CN112725063A - Subcritical tea seed oil extraction method - Google Patents
Subcritical tea seed oil extraction method Download PDFInfo
- Publication number
- CN112725063A CN112725063A CN202011427768.9A CN202011427768A CN112725063A CN 112725063 A CN112725063 A CN 112725063A CN 202011427768 A CN202011427768 A CN 202011427768A CN 112725063 A CN112725063 A CN 112725063A
- Authority
- CN
- China
- Prior art keywords
- tea seed
- extraction
- subcritical
- seed oil
- neutral protease
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000605 extraction Methods 0.000 title claims abstract description 85
- 239000010495 camellia oil Substances 0.000 title claims abstract description 45
- 241001122767 Theaceae Species 0.000 claims abstract description 68
- 239000000843 powder Substances 0.000 claims abstract description 33
- 108090000145 Bacillolysin Proteins 0.000 claims abstract description 27
- 102000035092 Neutral proteases Human genes 0.000 claims abstract description 27
- 108091005507 Neutral proteases Proteins 0.000 claims abstract description 27
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 239000006228 supernatant Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 15
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 239000011802 pulverized particle Substances 0.000 claims 1
- 238000010298 pulverizing process Methods 0.000 claims 1
- 150000002978 peroxides Chemical class 0.000 abstract description 6
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 239000010779 crude oil Substances 0.000 description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 23
- 239000003921 oil Substances 0.000 description 16
- 235000019198 oils Nutrition 0.000 description 16
- 238000000227 grinding Methods 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 102000035195 Peptidases Human genes 0.000 description 6
- 108091005804 Peptidases Proteins 0.000 description 6
- 239000004365 Protease Substances 0.000 description 6
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 239000003755 preservative agent Substances 0.000 description 5
- 230000002335 preservative effect Effects 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- 102000004190 Enzymes Human genes 0.000 description 4
- 108090000790 Enzymes Proteins 0.000 description 4
- 238000005119 centrifugation Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 3
- 239000005642 Oleic acid Substances 0.000 description 3
- 235000021314 Palmitic acid Nutrition 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 2
- LRFDUPNLCDXZOE-UHFFFAOYSA-N camellianin b Chemical compound OC1C(O)C(O)C(C)OC1OC1C(O)C(O)C(OC=2C=3C(=O)C=C(OC=3C=C(O)C=2)C=2C=CC(O)=CC=2)OC1CO LRFDUPNLCDXZOE-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 235000008390 olive oil Nutrition 0.000 description 2
- 239000004006 olive oil Substances 0.000 description 2
- SECPZKHBENQXJG-FPLPWBNLSA-N palmitoleic acid Chemical compound CCCCCC\C=C/CCCCCCCC(O)=O SECPZKHBENQXJG-FPLPWBNLSA-N 0.000 description 2
- 238000005502 peroxidation Methods 0.000 description 2
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 description 1
- MPDGHEJMBKOTSU-YKLVYJNSSA-N 18beta-glycyrrhetic acid Chemical compound C([C@H]1C2=CC(=O)[C@H]34)[C@@](C)(C(O)=O)CC[C@]1(C)CC[C@@]2(C)[C@]4(C)CC[C@@H]1[C@]3(C)CC[C@H](O)C1(C)C MPDGHEJMBKOTSU-YKLVYJNSSA-N 0.000 description 1
- 206010003210 Arteriosclerosis Diseases 0.000 description 1
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 1
- 235000021319 Palmitoleic acid Nutrition 0.000 description 1
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 1
- 208000011775 arteriosclerosis disease Diseases 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- SECPZKHBENQXJG-UHFFFAOYSA-N cis-palmitoleic acid Natural products CCCCCCC=CCCCCCCCC(O)=O SECPZKHBENQXJG-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 235000019197 fats Nutrition 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 235000020778 linoleic acid Nutrition 0.000 description 1
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 1
- 229960004488 linolenic acid Drugs 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229960005141 piperazine Drugs 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/025—Pretreatment by enzymes or microorganisms, living or dead
-
- 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
-
- 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
- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
Abstract
The invention discloses a subcritical tea seed oil extraction method, which comprises the following steps: (1) crushing a tea seed raw material to obtain tea seed powder; (2) heating tea seed powder, or adding neutral protease or aqueous solution of neutral protease into tea seed powder, and heating to obtain subcritical extraction raw material of tea seed; (3) mixing the material obtained in the step (2) with a subcritical extracting solution, and performing subcritical extraction to obtain tea seed oil; (4) and (3) centrifugally separating the tea seed oil, and taking supernatant to obtain the subcritical extracted tea seed oil. According to the invention, neutral protease or the aqueous solution thereof is added into the tea seeds, the tea seeds are heated, the subcritical extraction rate of the tea seed oil can be effectively improved, the neutral protease is added, the peroxide value in the tea seed oil can be effectively reduced, and the n-butane serving as an extraction solvent can be recycled, so that the method is very suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of tea seed oil extraction, and particularly relates to a subcritical tea seed oil extraction method.
