CN115340904B - Preparation method for improving stability of zanthoxylum oil - Google Patents
Preparation method for improving stability of zanthoxylum oil Download PDFInfo
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- CN115340904B CN115340904B CN202210826309.0A CN202210826309A CN115340904B CN 115340904 B CN115340904 B CN 115340904B CN 202210826309 A CN202210826309 A CN 202210826309A CN 115340904 B CN115340904 B CN 115340904B
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- 241000949456 Zanthoxylum Species 0.000 title claims abstract description 88
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 238000000926 separation method Methods 0.000 claims abstract description 168
- 238000000605 extraction Methods 0.000 claims abstract description 83
- 239000003921 oil Substances 0.000 claims abstract description 79
- 238000010008 shearing Methods 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims description 94
- 235000019198 oils Nutrition 0.000 claims description 72
- 239000000284 extract Substances 0.000 claims description 31
- 238000009210 therapy by ultrasound Methods 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 12
- 239000008158 vegetable oil Substances 0.000 claims description 12
- 239000010773 plant oil Substances 0.000 claims description 7
- 235000012424 soybean oil Nutrition 0.000 claims description 6
- 239000003549 soybean oil Substances 0.000 claims description 6
- 238000011278 co-treatment Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 35
- 150000001408 amides Chemical class 0.000 abstract description 26
- 239000011347 resin Substances 0.000 abstract description 25
- 229920005989 resin Polymers 0.000 abstract description 25
- 239000000341 volatile oil Substances 0.000 abstract description 24
- 239000001814 pectin Substances 0.000 abstract description 19
- 235000010987 pectin Nutrition 0.000 abstract description 19
- 229920001277 pectin Polymers 0.000 abstract description 19
- 238000010438 heat treatment Methods 0.000 abstract description 14
- 239000004519 grease Substances 0.000 abstract description 7
- 238000002425 crystallisation Methods 0.000 abstract description 6
- 230000008025 crystallization Effects 0.000 abstract description 6
- 238000005189 flocculation Methods 0.000 abstract description 6
- 230000016615 flocculation Effects 0.000 abstract description 6
- 238000012545 processing Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 235000013305 food Nutrition 0.000 abstract description 4
- 238000001132 ultrasonic dispersion Methods 0.000 abstract description 3
- 238000004321 preservation Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 22
- 235000002566 Capsicum Nutrition 0.000 description 18
- 241000758706 Piperaceae Species 0.000 description 15
- 239000012535 impurity Substances 0.000 description 8
- 238000001816 cooling Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
- 244000089698 Zanthoxylum simulans Species 0.000 description 5
- 239000000796 flavoring agent Substances 0.000 description 4
- 235000019634 flavors Nutrition 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000008601 oleoresin Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 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
- 238000004140 cleaning Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000000265 homogenisation Methods 0.000 description 2
- 230000001965 increasing effect Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000013409 condiments Nutrition 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000199 molecular distillation Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/006—Refining fats or fatty oils by extraction
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention relates to the technical field of food deep processing, in particular to a preparation method for improving the stability of zanthoxylum oil. By supercritical CO against the prior art 2 The method adopts the supercritical CO to control respectively, and solves the problems that the xanthoxylum oil resin extracted by the extraction equipment is easy to generate crystallization due to high content of amide substances, is unfavorable for blending and flocculation occurs in the preservation process due to high content of pectin 2 The pressure and the temperature of a separation kettle I and a separation kettle II in extraction equipment are respectively used for obtaining the zanthoxylum oil resin and volatile oil, the zanthoxylum oil resin is treated in an ultrasonic combined shearing mode, and then under the condition of heating, the zanthoxylum oil resin is fused into other grease through ultrasonic dispersion treatment, so that the effects of fully homogenizing substances such as pectin in the zanthoxylum oil resin in a system and obtaining stable zanthoxylum oil are achieved.
Description
Technical Field
The invention relates to the technical field of food deep processing, in particular to a preparation method for improving the stability of zanthoxylum oil.
