CN112391226A - Zanthoxylum oil and preparation method thereof - Google Patents
Zanthoxylum oil and preparation method thereof Download PDFInfo
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- CN112391226A CN112391226A CN202011351572.6A CN202011351572A CN112391226A CN 112391226 A CN112391226 A CN 112391226A CN 202011351572 A CN202011351572 A CN 202011351572A CN 112391226 A CN112391226 A CN 112391226A
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- 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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
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- 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
- A23D9/007—Other edible oils or fats, e.g. shortenings, cooking oils characterised by ingredients other than fatty acid triglycerides
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- 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
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- 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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
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- 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
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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- 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
- C11B3/16—Refining fats or fatty oils by mechanical means
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Abstract
The invention discloses zanthoxylum oil and a preparation method thereof. Using green pepper as raw material, removing impurities, pulverizing, and CO2Supercritical extraction, centrifugal separation, ultrasonic dewatering, low-temperature oil immersion, mixing and the like. By CO2The preparation method of the zanthoxylum oil can ensure the extraction rate of volatile oil and the extraction rate of numb-taste substances under the synergistic action of supercritical extraction, ultrasonic dewatering and low-temperature oil immersion. The invention solves the problem that the prior art uses dry pepper as the raw materialThe problem of low volatile oil content in the preparation of the zanthoxylum oil by using the raw materials and the problem of volatile oil loss caused by overhigh oil immersion temperature in the preparation of the zanthoxylum oil by using the fresh zanthoxylum, the contents of the volatile oil and the numb-taste substances in the fresh zanthoxylum are reserved to the greatest extent, and the taste level of the zanthoxylum oil is enriched.
Description
Technical Field
The invention relates to zanthoxylum oil and a preparation method thereof, belonging to the field of food processing.
Background
The fructus Zanthoxyli belongs to plant of Zanthoxylum of Rutaceae, is deciduous small tree or shrub, has tree height of 3m-6m, blooming in 3-4 months, and fruit ripening in 7-8 months. Compared with the red pepper, the green pepper has obviously higher contents of volatile oil, protein, mineral elements such as calcium, phosphorus, iron and the like than the red pepper. Meanwhile, the green zanthoxylum bungeanum maxim is dark green in color, large in particle, pure and thick in fragrance and taste, is an indispensable main ingredient for chafing dish, preserved szechuan pickle, Sichuan dish and pickled products, and is a top-grade excellent seasoning product.
The main substances affecting the quality of zanthoxylum oil are volatile oil and numb-taste substances in zanthoxylum. The volatile oil mainly influences the flavor of the zanthoxylum oil and is mainly characterized by fragrance, and the numb substance influences the numb degree of the zanthoxylum oil. The spicy substances are generally oil-melting, volatile oil and fat are extremely volatile, and the spicy substances are easy to lose in the processes of drying, heating, oil immersion and the like of the pepper. However, due to technical restrictions, most of the zanthoxylum oil on the market still takes dried zanthoxylum as the raw material, and although some zanthoxylum oil takes fresh zanthoxylum as the raw material, the zanthoxylum oil is also prepared by an oil immersion method. On one hand, the zanthoxylum oil prepared by an oil immersion method is easy to cause the loss of volatile oil if the oil immersion temperature is higher, but the effect of keeping volatile oil can not be achieved, and in addition, the generation of harmful substances can be caused by overhigh temperature; on the other hand, if the oil immersion temperature is low, the numb substance is not easily dissolved.
Therefore, the invention aims to provide the fresh zanthoxylum oil which can ensure that volatile oil and numb-taste substances in the fresh zanthoxylum are effectively dissolved out and can ensure the quality stability.
Disclosure of Invention
For the above reasons, the present invention provides a process for passing CO2The fresh zanthoxylum oil extracted by matching with the process flows of supercritical extraction, steam distillation, low-temperature oil immersion, ultrasonic dewatering and the like not only retains volatile oil and numb-flavor substances in the fresh zanthoxylum to the maximum extent, but also controls the moisture content of the fresh zanthoxylum oil, thereby ensuring the quality stability of the zanthoxylum oil.