Background
Tea seeds, called 'east olive oil', are a peculiar species in China, have unsaturated fatty acids of more than 90 percent, oleic acid of 80-83 percent, linoleic acid of 7-13 percent and palmitic acid of 8-10 percent, and contain specific physiological active substances which are not contained in the olive oil, such as camellin, tea polyphenol and the like, have the oxidation resistance, and can reduce blood pressure, blood fat and arteriosclerosis. The current tea seed oil extraction methods commonly used in industry mainly comprise a squeezing method, a leaching method and an organic solvent extraction method, and the application of a subcritical extraction method is not wide.
Subcritical extraction is a novel extraction and separation technology which utilizes subcritical fluid as an extractant, transfers fat-soluble components in solid materials to a liquid extractant through a molecular diffusion process of the extraction materials and the extractant in a soaking process in a closed, oxygen-free and low-pressure container according to the principle that organic matters are similar, and separates the extractant from a target product through a reduced pressure evaporation process to finally obtain the target product. The tea seed oil obtained by subcritical extraction is non-toxic and harmless, is environment-friendly, is pollution-free, is not subjected to thermal processing, keeps the active ingredients of the extract, is not damaged or oxidized, has high capacity, can be industrially produced in a large scale, is energy-saving, has low operation cost, is easy to separate from the product, and can not reach an ideal index on the extraction efficiency.
Disclosure of Invention
The invention aims to make up for the defects of the prior art and provides a subcritical tea seed oil extraction method to improve the extraction efficiency of the conventional subcritical tea seed oil extraction method.
In order to achieve the above object, the present invention provides the following technical solutions:
a subcritical tea seed oil extraction method comprises the following steps:
(1) crushing a tea seed raw material to obtain tea seed powder;
(2) heating tea seed powder, or adding neutral protease or aqueous solution of neutral protease into tea seed powder, and heating to obtain subcritical extraction raw material of tea seed;
(3) mixing the material obtained in the step (2) with a subcritical extracting solution, and performing subcritical extraction to obtain tea seed oil;
(4) and (3) centrifugally separating the tea seed oil, and taking supernatant to obtain the subcritical extracted tea seed oil.
Further, the temperature of the crushing treatment in the step 1 is 25-28 ℃, the size of the crushed particles is 20-120 meshes, preferably, the size of the crushed particles is 20-60 meshes, and more preferably, 20-40 meshes.
Further, in the step 2, the heating temperature is 40-80 ℃ and the time is not more than 2 hours, preferably, the heating temperature is 50-70 ℃ and the time is 1-1.5 hours, and more preferably, the heating temperature is 50 ℃ and the time is 1 hour.
Further, neutral protease is added in the step 2, and the addition amount is more than 0 and less than or equal to 4 percent by mass.
Further, the step 2 is to add the water solution of neutral protease, and the addition amount of the water solution of neutral protease is more than 0% and less than or equal to 4% by mass percent.