Background
The pepper is a commercial crop with both medicine and food purposes, and the fruit of the pepper is known as one of the eight-ingredient condiments. The zanthoxylum oil prepared from the zanthoxylum is the most common zanthoxylum processed product, has mild taste, rich zanthoxylum fragrance, pure and tasty, has the effects of removing fishy smell and mutton smell and enhancing flavor, and is deeply favored by consumers.
At present, the ways of producing the zanthoxylum oil by food processing enterprises comprise the following two main types: firstly, hot-dip extraction or solvent method is carried out on dry and fresh peppers by utilizing an oil-immersed method to directly obtain zanthoxylum oil; secondly, using cold pressing method and supercritical CO 2 The method of extraction and the like extracts the zanthoxylum oil resin from the zanthoxylum, and then the zanthoxylum oil resin is mixed with other grease for use. The zanthoxylum oil resin mainly comprises amide substances and volatile oil components in the zanthoxylum, and the zanthoxylum oil obtained by blending other grease with the zanthoxylum oil resin has the flavor more similar to the flavor of original fruits of the zanthoxylum, so that the zanthoxylum oil becomes a key point of research. Wherein, supercritical CO 2 The extraction rate of the zanthoxylum oil resin prepared by the extraction method is highThe method has the advantages of no solvent residue, high safety and obvious advantages, and is widely accepted.
But supercritical CO 2 On one hand, due to the high content of amide substances, the zanthoxylum oil resin extracted by the extraction method is easy to crystallize, thereby being unfavorable for the preparation of the zanthoxylum oil; on the other hand, pectin substances contained in the oil can cause unstable phenomena such as flocculation and the like in the process of preserving the zanthoxylum oil, thereby affecting the quality of the zanthoxylum oil.
Based on the phenomenon, the supercritical process of the zanthoxylum bungeanum is optimized, the raw materials are subjected to grading treatment, the blending process is optimized, and the prepared zanthoxylum bungeanum oil has strong stability and full flavor.
Disclosure of Invention
Based on the above problems, the present invention aims to provide a preparation method for increasing the stability of zanthoxylum oil by supercritical CO 2 The extracted zanthoxylum oil resin is subjected to the combined action of ultrasonic treatment and shearing treatment, and then is subjected to the blending treatment, so that substances such as pectin and the like are fully and uniformly arranged in the system, and the crystallization of amide substances is effectively reduced, so that a zanthoxylum oil product with stable system is obtained.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
the preparation method for improving the stability of the zanthoxylum oil comprises the steps of pretreatment, extraction and blending of the zanthoxylum oil, wherein the extraction comprises the following steps:
supercritical CO 2 Extraction: supercritical CO treatment of pretreated fructus Zanthoxyli 2 After the equipment is extracted, respectively receiving the extract liquid obtained in the separation kettle I and the separation kettle II to obtain extract liquid of the separation kettle I and extract liquid of the separation kettle II;
and (3) treating an extraction liquid in a separation kettle I: the extraction liquid of the separation kettle I is subjected to first ultrasonic and shearing treatment to obtain a first separation kettle I treatment liquid, the first separation kettle I treatment liquid is heated, vegetable oil is added into the first separation kettle I treatment liquid, and a second separation kettle I treatment liquid is obtained through second ultrasonic treatment;
and (3) treating an extraction liquid of a separation kettle II: and (3) centrifuging the extract liquid of the separation kettle II, and removing the lower water layer to obtain the treatment liquid of the separation kettle II.
Further, the superclinical settingBoundary CO 2 The extraction temperature is 40-50deg.C, the extraction pressure is 28-32MPa, and CO is used for extracting 2 The flow rate is 12-45L/h, and the extraction time is 120-150min.
Further, in the supercritical CO 2 The temperature of the separation kettle I is 40-45 ℃ and the pressure is 10-11MPa, and the temperature of the separation kettle II is 35-40 ℃ and the pressure is 5.5-6MPa in the extraction.
Further, the first ultrasonic treatment frequency is set to be 80-100HZ in the first separation kettle I treatment liquid obtained by carrying out first ultrasonic and shearing treatment on the extraction liquid of the separation kettle I, and the time is 10-15min; the shearing treatment is carried out at the frequency of 10000-15000r/min for 5-8min.
Further, the second ultrasonic treatment is carried out at a frequency of 80-100HZ for 10-15min.
