pulverizer, and the sieving is carried out by a sieve of 80 meshes.
4. The preparation method according to claim 1, wherein the volume concentration of the ethanol solution added in the step (2) is 50%, and the mass-to-volume ratio of the zanthoxylum oil cake meal to the ethanol solution is 1:12 g/mL.
5. The method according to claim 1, wherein the ethanol solution is extracted in the step (2) for 20 min.
6. The method according to claim 1, wherein the conditions of the ultrasound-assisted embedding in step S2 are as follows: the ultrasonic temperature is 35 ℃, the ultrasonic time is 10min, and the ultrasonic power is 240W.
7. The method according to claim 1, wherein the embedding temperature in step S3 is 35 ℃ and the embedding time is 90min under magnetic stirring.
8. The method according to claim 1, wherein the conditions of the centrifugation in step S4 are: the rotation speed is 6000rpm, and the centrifugation time is 12 min.
9. The method of claim 1, wherein the freeze-drying time in step S4 is 48 hours.
10. A pepper oil cake resin microcapsule prepared by the method of any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110244823.9A CN113142314A (en) | 2021-03-05 | 2021-03-05 | Zanthoxylum oil cake meal resin microcapsule and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110244823.9A CN113142314A (en) | 2021-03-05 | 2021-03-05 | Zanthoxylum oil cake meal resin microcapsule and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113142314A true CN113142314A (en) | 2021-07-23 |
Family
ID=76884325
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110244823.9A Pending CN113142314A (en) | 2021-03-05 | 2021-03-05 | Zanthoxylum oil cake meal resin microcapsule and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113142314A (en) |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1488279A (en) * | 2003-08-15 | 2004-04-14 | 中华全国供销合作总社南京野生植物综 | Zanthoxylum bungeanum esential oil and/or oily resin micro capsule and preparing process thereof |
| CN102349584A (en) * | 2011-09-22 | 2012-02-15 | 徐州工程学院 | Method for preparing myristica oil microcapsule by utilizing ultrasonic waves |
| CN104381953A (en) * | 2014-11-24 | 2015-03-04 | 青岛大学 | Preparation method of water-soluble zanthoxylum bungeanum oleoresin |
| CN104757531A (en) * | 2014-11-05 | 2015-07-08 | 四川省植物工程研究院 | Chinese prickly ash seed oil micro capsule and preparation method thereof |
| CN106509167A (en) * | 2016-11-08 | 2017-03-22 | 四川农业大学 | Production technology for preparing fresh zanthoxylum bungeanum oil by pressing method |
| CN106857876A (en) * | 2017-03-23 | 2017-06-20 | 四川农业大学 | Bean curd coagulant embedding capsule and preparation method thereof |
| CN107041549A (en) * | 2017-04-14 | 2017-08-15 | 广西大学 | A kind of preparation method of garlic oil microscapsule powder |
| CN107114799A (en) * | 2017-06-05 | 2017-09-01 | 江苏大学 | The ultrasonic preparation method of rapeseed protein microcapsules and the application as functional food |
| CN109157424A (en) * | 2018-10-12 | 2019-01-08 | 赵孔发 | A kind of preparation method and applications of Japan pepper essential oil microcapsules |
| CN109907123A (en) * | 2019-01-29 | 2019-06-21 | 青岛农业大学 | A kind of micro-encapsulation of pricklyash peel oleoresin and preparation method thereof |
-
2021
- 2021-03-05 CN CN202110244823.9A patent/CN113142314A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1488279A (en) * | 2003-08-15 | 2004-04-14 | 中华全国供销合作总社南京野生植物综 | Zanthoxylum bungeanum esential oil and/or oily resin micro capsule and preparing process thereof |
| CN102349584A (en) * | 2011-09-22 | 2012-02-15 | 徐州工程学院 | Method for preparing myristica oil microcapsule by utilizing ultrasonic waves |
| CN104757531A (en) * | 2014-11-05 | 2015-07-08 | 四川省植物工程研究院 | Chinese prickly ash seed oil micro capsule and preparation method thereof |
| CN104381953A (en) * | 2014-11-24 | 2015-03-04 | 青岛大学 | Preparation method of water-soluble zanthoxylum bungeanum oleoresin |
| CN106509167A (en) * | 2016-11-08 | 2017-03-22 | 四川农业大学 | Production technology for preparing fresh zanthoxylum bungeanum oil by pressing method |