Preferably, the adding amount of the neutral protease is more than 0 and less than or equal to 2 percent by mass percent, and the adding amount of the aqueous solution of the neutral protease is more than 0 and less than or equal to 2 percent by mass percent.
More preferably, the adding amount of the neutral protease is more than 0 and less than or equal to 1 percent by mass percent, and the adding amount of the aqueous solution of the neutral protease is more than 0 and less than or equal to 1 percent by mass percent.
Further, in the step 3, the subcritical extracting solution is n-butane, and the mass-to-volume ratio of the raw material for subcritical extraction of the tea seeds to the n-butane is 1: (0.05-0.25) g/L, subcritical extraction temperature in extraction process is 40 deg.C, vacuum concentration temperature is 30-50 deg.C, extraction time is 20-60min, and extraction pressure is 0.1 MPa.
Preferably, the mass-to-volume ratio of the raw material for subcritical extraction of tea seeds to n-butane is 1: 0.25g/L, subcritical extraction temperature of 40 deg.C, vacuum concentration temperature of 40 deg.C, extraction time of 30-40min, preferably 30min, and extraction pressure of 0.1 MPa.
Further, the centrifugation conditions in the step 4 are as follows: the rotation speed is not less than 5000r/min, preferably 10000r/min, and the centrifugation time is 5 min.
Furthermore, the extraction rate of the obtained tea seed oil reaches 25-34%, the tea seed oil contains 8-10% of palmitic acid and 80-85% of oleic acid, and the peroxide value is (0.06-0.12) g/100 g.
The inventor surprisingly discovers that by carrying out preheating treatment on tea seeds, the tissue structure of the tea seeds can be damaged through thermal reaction, and the oil yield of the tea seeds can be improved; by directly adding neutral protease to treat the tea seed sample, the oil yield of the tea seeds can be improved, and the peroxide value of the tea seed oil is obviously reduced; by adding neutral protease aqueous solution to treat a tea seed sample, drying treatment is carried out after reaction, so that the extraction rate of tea seed oil in a sub-critical way can be increased.
The invention has the advantages that:
1. the oil yield of the tea seed oil extracted by the invention can reach 118.1%, and the extract contains 8.06% of palmitic acid, 1.66% of stearic acid, 81.8% of oleic acid, 7.66% of linoleic acid, 0.065% of palmitoleic acid, 0.0504% of methyl heptadecacarbonate, 0.0536% of cis-10-methyl heptadecaenoate, 0.624% of alpha-linolenic acid and 0.0517% of cis-15-methyl tetracosanenoate. According to the invention, the peroxidation value of the tea seed oil of the tea seed sample subjected to heating treatment after the neutral protease is added is reduced to 0.069g/100g from 0.12g/100g of a control group, so that the oxidation degree of the grease is obviously reduced.
2. The oil yield of the tea seed oil can be obviously improved by the neutral protease and the heating treatment process, and the oil yield is increased from 97.2% to 118.1% of a control group.
3. According to the invention, neutral protease or the aqueous solution thereof is added into the tea seeds, the tea seeds are heated, the subcritical extraction rate of the tea seed oil can be effectively improved, the neutral protease is added, the peroxide value in the tea seed oil can be effectively reduced, and the n-butane serving as an extraction solvent can be recycled, so that the method is very suitable for industrial production.
Detailed Description
The technical scheme of the invention is further explained by combining the specific examples as follows:
the examples use raw materials and equipment:
tea seed: the oil content of tea seed kernels detected by the national standard method (GB/T5512-85) of Changlin series tea seeds provided by the great-block agriculture shares Co., Ltd, Liuan City, Anhui province is 48%, namely the average oil content in the obtained 20g of tea seed test products is 5.76 g.
A constant-temperature water bath kettle: jintan jie jerry electrical limited, model: HH-2 digital display constant temperature water bath.
Subcritical extraction equipment: critical biotechnology limited in south river asia, type: CBE-5L.
A centrifuge: saimer Feishale science and technology (China) Inc., model number Multifuge X1.