A zanthoxylum oil and a preparation method thereof comprise:
1. cleaning fresh fructus Zanthoxyli, removing seeds, and pulverizing to 20-60 mesh powder to obtain fructus Zanthoxyli powder;
2. subjecting fructus Zanthoxyli powder to CO2Performing supercritical extraction to obtain volatile oil (I) and extracted material residue (I);
further, the extraction pressure is 20-40MPa, the extraction temperature is 40-60 ℃, and CO is added2The flow rate is 17-20L/h;
3. centrifuging the volatile oil (I) to obtain a volatile oil (II);
further, the centrifugation condition is 2000-;
4. removing water from the residue (I) by ultrasonic wave to obtain dewatered residue (II)
Furthermore, the ultrasonic dewatering power is 80-120W, the time is 3-5s, the temperature is 50-70 ℃, and the settling time is 1-1.5 h.
5. Immersing the residue (II) in vegetable oil to obtain zanthoxylum oil (I);
further, the oil immersion temperature is 40-60 ℃, and the time is 5 d;
furthermore, the volume ratio of the material residue (II) to the vegetable oil in the oil immersion process is 1: 20-30;
6. and (3) mixing the zanthoxylum oil (I) with the volatile oil (II) to obtain the finished zanthoxylum oil.
The invention also discloses the zanthoxylum oil prepared by any one of the preparation methods.
The invention has the beneficial effects that:
1. according to the invention, the volatile oil is extracted by adopting carbon dioxide supercritical extraction, and the extraction rate of the volatile oil is retained to the maximum extent by adopting a mode of combining the carbon dioxide supercritical extraction and low-temperature oil immersion;
2. the invention adopts the mode of the synergistic effect of the carbon dioxide supercritical extraction, the ultrasonic technology and the oil immersion process, so that the spicy substances in the pepper can obtain higher dissolution rate at a lower oil immersion temperature.
Drawings
FIG. 1 shows the results of volatile oil content measurement;
FIG. 2 is a standard equation of the content of pungent substances;
FIG. 3 shows the results of the measurement of the pungent substance.
Detailed Description
The present invention is described in detail below by way of examples, and it should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention. The invention is susceptible to numerous insubstantial modifications and adaptations by those skilled in the art in view of the foregoing disclosure.
Example 1
A zanthoxylum oil and a preparation method thereof comprise the following steps:
1. cleaning fresh fructus Zanthoxyli, removing seeds, and pulverizing to 40 mesh to obtain fructus Zanthoxyli powder.
2. Subjecting fructus Zanthoxyli powder to CO2Performing supercritical extraction to obtain volatile oil I and extracted residue I, wherein the extraction pressure is 40MPa, the extraction temperature is 40 ℃, and CO is used2The flow rate was 19L/h.
3. Centrifuging the volatile oil I at 3000 rpm for 10min, and separating to obtain volatile oil II;
4. removing water from the material residue I by ultrasonic waves at 1000W and 60 ℃ for 4s, and settling for 1h to obtain material residue II after water removal
5. And (3) immersing the material residue II in vegetable oil at 40 ℃ for 5d to obtain the zanthoxylum oil I, wherein the volume ratio of the material residue II to the vegetable oil is 1: 25.
6. And mixing the zanthoxylum oil I with the volatile oil II to obtain the finished zanthoxylum oil.
Example 2
A zanthoxylum oil and a preparation method thereof comprise the following steps:
1. cleaning fresh fructus Zanthoxyli, removing seeds, and pulverizing to 20 mesh to obtain fructus Zanthoxyli powder.
2. Subjecting fructus Zanthoxyli powder to CO2Performing supercritical extraction to obtain volatile oil I and extracted residue I, wherein the extraction pressure is 20, the extraction temperature is 45 ℃, and CO is used2The flow rate was 17L/h.
3. Centrifuging the volatile oil I at 2500 rpm for 12min, and separating to obtain volatile oil II.
4. And (3) ultrasonically dewatering the material slag I for 3s at 50 ℃ under the condition of 80W, and settling for 1.5h to obtain dewatered material slag II.
