CN112322379A - Extraction process of litsea pungens fatty oil - Google Patents
Extraction process of litsea pungens fatty oil Download PDFInfo
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- CN112322379A CN112322379A CN202011137271.3A CN202011137271A CN112322379A CN 112322379 A CN112322379 A CN 112322379A CN 202011137271 A CN202011137271 A CN 202011137271A CN 112322379 A CN112322379 A CN 112322379A
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- 238000000605 extraction Methods 0.000 title claims abstract description 112
- 239000010685 fatty oil Substances 0.000 title claims abstract description 74
- 241000633855 Litsea pungens Species 0.000 title claims abstract description 39
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000002904 solvent Substances 0.000 claims abstract description 47
- 239000003208 petroleum Substances 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000010298 pulverizing process Methods 0.000 claims abstract description 13
- 235000012854 Litsea cubeba Nutrition 0.000 claims description 39
- 240000002262 Litsea cubeba Species 0.000 claims description 38
- 239000000463 material Substances 0.000 description 19
- 239000002245 particle Substances 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 8
- 235000013399 edible fruits Nutrition 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 238000007873 sieving Methods 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 238000012216 screening Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 3
- 206010008479 Chest Pain Diseases 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000013401 experimental design Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 239000000341 volatile oil Substances 0.000 description 2
- 206010002383 Angina Pectoris Diseases 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 241000218195 Lauraceae Species 0.000 description 1
- 241001081179 Litsea Species 0.000 description 1
- 241000133744 Litsea lancilimba Species 0.000 description 1
- 238000000944 Soxhlet extraction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 208000029078 coronary artery disease Diseases 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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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
-
- 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
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses an extraction process of litsea pungens fatty oil. The method comprises the following steps: (1) pulverizing Litsea pungens to 10-80 mesh to obtain product A; (2) adding the product A into a Soxhlet extractor, wherein the extraction solvent in the extraction tank is petroleum ether, and the mass ratio of the product A to the petroleum ether is 1: 4-12, extracting in water bath at 85-99 ℃ for 1.5-2.5h, and recovering solvent by reduced pressure volatilization to obtain fatty oil. The method has the advantages of high extraction rate and low cost.
Description
Technical Field
The invention relates to litsea cubeba fatty oil, in particular to an extraction process of litsea cubeba fatty oil.
Background
Litsea pungens (scientific name: Litsea lancilimba Merr.) are evergreen trees of the genus Litsea in the family Lauraceae, up to 10 meters; the bark is grey brown or black brown, the highest big fruit can reach 20 m, the fruit is generally ripe in november to december, the ripe fruit is red and is in a tray shape, and the fruit looks very pleasant in a far distance. Besides the ornamental value, the medicinal value is also one of the effects of the litsea pungens, the litsea pungens contain a plurality of chemical components which are traditional Chinese medicinal materials with extremely good curative effects, and the litsea pungens are used for treating chest pain, chest distress and asthma in folk, and particularly have obvious relieving effect on patients diagnosed with coronary heart disease and angina. The existing extraction process of litsea cubeba fatty oil has the technical problems of low extraction rate and high cost. Therefore, aiming at the technical problems, a process for extracting the litsea cubeba fatty oil is developed.
Disclosure of Invention
The invention aims to provide an extraction process of litsea pungens fatty oil. The method has the characteristics of high extraction rate and low cost.
The technical scheme of the invention is as follows: an extraction process of litsea pungens fatty oil comprises the following steps:
(1) pulverizing Litsea pungens to 10-80 mesh to obtain product A;
(2) adding the product A into a Soxhlet extractor, wherein the extraction solvent in the extraction tank is petroleum ether, and the mass ratio of the product A to the petroleum ether is 1: 4-12, extracting in water bath at 85-99 ℃ for 1.5-2.5h, and recovering solvent by reduced pressure volatilization to obtain fatty oil.
In the process for extracting the litsea cubeba fatty oil, in the step (1), litsea cubeba is crushed to 50-80 meshes.