Example 1
(1) Grinding tea seeds into powder (20 meshes), taking 20g of tea seed powder and 0.1g of protease, uniformly mixing, and placing in a beaker;
(2) performing subcritical extraction with n-butane as extraction medium for 30min, and desolventizing to desolventizing pressure below 0.1MPa to obtain crude oil;
(3) placing the crude oil in a centrifuge tube, and centrifuging at 10000r/min for 5min to obtain crude oil supernatant;
(4) weighing the crude oil supernatant, and recording data;
the oil yield of the obtained tea seeds is 5.8g, the extraction rate is 29 percent,
example 2
(1) Grinding tea seeds into powder (20 meshes), taking 20g of tea seed powder and 0.15g of protease, uniformly mixing, and placing in a beaker;
(2) performing subcritical extraction with n-butane as extraction medium for 30min, and desolventizing to desolventizing pressure below 0.1MPa to obtain crude oil;
(3) placing the crude oil in a centrifuge tube, and centrifuging at 10000r/min for 5min to obtain crude oil supernatant;
(4) weighing the crude oil supernatant, and recording data;
the obtained tea seed has oil yield of 6.0g and extraction rate of 30%,
example 3
(1) Grinding tea seeds into powder of 20 meshes), putting 20g of tea seed powder into a beaker, and sealing the beaker by using a preservative film;
(2) putting the beaker into a water bath at 50 ℃, and heating for 30 min;
(3) recovering the tea seed powder to room temperature, performing subcritical extraction with n-butane as extraction medium for 30min, and desolventizing to desolventizing pressure below 0.1MPa to obtain crude oil;
(4) after extraction, placing the crude oil in a centrifuge tube, and carrying out centrifugation treatment for 5min at a rotation speed of 10000r/min to obtain crude oil supernatant;
(5) weighing the crude oil supernatant, and recording data;
the obtained tea seed has oil yield of 6.5g and extraction rate of 32.5%,
example 4
(1) Grinding tea seeds into powder (20 meshes), putting 20g of tea seed powder into a beaker, and sealing the beaker by using a preservative film;
(2) putting the beaker into a water bath at 50 ℃, and heating for 60 min;
(3) recovering the tea seed powder to room temperature, performing subcritical extraction with n-butane as extraction medium for 30min, and desolventizing to desolventizing pressure below 0.1MPa to obtain crude oil;
(4) placing the crude oil in a centrifuge tube for centrifuging at a rotation speed of 10000r/min for 5min to obtain crude oil supernatant;
(5) weighing the crude oil supernatant, and recording data;
the obtained tea seed has oil yield of 6.8g and extraction rate of 34%,
example 5
(1) Grinding tea seeds into powder (20 meshes), uniformly mixing 20g of tea seed powder and 0.1g of protease, placing the mixture into a beaker, and sealing the beaker by using a preservative film;
(2) putting the beaker into a water bath at 50 ℃, and heating for 60 min;
(3) recovering the tea seed powder to room temperature, performing subcritical extraction with n-butane as extraction medium for 30min, and desolventizing to desolventizing pressure below 0.1MPa to obtain crude oil;
(4) after extraction, placing the crude oil in a centrifuge tube, and carrying out centrifugation treatment for 5min at a rotation speed of 10000r/min to obtain crude oil supernatant;
(5) weighing the crude oil supernatant, and recording data;
obtained byThe oil yield of the tea seeds is 6.8g, the extraction rate is 34 percent,
example 6
(1) Grinding tea seeds into powder (20 meshes), taking 20g of tea seed powder, mixing 0.1g of protease and 4mL of distilled water in a centrifuge tube to obtain a mixed solution, placing the tea seed powder in a beaker, and sealing the beaker by using a preservative film;
(2) putting the beaker and the centrifuge tube into a water bath at 50 ℃, and heating for 60min in the water bath;
(3) mixing the mixed solution with tea seed powder, placing into water bath, and heating in water bath for 60 min;
(4) placing the mixture after the water bath into a plate, flattening, and placing the plate into a drying oven for drying at 50 ℃ for 1.5 h;