5. And (3) immersing the material residue II in vegetable oil at 50 ℃ for 5d to obtain the zanthoxylum oil I, wherein the volume ratio of the material residue II to the vegetable oil is 1: 20.
6. And mixing the zanthoxylum oil I with the volatile oil II to obtain the finished zanthoxylum oil.
Comparative example 1
Compared with example 1, comparative example 1 does not contain CO2Supercritical extraction without the associated steps of volatile oil treatment, comprising the steps of:
1. taking fresh pepper, cleaning, removing seeds, and crushing to 40 meshes to obtain pepper powder I.
2. And (3) ultrasonically dewatering the pepper powder I for 4s at the temperature of 60 ℃ under 1000W, and settling for 1h to obtain dewatered pepper powder II.
3. And (3) immersing the Chinese prickly ash powder II in vegetable oil at 40 ℃ for 5d to obtain a finished product of Chinese prickly ash oil I, wherein the volume ratio of the Chinese prickly ash powder II to the vegetable oil is 1: 25.
Comparative example 2
Compared with the example 1, the comparative example 1 does not carry out ultrasonic wave dewatering and comprises the following steps:
1. cleaning fresh fructus Zanthoxyli, removing seeds, and pulverizing to 40 mesh to obtain fructus Zanthoxyli powder.
2. Subjecting fructus Zanthoxyli powder to CO2Performing supercritical extraction to obtain volatile oil I and extracted residue I, wherein the extraction pressure is 40MPa, the extraction temperature is 40 ℃, and CO is used2The flow rate was 19L/h.
3. Centrifuging the volatile oil I at 3000 rpm for 10min, and separating to obtain volatile oil II;
5. and (3) immersing the material residue I in vegetable oil at 40 ℃ for 5d to obtain the zanthoxylum oil I, wherein the volume ratio of the material residue I to the vegetable oil is 1: 25.
6. And mixing the zanthoxylum oil I with the volatile oil II to obtain the finished zanthoxylum oil.
Comparative example 3
Compared with example 1, comparative example 1 does not contain CO2Supercritical extraction and ultrasonic dewatering, comprising the following steps:
1. taking fresh pepper, cleaning, removing seeds, and crushing to 40 meshes to obtain pepper powder I.
3. And (3) immersing the Chinese prickly ash powder I in vegetable oil at 40 ℃ for 5d to obtain a finished product of Chinese prickly ash oil I, wherein the volume ratio of the Chinese prickly ash powder I to the vegetable oil is 1: 25.
Comparative example 4
Compared with the example 1, the zanthoxylum oil and the preparation method thereof have the advantages that the comparative example 1 does not need ultrasonic wave for removing water, the oil immersion temperature is 90 ℃, and the preparation method comprises the following steps:
1. cleaning fresh fructus Zanthoxyli, removing seeds, and pulverizing to 40 mesh to obtain fructus Zanthoxyli powder.
2. Subjecting fructus Zanthoxyli powder to CO2Performing supercritical extraction to obtain volatile oil I and extracted residue I, wherein the extraction pressure is 40MPa, the extraction temperature is 40 ℃, and CO is used2The flow rate was 19L/h.
3. Centrifuging the volatile oil I at 3000 rpm for 10min, and separating to obtain volatile oil II;
4. and (3) immersing the material residue I in vegetable oil at 90 ℃ for 5d to obtain the zanthoxylum oil I, wherein the volume ratio of the material residue I to the vegetable oil is 1: 25.
5. And mixing the zanthoxylum oil I with the volatile oil II to obtain the finished zanthoxylum oil.
Comparative example 5
Compared with the example 1, the zanthoxylum oil and the preparation method thereof have the advantages that the oil immersion temperature of the comparative example 1 is 90 ℃, and the method comprises the following steps:
1. cleaning fresh fructus Zanthoxyli, removing seeds, and pulverizing to 40 mesh to obtain fructus Zanthoxyli powder.
2. Subjecting fructus Zanthoxyli powder to CO2Performing supercritical extraction to obtain volatile oil I and extracted residue I, wherein the extraction pressure is 40MPa, the extraction temperature is 40 ℃, and CO is used2The flow rate was 19L/h.