Further, the first separation kettle I treatment liquid is heated until the temperature of the first separation kettle I treatment liquid is 45-50 ℃.
Further, the vegetable oil is a breaker vegetable oil; and the adding ratio of the treatment liquid of the separation kettle I to the secant vegetable oil is (1-10) according to the weight parts: (90-99).
The application also discloses the zanthoxylum oil prepared by the preparation method, which comprises, by weight, 100 parts of soybean oil, 5-20 parts of second separation kettle I treatment liquid and 0.1-0.3 part of separation kettle II treatment liquid.
Compared with the prior art, the application has the following beneficial effects:
the application aims at the prior art of passing through supercritical CO 2 The amide substances and volatile oil substances in the zanthoxylum oil resin extracted by the extraction equipment are often mixed together, and the zanthoxylum oil resin also contains moisture and pectin wind impurities, and meanwhile, the problem of flocculation in the preservation process caused by the fact that the crystallization is easy to generate due to the high content of the amide substances and the blending is unfavorable and the pectin content is high; the application adopts the separate control of supercritical CO 2 The pressure and temperature of the separating kettle I and the separating kettle II in the extraction equipment separate the amide substances and volatile oil in the zanthoxylum oil resin by controlling the temperature and the pressure, and simultaneously pectinThe components are concentrated in the amide substances, and the moisture is concentrated in the volatile oil, so that the subsequent treatment is facilitated; then the amide components in the zanthoxylum oil resin are treated in a mode of ultrasonic combination and shearing, and then the zanthoxylum oil resin is fused into other grease through ultrasonic dispersion treatment under the condition of heating, so that the effects of fully and uniformly mixing substances such as pectin and the like in the zanthoxylum oil resin in a system and obtaining stable zanthoxylum oil are achieved.
Drawings
FIG. 1: test example 1 Zanthoxylum oil sample status at day 30.
Detailed Description
The present invention will be further described in detail with reference to the following embodiments, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the description is only illustrative and is not intended to limit the scope of the invention. In addition, in the following description, descriptions of well-known structures and techniques are omitted so as not to unnecessarily obscure the present invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The first embodiment of the invention provides a preparation method for improving the stability of zanthoxylum oil, which comprises the steps of pretreatment, extraction and blending of the zanthoxylum oil, wherein the extraction comprises the following steps:
supercritical CO 2 Extraction: supercritical CO treatment of pretreated fructus Zanthoxyli 2 After the equipment is extracted, respectively receiving the extract liquid obtained in the separation kettle I and the separation kettle II to obtain extract liquid of the separation kettle I and extract liquid of the separation kettle II;
and (3) treating an extraction liquid in a separation kettle I: the extraction liquid of the separation kettle I is subjected to first ultrasonic and shearing treatment to obtain a first separation kettle I treatment liquid, the first separation kettle I treatment liquid is heated, vegetable oil is added into the first separation kettle I treatment liquid, and a second separation kettle I treatment liquid is obtained through second ultrasonic treatment;
and (3) treating an extraction liquid of a separation kettle II: and (3) centrifuging the extract liquid of the separation kettle II, and removing the lower water layer to obtain the treatment liquid of the separation kettle II.
In the embodiment of the invention, the pretreatment is to select fresh peppers, screen and remove shell and leaf and impurities of the peppers, clean and dry the peppers until the water content of the fresh peppers is not higher than 15%, crush the peppers and then pass through a 20-mesh sieve.
In the embodiment of the invention, the extraction liquid of the separation kettle I is actually amide substances in the extracted zanthoxylum oil resin, and pectin impurities are entrained, and as the amide substances are easy to crystallize and pectin components exist in the extracted zanthoxylum oil resin, the direct use can lead to uneven distribution of the zanthoxylum oil resin, flocculation of the pectin substances in the storage process and the like, and subsequent treatment is needed to solve the technical problem.
In the embodiment of the invention, the extract liquid of the separation kettle II is actually volatile oil in the extracted zanthoxylum oleoresin, and the supercritical CO is controlled respectively according to the properties of different components in the zanthoxylum 2 The temperature and pressure of the separation kettle I and the separation kettle II in the extraction equipment are separated, and the water is more contained in the separation kettle I and the separation kettle II, so that the water removal treatment is needed.