In the process for extracting the litsea cubeba fatty oil, in the step (1), litsea cubeba is crushed to 80 meshes.
In the extraction process of the litsea cubeba fatty oil, in the step (2), the mass ratio of the product A to the petroleum ether is 1: 6-8.
In the extraction process of the litsea cubeba fatty oil, in the step (2), the mass ratio of the product A to the petroleum ether is 1: 7.
in the process for extracting the litsea cubeba fatty oil, in the step (2), water bath extraction is carried out at 85-95 ℃.
In the process for extracting the litsea cubeba fatty oil, in the step (2), the litsea cubeba fatty oil is extracted in a water bath at 90 ℃.
In the process for extracting the litsea cubeba fatty oil, in the step (2), the water bath extraction time is 2 hours.
Compared with the prior art, the invention has the following technical effects:
the optimal extraction process of the litsea cubeba fatty oil comprises the following steps: adding solvent 7.14 times, pulverizing, sieving with No. 5 sieve, extracting at 90.04 deg.C, with extraction rate of 51.23%, correcting for adding solvent 7 times, pulverizing, sieving with No. 5 sieve (80 mesh), and extracting at 90 deg.C; the method specifically comprises the following steps: (1) pulverizing Litsea pungens to 80 mesh to obtain product A; (2) adding the product A into a Soxhlet extractor, wherein the extraction solvent in the extraction tank is petroleum ether, and the mass ratio of the product A to the petroleum ether is 1: and 7, performing water bath extraction at 90 ℃, wherein the water bath extraction time is 2 hours, and recovering the solvent through reduced pressure volatilization to obtain the fatty oil. And through literature reference, no literature for optimizing the litsea cubeba fatty oil extraction process is found, and the method has the advantages of simplicity and high extraction rate for the first time.
1, the experiment proves that:
2 big fruit litsea cubeba fatty oil
2.1 materials practice and instrumentation
Large fruit Litsea pungens purchased in Rosen
JM.A 1002 electronic balance (Yuyao Jiming check weighing apparatus Co., Ltd., ultra-Zener apparatus Co., Ltd., Zhu City), RRH-A1000 type high-speed multifunctional pulverizer (the country in Shanghai, Vol. Co., Ltd.), DK-98-II electric heating thermostat water bath (Tess apparatus Co., Ltd., Tianjin City), RE-2000A rotary evaporator (Shanghai Yangrong biochemical apparatus Co., Ltd.), Soxhlet extraction apparatus, petroleum ether (boiling range, 60-90 deg.C.)
Fatty oil extraction rate ═ volatile oil volume/crude drug amount ×%%
2.2 optimization of the Litsea pungens fatty oil extraction Process
2.2.1 solvent screening
Crushing the litsea pungens to the corresponding granularity, precisely weighing 20g, respectively adding into 10 times of solvents of petroleum ether, chloroform, n-hexane and absolute ethyl alcohol, and extracting in water bath at 90 ℃ for 2 h. And recovering the solvent through reduced pressure volatilization to obtain the fatty oil.
2.2.2 additive amount
Crushing the litsea pungens to the corresponding granularity, precisely weighing 20g, respectively adding 12, 10, 8, 6 and 4 times of petroleum ether, and extracting in water bath at 90 ℃ for 2 h. And recovering the solvent through reduced pressure volatilization to obtain the fatty oil.
2.2.3 particle size of Material
Respectively pulverizing fructus Litseae pungentis, sieving with No. 1, No. 35 mesh sieve, No. 3 sieve and No. 5 sieve, precisely weighing 20g, adding 8 times of petroleum ether, and extracting in water bath at 90 deg.C for 2 hr. And recovering the solvent through reduced pressure volatilization to obtain the fatty oil.
2.2.4 extraction temperature
Pulverizing fructus Litseae pungentis respectively, sieving with No. 3 sieve, precisely weighing 20g, adding 8 times of petroleum ether, and extracting in water bath at 85 deg.C, 90 deg.C, 95 deg.C, and 99 deg.C for 2 hr. And recovering the solvent through reduced pressure volatilization to obtain the fatty oil.