3. Centrifuging the volatile oil I at 3000 rpm for 10min, and separating to obtain volatile oil II;
4. removing water from the material residue I by ultrasonic waves at 1000W and 60 ℃ for 4s, and settling for 1h to obtain material residue II after water removal
5. And (3) immersing the material residue II in vegetable oil at 90 ℃ for 5d to obtain the zanthoxylum oil I, wherein the volume ratio of the material residue II to the vegetable oil is 1: 25.
6. And mixing the zanthoxylum oil I with the volatile oil II to obtain the finished zanthoxylum oil.
Test example 1
Determination of volatile oil and numb taste substance:
the content of volatile oil and numb-taste substances in zanthoxylum oil affects the quality of zanthoxylum oil. The volatile oil content influences the flavor of the zanthoxylum oil, and the content of the numbing substances influences the numbing degree of the zanthoxylum oil, so the zanthoxylum oil quality of the examples and the comparative examples is evaluated by the volatile oil content and the numbing substance content in the zanthoxylum oil.
1. Determination of volatile oils
According to the standard of GB/T30385-2013' determination of the content of volatile oil of spices and seasonings
The results of the volatile oils of the examples and comparative examples are shown in the attached FIG. 1:
as can be seen from FIG. 1, the volatile oil content in examples 1 and 2 is relatively high, and that in comparative examples 1 and 2, the CO is not added2The supercritical extraction leads the content of the volatile oil to be obviously reduced, and the comparative example 4 are slightly reduced compared with the example and the comparative example 2 because the oil immersion temperature of the paprika powder is higher.
It can be seen from this that CO2The supercritical extraction has the greatest influence on the volatile oil, and the oil immersion temperature also has certain influence on the volatile oil, so that the extraction rate of the volatile oil is improved by the synergistic effect of the supercritical extraction and the oil immersion temperature.
2. Measurement of spicy substance
Measuring the content of the numb-taste substances by using an ultraviolet spectrophotometer method
(1) Pretreatment: taking a proper amount of zanthoxylum oil (2 g) in a triangular flask with a stopper, adding 20 times of methanol in water bath at 40 ℃, carrying out oscillating extraction for 30min, then transferring the zanthoxylum oil into a separating funnel, shaking for 2min, standing, carrying out layering, taking an upper layer solvent part, carrying out constant volume to 100mL, and then measuring the absorbance value at 254 nm.
(2) Drawing a standard curve: respectively sucking 2.0-10.0mL of pepper sesame flavor substance standard substance, fixing the volume to 25mL with methanol, preparing into 4.4, 8.8, 13.2, 17.6 and 22 mug/mL standard solutions, detecting the absorbance value at 254nm, and making a standard curve by taking the absorbance as a vertical coordinate and the content of the corresponding standard sample as a horizontal coordinate. Dissolving the pretreated sample to be detected with methanol, detecting the light absorption value of the solution, and finding out the content of the numb-taste substances in the zanthoxylum oil from the standard curve. (Standard curve equation of the standards is shown in figure 2)
(3) Test results
The measurement results of the pungent substances of the examples and the comparative examples are shown in FIG. 3.
As shown in the attached figure 3, the content of the spicy substance in the zanthoxylum oil extracted by the synergistic action of the carbon dioxide supercritical extraction, the ultrasonic technology and the oil immersion process is slightly higher than that in the comparative example 4 and the comparative example 5, so that the content of the spicy substance in the zanthoxylum oil extracted by the synergistic action of the carbon dioxide supercritical extraction, the ultrasonic technology and the oil immersion process can completely replace or even exceed the content of the spicy substance extracted by the high-temperature oil immersion process. The content of the numbing substances is influenced to a greater or lesser extent without carbon dioxide supercritical extraction or without ultrasonic technology.
Therefore, the carbon dioxide supercritical extraction, the ultrasonic technology and the oil immersion are inseparable technical processes, and the three cooperate to improve and ensure the extraction amount of the spicy substances.