In an embodiment of the invention, the supercritical CO 2 The common supercritical CO is adopted for extraction 2 Extraction equipment, it generally divide into two separation kettles, and according to the difference of extract polarity size, boiling point height, molecular weight size, selectively separates out the composition in proper order, and this application is through carrying out pressure and temperature control to separation kettle I and separation kettle II respectively, optimizes extraction technology, makes amide class material concentrate in separation kettle I, and volatile oil material concentrate in separation kettle II, for follow-up pertinence treatment separation kettle I, separation kettle II material provide basis.
In the embodiment of the invention, the extraction liquid of the separation kettle I is concentrated extracted zanthoxylum oleoresin, and the main component of the extraction liquid is amide substances, and the extraction liquid is easy to crystallize and has higher pectin content, so that flocculates are generated in the storage process; the pectin substances are uniformly dispersed in the system through ultrasonic combination and shearing treatment; meanwhile, the zanthoxylum oil resin is blended into the vegetable oil by utilizing the ultrasonic dispersion treatment with the temperature rise so as to stabilize the finished zanthoxylum oil system.
In the embodiment of the invention, the extract liquid of the separation kettle II is volatile grease, and contains certain moisture, so that the layering and quality of the grease can be reduced, and the moisture in the grease is removed through centrifugal treatment, thereby achieving the aim of stabilizing the zanthoxylum oil system.
In the embodiment of the invention, 100 parts of soybean oil is taken according to parts by weight, the temperature is raised to 120-150 ℃, the temperature is lowered to 40-50 ℃, 5-20 parts of the second separation kettle I treatment liquid which is raised to 45-50 ℃ is added, the mixture is stirred and mixed uniformly, the temperature is lowered to 30-35 ℃,0.1-0.3 part of the kettle II treatment liquid is added, the mixture is stirred and mixed uniformly, and the mixture is stood for 40-48 hours, thus obtaining the zanthoxylum oil.
In some embodiments, the supercritical CO is provided 2 The extraction temperature is 40-50deg.C, the extraction pressure is 28-32MPa, and CO is used for extracting 2 The flow rate is 12-45L/h, and the extraction time is 120-150min.
In some embodiments, in the supercritical CO 2 The temperature of the separation kettle I is 40-45 ℃ and the pressure is 10-11MPa, and the temperature of the separation kettle II is 35-40 ℃ and the pressure is 5.5-6MPa in the extraction.
In some specific embodiments, the first ultrasonic treatment frequency is set to be 80-100HZ in the first separation kettle I treatment liquid obtained by carrying out first ultrasonic and shearing treatment on the extraction liquid of the separation kettle I, and the time is 10-15min; the shearing treatment is carried out at the frequency of 10000-15000r/min for 5-8min.
In some embodiments, the second ultrasonic treatment is performed at a frequency of 80-100HZ for a treatment time of 10-15 minutes.
In some embodiments, the heating of the first separation vessel I treatment fluid to the first separation vessel I treatment fluid temperature is in the range of 45-50deg.C.
In some embodiments, the vegetable oil is a breaker vegetable oil; and the adding ratio of the treatment liquid of the separation kettle I to the secant vegetable oil is (1-10) according to the weight parts: (90-99).
The broken plant oil is cooked plant oil prepared by heating plant oil.
The second embodiment of the application proves that the extraction rates of the xanthoxylum amides and volatile oil substances in the separation kettle I and the separation kettle II are compared with each other at different temperatures and pressures through specific experimental verification.
According to the application, the amide substances and volatile oil substances in the zanthoxylum oleoresin are respectively extracted by controlling the temperature and the pressure of the separation kettle I and the separation kettle II, based on the difference of polarity and volatility, pectin substances are concentrated in the amide substances (the separation kettle I) in a large amount, and moisture is concentrated in the volatile oil (the separation kettle II) in a large amount, so that the pectin substances are concentrated in the volatile oil (the separation kettle I) in a large amount and are mixed with the existing supercritical CO 2 After extraction, the molecular distillation means is adopted for further purification and separation treatment, and the technical means can be used for more simply and conveniently treating impurities, so that the subsequent homogenization and water removal treatment of amide substances and volatile oil are facilitated.