2.2.5 extraction time
Crushing litsea pungens, sieving with No. 3 sieve, precisely weighing 20g, adding 8 times of petroleum ether, and extracting at 90 deg.C for 1.5 hr, 2 hr, and 2.5 hr respectively. And recovering the solvent through reduced pressure volatilization to obtain the fatty oil.
2.2.6 response surface design
On the basis of a single-factor experiment, the solvent adding amount (A), the material granularity (B) and the extraction temperature (C) are selected as 3 factors of Box-Behnken experiment design, a design scheme of 3 factors and 3 levels is adopted by combining the design principle of a response surface method, 17 groups of experiments are totally performed, and the factors and the levels of the response surface method experiment are shown in Table 1.
TABLE 1 level table of litsea cubeba fatty oil response surface
| Level of | Adding amount of solvent (A) | Granularity of material (B) | Temperature of extraction (C) |
| -1 | 6 | 35 |
85 |
| 0 | 8 | 3 | 90 |
| 1 | 10 | 5 | 95 |
2.3 results and discussion
2.3.1 solvent screening
As shown in figure 1, the petroleum ether is used for extracting the litsea cubeba fatty oil under the same extraction condition, the highest problem rate can be achieved, and the highest problem rate can reach 33.5%.
2.3.2 addition of solvent
As shown in fig. 2, under the same extraction conditions, the extraction rate of fatty oil tends to increase and decrease with the amount of solvent added, and at 8 times the amount of solvent, the extraction rate reaches a maximum of 29.74%.
2.2.3 particle size of Material
As shown in figure 3, under the same extraction conditions, the extraction rate of the fatty oil shows a remarkable increasing trend along with the increase of the crushed particle size, after the extraction rate is screened by a No. 5 screen, the extraction rate is 39.74 percent, the increasing trend is not reduced, but the viscosity of the material is gradually increased along with the increase of the particle size, and the screening is difficult.
2.2.4 extraction temperature
As shown in fig. 4, under the same extraction conditions, the extraction rate of the fatty oil showed a clear trend of increasing first and then decreasing with the increase of the extraction temperature, and the extraction rate was 45.77% with the highest extraction rate at 95 ℃.
2.2.5 extraction time
As shown in fig. 5, under the same extraction conditions, the extraction rate of the litsea cubeba fatty oil tends to increase first and then gradually decrease with the increase of the extraction time, and the extraction rate is highest at 37.34% when the extraction time is 2 hours.
2.2.6 response surface design
TABLE 2 Experimental design and results of the fatty oil response surface of litsea cubeba
Taking the solvent adding amount, the crushing degree and the extraction temperature as independent variables, taking the fatty oil extraction rate of the litsea pungens as dependent variables, adopting design-expert software to fit all the factors, and obtaining a quadratic regression equation, wherein the experimental design and the result of the response surface are shown in the table 2:
Y＝34.09-2.34A+16.0975B+2.745C-1.725AB+4.785AC-0.5BC-4.6525A2+0.1625B2-9.0175C2，
TABLE 3 big fruit litsea cubeba fatty oil response surface regression equation
| Sources of variance | Sum of squares | Degree of freedom | Mean square error | F value | P value | Significance of |
| Model (model) | 2736.49 | 9 | 304.05 | 17.8 | 0.0005 | Is remarkable in that |
| A-amount of solubilizer | 43.8 | 1 | 43.8 | 2.56 | 0.1533 | |
| B-particle size of Material | 2073.04 | 1 | 2073.04 | 121.37 | <0.0001 | Is extremely remarkable |
| C-extraction temperatureDegree of rotation | 60.28 | 1 | 60.28 | 3.53 | 0.1024 | |
| AB | 11.9 | 1 | 11.9 | 0.6969 | 0.4314 | |
| AC | 91.58 | 1 | 91.58 | 5.36 | 0.0537 | |
| |
1 | 1 | 1 | 0.0585 | 0.8157 | |
| A2 | 91.14 | 1 | 91.14 | 5.34 | 0.0542 | |
| B2 | 0.1112 | 1 | 0.1112 | 0.0065 | 0.938 | |
| C2 | 342.38 | 1 | 342.38 | 20.05 | 0.0029 | |
| Residual error | 119.56 | 7 | 17.08 | |||
| Difference of deviation from true to false | 83.88 | 3 | 27.96 | 3.13 | 0.1494 | Is not significant |
| Pure error | 35.69 | 4 | 8.92 | |||
| Total deviation of | 2856.05 | 16 |
From table 3 and a regression equation, the F value of the model is 17.8(P is less than 0.001), which indicates that the model has significance, the model has good fitting degree with the actual experiment, the relative error of the experiment is small, the relation between the solvent addition amount, the material granularity, the extraction temperature and the fatty oil extraction rate can be reflected, the F value of the mismatch is 3.13 which is more than 0.05, which indicates that the fitting degree of the experiment is good, and the sequence of the volatile oil extraction rate affecting the litsea cubeba can be known according to the values of the F value and the P value: the granularity of the material is more than the extraction temperature and more than the solvent adding amount, and the granularity of the material has very obvious influence on the extraction rate of the fatty oil.