(5) recovering the tea seed powder to room temperature, performing subcritical extraction with n-butane as extraction medium for 30min, and desolventizing to desolventizing pressure below 0.1MPa to obtain crude oil;
(6) and after extraction, placing the crude oil in a centrifuge tube for centrifugal treatment. Centrifuging for 5min at 10000r/min to obtain crude oil supernatant;
(7) weighing the crude oil supernatant, and recording data;
the obtained tea seed has oil yield of 5.5g and extraction rate of 27.5%,
example 7
(1) Grinding tea seeds into powder (20 meshes), taking 20g of tea seed powder, mixing 0.1g of protease and 4ml of distilled water in a centrifugal tube to obtain a mixed solution, placing the tea seed powder in a beaker, and sealing the beaker by using a preservative film;
(2) preheating a water bath kettle, putting a beaker and a centrifuge tube into the water bath kettle when the temperature reaches about 50 ℃, and heating in a water bath for 60 min;
(3) mixing the mixed solution with tea seed powder, placing into water bath, and heating in water bath for 120 min;
(4) placing the mixture after the water bath into a plate, flattening, and placing the plate into a drying oven for drying for 1 h;
(5) recovering the tea seed powder to room temperature, performing subcritical extraction with n-butane as extraction medium for 30min, and desolventizing to desolventizing pressure below 0.1 MPa;
(6) and after extraction, placing the crude oil in a centrifuge tube for centrifugal treatment. Centrifuging for 5min at 10000r/min to obtain crude oil supernatant;
(7) weighing the tea seed oil, and recording data;
the obtained tea seed has oil yield of 5.9g, extraction rate of 29.5%,
comparative example
The comparative example is similar to example 1 except that, without the enzyme addition or heating process described in step (1), the tea seed powder at room temperature was directly subjected to the subcritical extraction of step (2), and the extraction rate of tea seeds was 28% and the oil yield was 97.2%.
The crude oil supernatants of examples 5 and 7 and comparative example above were subjected to peroxide number measurements, respectively: 0.069g/100g, 0.12g/100g, 0.12g/100 g. The result shows that the peroxidation of the tea seed oil can be effectively reduced by singly adding the enzyme to treat the tea seeds, the oxidation degree of fatty acid in the oil is reduced, and the quality of the tea seed oil is effectively improved. The peroxide value of the tea seed oil obtained by adding water and adding enzyme is the same as that of the tea seed oil obtained by adding water and adding enzyme, probably because the action of protease is counteracted by adding water, and the specific mechanism needs to be further discussed.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The subcritical tea seed oil extraction method is characterized by comprising the following steps of:
(1) crushing a tea seed raw material to obtain tea seed powder;
(2) heating tea seed powder, or adding neutral protease or aqueous solution of neutral protease into tea seed powder, and heating to obtain subcritical extraction raw material of tea seed;
(3) mixing the material obtained in the step (2) with a subcritical extracting solution, and performing subcritical extraction to obtain tea seed oil;
(4) and (3) centrifugally separating the tea seed oil, and taking supernatant to obtain the subcritical extracted tea seed oil.
2. The subcritical tea seed oil extraction method according to claim 1, wherein the temperature for the pulverization treatment in the step 1 is 25-28 ℃, and the size of the pulverized particles is 20-120 meshes.
3. The method for subcritical extraction of tea seed oil according to claim 2, wherein the size of the crushed particles is 20-60 mesh.
4. The method for subcritical extraction of tea seed oil according to claim 1, wherein the heating temperature in the step 2 is 40-80 ℃ and the time is not more than 2 hours.
5. The method for subcritical extraction of tea seed oil according to claim 4, wherein the heating temperature is 50-70 ℃ and the time is 1-1.5 hours.
6. The subcritical tea seed oil extraction method according to claim 1, wherein neutral protease is added in the step 2, and the addition amount is more than 0 and less than or equal to 4% by mass.