The test method comprises the following steps: three experimental groups and 2 control groups are arranged, wherein the temperature and the pressure of the separation kettle I and the separation kettle II are respectively set as follows:
experiment group 1: the temperature of the separation kettle I is 43 ℃, the pressure is 10MPa, the temperature of the separation kettle II is 38 ℃, and the pressure is 5.8MPa;
experiment group 2: the temperature of the separation kettle I is 40 ℃, the pressure is 10MPa, the temperature of the separation kettle II is 35 ℃, and the pressure is 5.5MPa;
experiment group 3: the temperature of the separation kettle I is 45 ℃, the pressure is 11MPa, the temperature of the separation kettle II is 40 ℃, and the pressure is 6MPa;
control group 1: the temperature of the separation kettle I is 35 ℃, the pressure is 8MPa, the temperature of the separation kettle II is 32 ℃ and the pressure is 5MPa;
control group 2: the temperature of the separation kettle I is 48 ℃, the pressure is 12MPa, the temperature of the separation kettle II is 42 ℃, and the pressure is 6.5 MPa;
controlling supercritical CO 2 The extraction temperature of the extraction equipment is 45 ℃, the extraction pressure is 30 MPa, and the CO is extracted 2 The flow rate was 30L/h and the extraction time was 135min.
The testing method comprises the following steps: measurement of total content of Zanthoxylum bungeanum amide: ultraviolet spectrophotometry for determining total content of Zanthoxylum bungeanum amide in processed products of Zanthoxylum bungeanum with GH/T1290-2020
And (3) measuring the content of the volatile oil of the zanthoxylum oil resin: referring to GB/T17527-2009 determination of content of pepper essential oil, 20.0g of good zanthoxylum oleoresin is weighed and put into a flask, a proper amount of distilled water and anti-explosion boiling grains are added, a volatile oil determination device is connected, and a distillation receiving tube is filled with water in advance. Heating the flask, slowly distilling, controlling the distilling rate to be 1-1.5 drops per second when heating, stopping heating until the oil quantity is not increased after 2 times of reading continuously for 1h, standing for a while, waiting for the oil layer to become clear, starting reading, and calculating the volatile oil content.
Yield is as follows: extraction ratio (%) = (weight of volatile oil)/(weight of powder) 100%.
Test results: see table 1.
Analysis of results: as can be seen from the experimental results in Table 1, under the conditions of the temperature and the pressure of the separating kettle I and the separating kettle II specified in the application, the amide substances in the zanthoxylum oil resin are concentrated in the separating kettle 1, the volatile oil substances are concentrated in the separating kettle II, in this case, the subsequent separate processing of the substances in the separating kettle I and the separating kettle II can be simplified, the foundation is laid for subsequent separate homogenization and water removal, if the separate processing is not carried out, the amide substances and the volatile oil are mixed together, meanwhile, the pectin and the impurities are mixed together, so that the separating kettle I contains more volatile oil and water, the technical scheme of carrying out ultrasonic and shearing on the ultrasonic and shearing treatment on the volatile oil can not effectively remove the water, the volatile oil is lost, the separating kettle II contains more amide substances and pectin, and the centrifugal separation treatment on the volatile oil can not effectively remove the pectin, thereby causing flocculation and turbidity in the subsequent storage process.
Table 1 experimental results
。
The following examples disclose the preparation of the present application to increase the stability of zanthoxylum oil, and it is apparent that the described examples are some, but not all, of the examples of the present disclosure. All other embodiments, which can be made by one of ordinary skill in the art without the need for inventive faculty, are within the scope of the present disclosure, based on the described embodiments of the present disclosure.