The contour map and the three-dimensional map of the response surface can intuitively reflect the influence of two delivery factors on the extraction rate of the litsea cubeba fatty oil, the ellipse of the contour map shows that the two factors have a heavier influence on the experimental result, and if the contour map is rounder, the influence is smaller. From the figure, the solvent adding amount and the material granularity as well as the material granularity and the extraction temperature do not present a circle or an ellipse, the interaction effect is small or no effect, and the solvent adding amount and the extraction temperature present an ellipse, and the interaction effect is large. The a and c pictures show that the influence of the material granularity on the extraction of the litsea cubeba fatty oil is large, but the powder sieving difficulty is large, so that the extraction rate is not found to be the highest point, the three-dimensional picture shows an obvious trend, but the influence of the material granularity on the extraction rate of the litsea cubeba fatty oil is intuitively obvious.
The optimal extraction process of the litsea cubeba fatty oil analyzed by design-expert software comprises the following steps: the solvent adding amount is 7.14 times, the powder passes through a No. 5 sieve, the extraction temperature is 90.04 ℃, the extraction rate is 51.23 percent, the solvent adding amount is more than 7 times, the powder passes through the No. 5 sieve, and the extraction temperature is 90 ℃.
In conclusion, the method has the advantages of high extraction rate and low cost.
Drawings
FIG. 1 is a graph of the extraction rate of litsea pungens fatty oil (solvent screening) of the present invention;
FIG. 2 is a graph of the extraction rate of fat oil from Litsea pungens (amount of solvent) according to the present invention;
FIG. 3 is a graph of the extraction rate of litsea pungens fatty oil (material particle size) of the present invention;
FIG. 4 is a graph of the extraction rate (extraction temperature) of litsea pungens fatty oil of the present invention;
FIG. 5 is a graph of the extraction rate (extraction time) of the litsea pungens fatty oil of the present invention;
FIG. 6 is a contour plot of the amount of solvent added to litsea cubeba fatty oil and the particle size of the material according to the present invention;
FIG. 7 is a three-dimensional graph of the amount of solvent added to litsea cubeba fatty oil and the particle size of the material according to the present invention;
FIG. 8 is a line contour diagram of the solvent addition amount and extraction temperature of litsea pungens fatty oil of the present invention;
FIG. 9 is a three-dimensional plot of solvent loading and extraction temperature for litsea cubeba fatty oil of the present invention;
FIG. 10 is a line contour diagram of particle size and extraction temperature of litsea pungens fatty oil of the present invention;
FIG. 11 is a three-dimensional graph of particle size and extraction temperature of litsea cubeba fatty oil material of the present invention.
Detailed Description
The invention is further illustrated by the following figures and examples, which are not to be construed as limiting the invention.