| CN106857876A (en) * | 2017-03-23 | 2017-06-20 | 四川农业大学 | Bean curd coagulant embedding capsule and preparation method thereof |
| CN107041549A (en) * | 2017-04-14 | 2017-08-15 | 广西大学 | A kind of preparation method of garlic oil microscapsule powder |
| CN107114799A (en) * | 2017-06-05 | 2017-09-01 | 江苏大学 | The ultrasonic preparation method of rapeseed protein microcapsules and the application as functional food |
| CN109157424A (en) * | 2018-10-12 | 2019-01-08 | 赵孔发 | A kind of preparation method and applications of Japan pepper essential oil microcapsules |
| CN109907123A (en) * | 2019-01-29 | 2019-06-21 | 青岛农业大学 | A kind of micro-encapsulation of pricklyash peel oleoresin and preparation method thereof |
Non-Patent Citations (6)
| Title |
|---|
| 唐菊等: "花椒籽油不饱和脂肪酸β-环糊精包合物制备研究", 《中国酿造》 * |
| 张璇等: "固体花椒精油加工关键技术的研究", 《食品工业科技》 * |
| 李萍等: "超声波法制备八角茴香油-β-环糊精微胶囊及其表征分析", 《食品科学》 * |
| 樊振江等: "超声法制备花椒精油微胶囊的研究", 《现代食品科技》 * |
| 蒋凌燕等: "矩阵分析法优化花椒树脂提取工艺研究", 《中国油脂》 * |
| 薛小辉等: "花椒风味成分研究与产品开发现状", 《核农学报》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102161611A (en) | Method for preparing squalene based on tobacco as raw material | |
| CN103361176B (en) | Aroma compound | |
| CN103484245B (en) | The one directed composite extracting method growing tobacco this Studies of The Aromatic Substances of endogenous | |
| CN103462205A (en) | Reconstructed tobacco leaves containing basic incense substances in tobaccos prepared by water extraction method and ethanol extraction method and cigarettes produced by reconstructed tobacco leaves | |
| Zhang et al. | Ultrasound processing of coffee silver skin, brewer’s spent grain and potato peel wastes for phenolic compounds and amino acids: a comparative study | |
| CN104031741A (en) | Preparation method for maillard reaction production particles of tobacco leaf extract | |
| CN112481036A (en) | Enzymolysis preparation method of high-aroma tobacco essential oil | |
| CN113142314A (en) | Zanthoxylum oil cake meal resin microcapsule and preparation method thereof | |
| Zhang et al. | Effects of traditional grinding and superfine grinding technologies on the properties and volatile components of Protaetia brevitarsis larvae powder | |
| CN103478892B (en) | This Studies of The Aromatic Substances in the tobacco of water extraction and ethanol extraction method directed compound collecting from tobacco material | |
| CN103468405B (en) | A kind of water extraction and the ethanol extraction method method of this Studies of The Aromatic Substances in directed compound collecting tobacco from tobacco material | |
| CN103468406B (en) | This Studies of The Aromatic Substances of tobacco endogenous of a kind of directed compound collecting | |
| CN103462204B (en) | Reconstituted tobacco containing composite tobacco aroma substances prepared by water extraction method and supercritical CO2 extraction method and cigarette prepared of same | |
| CN102276455B (en) | Method for extracting effective ingredients from dry cinnamomum burmannii fruits | |
| CN107746748A (en) | A kind of pungent fragrant and sweet rhythm cigarette additive and preparation method thereof and the application in cigarette | |
| CN102276569B (en) | Method of extracting procyanidins from unripe fruits of syzygium cumini | |
| KR101920462B1 (en) | Mineral curcumin drink and its manufacturing method | |
| CN107586594B (en) | Ethanol homogenization-assisted peony seed oil extraction method | |
| CN108065015A (en) | Reducing blood lipid pressed candy of the dragon protein containing ground and preparation method thereof | |
| CN105380168B (en) | A kind of processing technology of instant red date powder | |
| CN104327943A (en) | Method for extracting antrodia camphorata oil from antrodia camphorata sporophore | |
| CN106108105A (en) | A kind of stems of tobacco leaves prepares the method for strong nut note essence | |
| JP2000136181A (en) | Production of high purity cryptoxanthin | |
| JPWO2004048419A1 (en) | Separation, purification and utilization of fenugreek seeds | |
| CN105581374A (en) | Glycerol triacetate extract of pelargonium graveolens L'Herit. and application of extract in cigarettes |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210723 |