Example 1 preparation of Zanthoxylum oil
1. Pretreatment: selecting fresh peppers, screening to remove shell and leaf of the peppers and impurities, cleaning and drying until the water content of the fresh peppers is not higher than 15%, crushing and sieving with a 20-mesh sieve;
2. extracting: (1) Supercritical CO 2 Extraction: placing pretreated fructus Zanthoxyli in supercritical CO 2 Equipment extraction equipment, extraction temperature is controlled to be 45 ℃, extraction pressure is controlled to be 30 MPa, and CO is extracted 2 The flow rate is 16L/h, the temperature of the separation kettle I is controlled to be 43 ℃, the pressure is controlled to be 10MPa, the temperature of the separation kettle II is controlled to be 38 ℃, and the pressure is controlled to be 5.8MPa; extracting for 135min, and respectively connecting the extracts in the separation kettle I and the separation kettle II to obtain an extraction liquid of the separation kettle I and an extraction liquid of the separation kettle II;
(2) And (3) treating an extraction liquid in a separation kettle I: carrying out ultrasonic treatment on the extract of the separation kettle I for 90 HZ and 13min, and carrying out shearing treatment on the extract of the separation kettle I for 13000 r/min and 7min to obtain a first treatment liquid of the separation kettle I; heating 5 parts of the first separation kettle I treatment liquid to 48 ℃, adding 95 parts of the off-plant oil into the first separation kettle I treatment liquid, and carrying out ultrasonic treatment for 90 HZ and 13min to obtain a second separation kettle I treatment liquid;
(3) And (3) treating an extraction liquid of a separation kettle II: centrifuging the extract of the separation kettle II for 15min at 5500 r/min, and removing the lower water layer to obtain a treatment liquid of the separation kettle II;
3. and (3) blending: taking 100 parts of soybean oil, heating to 130 ℃ for breaking growth, cooling to 45 ℃, adding 12 parts of the second separation kettle I treatment liquid heated to 48 ℃, stirring and mixing uniformly, cooling to 33 ℃, adding 0.2 part of the separation kettle II treatment liquid, stirring and mixing uniformly, and standing for 44h to obtain the zanthoxylum oil.
Example 2 preparation of Zanthoxylum oil
1. Pretreatment: selecting fresh peppers, screening to remove shell and leaf of the peppers and impurities, cleaning and drying until the water content of the fresh peppers is not higher than 15%, crushing and sieving with a 20-mesh sieve;
2. extracting: (1) Supercritical CO 2 Extraction: placing pretreated fructus Zanthoxyli in supercritical CO 2 Equipment extraction equipment, extraction temperature is controlled to be 40 ℃, and extraction pressure is controlled to be 28 MPa,CO 2 The flow rate is 12L/h, the temperature of the separation kettle I is controlled to be 40 ℃, the pressure is controlled to be 10MPa, the temperature of the separation kettle II is controlled to be 35 ℃, and the pressure is controlled to be 5.5MPa; extracting for 120 min, and respectively connecting the extracts in the separation kettle I and the separation kettle II to obtain an extraction liquid of the separation kettle I and an extraction liquid of the separation kettle II;
(2) And (3) treating an extraction liquid in a separation kettle I: carrying out ultrasonic treatment on the extract of the separation kettle I for 80HZ and 10min, and shearing for 10000 r/min and 5min to obtain a first treatment liquid of the separation kettle I; heating 1 part of the first separation kettle I treatment liquid to 45 ℃, adding 99 parts of the raw plant oil, and carrying out ultrasonic treatment for 10min at 80HZ to obtain a second separation kettle I treatment liquid;
(3) And (3) treating an extraction liquid of a separation kettle II: centrifuging the extract of the separation kettle II for 5000r/min and 10min, and removing the lower water layer to obtain a treatment liquid of the separation kettle II;
3. and (3) blending: taking 100 parts of soybean oil, heating to 120 ℃ for breaking, cooling to 40 ℃, adding 5 parts of the second separation kettle I treatment liquid heated to 45 ℃, stirring and mixing uniformly, cooling to 30 ℃, adding 0.1 part of the separation kettle II treatment liquid, stirring and mixing uniformly, and standing for 40 hours to obtain the zanthoxylum oil.