Example 1: an extraction process of litsea pungens fatty oil comprises the following steps:
(1) pulverizing Litsea pungens to 10 mesh to obtain product A;
(2) adding the product A into a Soxhlet extractor, wherein the extraction solvent in the extraction tank is petroleum ether, and the mass ratio of the product A to the petroleum ether is 1: 4, extracting in water bath at 85 ℃ for 1.5h, and recovering the solvent through reduced pressure volatilization to obtain the fatty oil.
Example 2: an extraction process of litsea pungens fatty oil comprises the following steps:
(1) pulverizing Litsea pungens to 30 mesh to obtain product A;
(2) adding the product A into a Soxhlet extractor, wherein the extraction solvent in the extraction tank is petroleum ether, and the mass ratio of the product A to the petroleum ether is 1: and 6, performing water bath extraction at 90 ℃ for 2 hours, and recovering the solvent through reduced pressure volatilization to obtain the fatty oil.
Example 3: an extraction process of litsea pungens fatty oil comprises the following steps:
(1) pulverizing Litsea pungens to 50 mesh to obtain product A;
(2) adding the product A into a Soxhlet extractor, wherein the extraction solvent in the extraction tank is petroleum ether, and the mass ratio of the product A to the petroleum ether is 1: 8, performing water bath extraction at 95 ℃ for 2.5h, and recovering the solvent through reduced pressure volatilization to obtain the fatty oil.
Example 4: an extraction process of litsea pungens fatty oil comprises the following steps:
(1) pulverizing Litsea pungens to 80 mesh to obtain product A;
(2) adding the product A into a Soxhlet extractor, wherein the extraction solvent in the extraction tank is petroleum ether, and the mass ratio of the product A to the petroleum ether is 1: and 7, performing water bath extraction at 90 ℃ for 2h, and recovering the solvent through reduced pressure volatilization to obtain the fatty oil.
Example 5: an extraction process of litsea pungens fatty oil comprises the following steps:
(1) pulverizing Litsea pungens to 80 mesh to obtain product A;
(2) adding the product A into a Soxhlet extractor, wherein the extraction solvent in the extraction tank is petroleum ether, and the mass ratio of the product A to the petroleum ether is 1: 12, extracting in water bath at 99 ℃ for 2.5h, and recovering the solvent through reduced pressure volatilization to obtain the fatty oil.
Claims (8)
1. A process for extracting litsea cubeba fatty oil is characterized by comprising the following steps: the method comprises the following steps:
(1) pulverizing Litsea pungens to 10-80 mesh to obtain product A;
(2) adding the product A into a Soxhlet extractor, wherein the extraction solvent in the extraction tank is petroleum ether, and the mass ratio of the product A to the petroleum ether is 1: 4-12, extracting in water bath at 85-99 ℃ for 1.5-2.5h, and recovering solvent by reduced pressure volatilization to obtain fatty oil.
2. The extraction process of litsea cubeba fatty oil according to claim 1, characterized in that: in the step (1), the litsea cubeba are crushed to 50-80 meshes.
3. The extraction process of litsea pungens fatty oil according to claim 2, wherein: in the step (1), the litsea cubeba is crushed to 80 meshes.
4. The extraction process of litsea cubeba fatty oil according to claim 1, characterized in that: in the step (2), the mass ratio of the product A to the petroleum ether is 1: 6-8.
5. The extraction process of litsea pungens fatty oil according to claim 4, wherein: in the step (2), the mass ratio of the product A to the petroleum ether is 1: 7.
6. the extraction process of litsea cubeba fatty oil according to claim 1, characterized in that: in the step (2), water bath extraction is carried out at 85-95 ℃.
7. The extraction process of litsea pungens fatty oil according to claim 6, wherein: in the step (2), water bath extraction is performed at 90 ℃.
8. The extraction process of litsea cubeba fatty oil according to claim 1, characterized in that: in the step (2), the water bath extraction time is 2 h.
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| CN115420832A (en) * | 2022-09-20 | 2022-12-02 | 贵州医科大学 | GC-MS fingerprint spectrum and multi-index content determination method of litsea pungens oil |
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Application publication date: 20210205 |
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