Claims (7)
1. The preparation method of the zanthoxylum oil is characterized by sequentially comprising the following steps:
(1) removing impurities: cleaning fresh pepper, removing seeds and impurities to obtain the fresh pepper after impurity removal;
(2) crushing: crushing the fresh pepper after impurity removal to 20-60 meshes to obtain pepper powder;
（3）CO2supercritical extraction: subjecting fructus Zanthoxyli powder to CO2Performing supercritical extraction to obtain volatile oil (I) and extracted material residue (I);
(4) centrifugal separation: centrifuging the volatile oil (I) to obtain a volatile oil (II);
(5) ultrasonic dewatering: ultrasonically removing water from the material slag (I) to obtain material slag (II) after water removal;
(6) low-temperature oil immersion: immersing the residue (II) in vegetable oil to obtain zanthoxylum oil (I);
(7) mixing: and (3) mixing the zanthoxylum oil (I) with the volatile oil (II) to obtain the finished zanthoxylum oil.
2. The process according to claim 1, wherein the extraction pressure in the step (3) is 20 to 40MPa, the extraction temperature is 40 to 60 ℃, and CO is added2The flow rate is 17-20L/h.
3. The method as set forth in claim 1, wherein the centrifugation conditions in step (4) are 2000-3500 rpm.
4. The preparation method of claim 1, wherein the ultrasonic dewatering power in the step (5) is 80-120W, the time is 3-5s, the temperature is 50-70 ℃, and the settling time is 1-1.5 h.
5. The method according to claim 1, wherein the immersion temperature in step (6) is 40-60 ℃ and the immersion time is 5 days.
6. The preparation method according to claim 1, wherein the solid-to-liquid ratio (g/ml) of the residue (II) to the vegetable oil in the step (7) is 1: 20-30.
7. Zanthoxylum oil obtained by the preparation method according to any one of claims 1 to 6.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114343023A (en) * | 2022-01-18 | 2022-04-15 | 晨光生物科技集团股份有限公司 | Pepper oil with cooked flavor and preparation method thereof |
| CN115340904A (en) * | 2022-07-14 | 2022-11-15 | 四川五丰黎红食品有限公司 | Preparation method for improving stability of zanthoxylum oil |
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| CN103820202A (en) * | 2012-11-16 | 2014-05-28 | 丰益(上海)生物技术研发中心有限公司 | Method for producing fresh zanthoxylum oil |
| CN106561844A (en) * | 2015-10-10 | 2017-04-19 | 重庆市涪陵区屋机花椒种植场 | A pricklyash peel oil producing process |
| CN109666538A (en) * | 2019-02-27 | 2019-04-23 | 成都新润油脂有限责任公司 | A kind of Zanthoxylum essential oil and its preparation process |
| CN111011543A (en) * | 2019-12-05 | 2020-04-17 | 颐海(霸州)食品有限公司 | Pepper seasoning oil and preparation method and application thereof |
| CN111557347A (en) * | 2020-06-05 | 2020-08-21 | 遵义职业技术学院 | Preparation method of pepper composite seasoning oil |
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2020
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| CN103820202A (en) * | 2012-11-16 | 2014-05-28 | 丰益(上海)生物技术研发中心有限公司 | Method for producing fresh zanthoxylum oil |
| CN106561844A (en) * | 2015-10-10 | 2017-04-19 | 重庆市涪陵区屋机花椒种植场 | A pricklyash peel oil producing process |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114343023A (en) * | 2022-01-18 | 2022-04-15 | 晨光生物科技集团股份有限公司 | Pepper oil with cooked flavor and preparation method thereof |
| CN114343023B (en) * | 2022-01-18 | 2024-02-27 | 晨光生物科技集团股份有限公司 | Zanthoxylum oil with cooked flavor and preparation method thereof |
| CN115340904A (en) * | 2022-07-14 | 2022-11-15 | 四川五丰黎红食品有限公司 | Preparation method for improving stability of zanthoxylum oil |
| CN115340904B (en) * | 2022-07-14 | 2023-12-29 | 四川五丰黎红食品有限公司 | Preparation method for improving stability of zanthoxylum oil |
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