Example 3 preparation of Zanthoxylum oil
1. Pretreatment: selecting fresh peppers, screening to remove shell and leaf of the peppers and impurities, cleaning and drying until the water content of the fresh peppers is not higher than 15%, crushing and sieving with a 20-mesh sieve;
2. extracting: (1) Supercritical CO 2 Extraction: placing pretreated fructus Zanthoxyli in supercritical CO 2 Equipment extraction equipment, extraction temperature is controlled to be 50 ℃, extraction pressure is controlled to be 32MPa, and CO is extracted 2 The flow rate is 45L/h, the temperature of the separation kettle I is controlled to be 45 ℃, the pressure is controlled to be 11MPa, the temperature of the separation kettle II is controlled to be 40 ℃, and the pressure is controlled to be 6MPa; extracting for 150min, and respectively connecting the extracts in the separation kettle I and the separation kettle II to obtain an extraction liquid of the separation kettle I and an extraction liquid of the separation kettle II;
(2) And (3) treating an extraction liquid in a separation kettle I: carrying out ultrasonic treatment on the extract of the separation kettle I for 15min at 100HZ, and carrying out shearing treatment at 15000r/min for 8min to obtain a first treatment liquid of the separation kettle I; heating 10 parts of the first separation kettle I treatment liquid to 50 ℃, adding 90 parts of the raw plant oil, and carrying out ultrasonic treatment for 15min at 100HZ to obtain a second separation kettle I treatment liquid;
(3) And (3) treating an extraction liquid of a separation kettle II: centrifuging the extract of the separation kettle II at 6000r/min for 15min, and removing the lower water layer to obtain a treatment liquid of the separation kettle II;
3. and (3) blending: taking 100 parts of soybean oil, heating to 150 ℃ for breaking growth, cooling to 50 ℃, adding 20 parts of the second separation kettle I treatment liquid heated to 50 ℃, stirring and mixing uniformly, cooling to 35 ℃, adding 0.3 part of the separation kettle II treatment liquid, stirring and mixing uniformly, and standing for 48 hours to obtain the zanthoxylum oil.
Comparative example 1 preparation of Zanthoxylum oil
The preparation process was the same as in example 1, except that comparative example 1 did not treat the extract from separation tank I.
Comparative example 2 preparation of Zanthoxylum oil
The preparation method is the same as in example 1, except that the extract of the separation kettle I in comparative example 2 is subjected to only shearing treatment and no first ultrasonic treatment.
Comparative example 3 preparation of Zanthoxylum oil
The preparation method is the same as in example 1, except that comparative example 3 only carries out the first ultrasonic treatment on the extract of the separation tank I, and does not carry out the shearing treatment.
Comparative example 4 preparation of Zanthoxylum oil
The preparation method is the same as in example 1, except that the treatment solution of the first separation tank I is not treated in comparative example 4.
Comparative example 5 preparation of Zanthoxylum oil
The preparation process was the same as in example 1, except that in comparative example 5, the temperature of separation vessel I was 35℃and the pressure was 8MPa, and the temperature of separation vessel II was 32℃and the pressure was 5 MPa.
Comparative example 6 preparation of Zanthoxylum oil
The preparation process was the same as in example 1, except that in comparative example 5, the temperature of separation vessel I was 48℃and the pressure was 12MPa, the temperature of separation vessel II was 42℃and the pressure was 6.5 MPa.
Test example 1 sample State observation
The test method comprises the following steps: the Zanthoxylum oil prepared in examples 1-3 and comparative examples 1-5 was placed at 37℃in days, and the state changes of the samples on day 0, day 3, day 7, day 15 and day 30 were recorded, respectively, to evaluate the texture state of Zanthoxylum oil.
Judgment standard: see table 2.
Experimental results: see table 3.
Analysis of results: as can be seen from Table 1 in combination with FIG. 1, the quality of examples 1-3 is not greatly reduced after 30 days of storage, and the zanthoxylum oil is transparent and clear and has no insoluble substances (see FIG. 1); example 1 compared with comparative example 1 (without treatment of the extract of separation tank I), the quality was reduced from 3 days of storage to 30 days of precipitation or insolubles in the zanthoxylum oil (see FIG. 1), demonstrating that the zanthoxylum oil without treatment of the extract of separation tank I is prone to precipitation or flocculation during storage due to the presence of pectin, which is a characteristic of easy crystallization; example 1 compared with comparative example 2 (the extraction liquid of separation kettle I is only subjected to shearing treatment and is not subjected to first ultrasonic treatment) and comparative example 3 (the extraction liquid of separation kettle I is only subjected to first ultrasonic treatment and is not subjected to shearing treatment), comparative examples 2 and 3 are obviously turbid after being stored for 30 days (see figure 1), and the quality of the zanthoxylum oil is influenced by ultrasonic treatment and shearing, so that the combination of ultrasonic treatment and shearing treatment is necessary to effectively control crystallization and disperse pectin, thereby stabilizing the quality of the zanthoxylum oil; in example 1, compared with comparative example 4 (the first separation tank I treatment liquid is not treated), comparative example 4 obviously produces turbidity (see figure 1), which shows that the first separation tank I treatment liquid is obtained by ultrasonic combination and shearing treatment, and the crystallization of amide substances is reduced by ultrasonic treatment under the condition of heating, so that the amide substances are dispersed in the zanthoxylum oil product, and only a plurality of the amide substances are combined to obtain the zanthoxylum oil with stable system; example 1 and comparative examples 5 and 6 (changing the temperature and pressure parameters of separation kettles I and II respectively), comparative example 5 is obviously turbid, comparative example 6 generates flocculate (see figure 1), which shows that the temperature and parameters of separation kettles I and II have important influence on subsequent treatment respectively, and amide substances and volatile oil in zanthoxylum oil resin must be separated as far as possible in the early stage and treated respectively, so that the technical effect of the application can be achieved.
TABLE 2 insoluble scoring criteria
。
TABLE 3 observations
。
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (7)
1. The preparation method for improving the stability of the zanthoxylum oil comprises the steps of pretreatment, extraction and blending of the zanthoxylum oil, and is characterized in that the extraction comprises the following steps:
supercritical CO 2 Extraction: supercritical CO treatment of pretreated fructus Zanthoxyli 2 After the equipment is extracted, respectively receiving the extract liquid obtained in the separation kettle I and the separation kettle II to obtain extract liquid of the separation kettle I and extract liquid of the separation kettle II;
and (3) treating an extraction liquid in a separation kettle I: the extraction liquid of the separation kettle I is subjected to first ultrasonic and shearing treatment to obtain a first separation kettle I treatment liquid, the first separation kettle I treatment liquid is heated, vegetable oil is added into the first separation kettle I treatment liquid, and a second separation kettle I treatment liquid is obtained through second ultrasonic treatment;
and (3) treating an extraction liquid of a separation kettle II: centrifuging the extract of the separation kettle II, and removing the lower water layer to obtain a treatment liquid of the separation kettle II;
at the supercritical CO 2 Setting the temperature of the separation kettle I at 40-45 ℃ and the pressure at 10-11MPa in the extraction, and setting the separation kettle IIThe temperature is 35-40 ℃ and the pressure is 5.5-6MPa;
the first ultrasonic treatment frequency is set to be 80-100HZ in the first separation kettle I treatment liquid obtained by carrying out first ultrasonic and shearing treatment on the extraction liquid of the separation kettle I, and the time is 10-15min; the shearing treatment is carried out at the frequency of 10000-15000r/min for 5-8min;
the second ultrasonic treatment is carried out at the frequency of 80-100HZ for 10-15min.
2. The method of claim 1, wherein the supercritical CO is provided 2 The extraction temperature is 40-50deg.C, the extraction pressure is 28-32MPa, and CO is used for extracting 2 The flow rate is 12-45L/h, and the extraction time is 120-150min.
3. The method according to claim 1, wherein the first separation vessel I treatment liquid is heated to a temperature of 45-50 ℃.
4. The method of claim 1, wherein the vegetable oil is a stump vegetable oil; and the adding ratio of the treatment liquid of the separation kettle I to the off-plant oil is (1-10) to (90-99) according to the weight parts.
5. The method according to claim 1, wherein the centrifugation is performed at 5000-6000r/min for 10-20min.
6. A zanthoxylum oil prepared according to the preparation method of any one of claims 1-5.
7. The zanthoxylum oil according to claim 6, comprising 100 parts by weight of soybean oil, 5-20 parts by weight of the second separation tank I treatment liquid, and 0.1-0.3 parts by weight of the separation tank II treatment liquid.
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