7. The method for subcritical extraction of tea seed oil according to claim 1, wherein the aqueous solution of neutral protease is added in the step 2, and the addition amount is more than 0% and less than or equal to 4% by mass.
8. The method for subcritical extraction of tea seed oil according to claim 6 or 7, characterized in that the addition amount of neutral protease is 0 < neutral protease.ltoreq.2% by mass, and the addition amount of the aqueous solution of neutral protease is 0 < neutral protease.ltoreq.2% by mass.
9. The method for subcritical extraction of tea seed oil according to claim 1, wherein the subcritical extraction liquid in the step 3 is n-butane, and the mass-to-volume ratio of the raw material for subcritical extraction of tea seed to n-butane is 1: (0.05-0.25) g/L, subcritical extraction temperature in extraction process is 40 deg.C, vacuum concentration temperature is 30-50 deg.C, extraction time is 20-60min, and extraction pressure is 0.1 MPa.
10. The method for subcritical extraction of tea seed oil according to claim 9, wherein the mass volume ratio of the raw material for subcritical extraction of tea seed to n-butane is 1: 0.25g/L, subcritical extraction temperature of 40 deg.C, vacuum concentration temperature of 40 deg.C, extraction time of 30-40min, and extraction pressure of 0.1 MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011427768.9A CN112725063A (en) | 2020-12-07 | 2020-12-07 | Subcritical tea seed oil extraction method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011427768.9A CN112725063A (en) | 2020-12-07 | 2020-12-07 | Subcritical tea seed oil extraction method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112725063A true CN112725063A (en) | 2021-04-30 |
Family
ID=75598573
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011427768.9A Pending CN112725063A (en) | 2020-12-07 | 2020-12-07 | Subcritical tea seed oil extraction method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112725063A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106147989A (en) * | 2016-08-01 | 2016-11-23 | 岳西县光圣茶油有限公司 | Semen Persicae supplementing the brain Oleum Camelliae subcritical abstraction technique |
| CN106350202A (en) * | 2016-08-31 | 2017-01-25 | 安徽省康龙农业开发有限公司 | Method for performing subcritical fluid extraction on tea seed oil |
| CN106675769A (en) * | 2017-02-28 | 2017-05-17 | 上海时迅农业科技发展有限公司 | Method for extracting vegetable oil under subcritical low temperature |
-
2020
- 2020-12-07 CN CN202011427768.9A patent/CN112725063A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106147989A (en) * | 2016-08-01 | 2016-11-23 | 岳西县光圣茶油有限公司 | Semen Persicae supplementing the brain Oleum Camelliae subcritical abstraction technique |
| CN106350202A (en) * | 2016-08-31 | 2017-01-25 | 安徽省康龙农业开发有限公司 | Method for performing subcritical fluid extraction on tea seed oil |
| CN106675769A (en) * | 2017-02-28 | 2017-05-17 | 上海时迅农业科技发展有限公司 | Method for extracting vegetable oil under subcritical low temperature |
Non-Patent Citations (2)
| Title |
|---|
| 《贵州油茶》: "《贵州油茶》", 30 June 2016, 贵州科学技术出版社 * |
| 何秀芬主编, 中国农业大学出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103045356B (en) | Production method for linseed oil | |
| CN101020917A (en) | Process of preparing lutein with marigold | |
| CN107858197A (en) | A kind of production and processing method of low acid value high-quality edible oil tea-seed oil | |
| CN106810620B (en) | A kind of gingko episperm pectin extraction method | |
| CN105238551A (en) | Method for supercritical CO2 extraction and purification of camellia seed oil | |
| CN107573317A (en) | A kind of extracting method of blueberry anthocyanin | |
| CN103087828A (en) | Yunnan black tea essential oil and preparation method thereof | |
| CN106146681B (en) | A kind of method of low temperature continuous phase transistion extraction sea grass polysaccharide | |
| CN111588758A (en) | Extraction method of rose extract | |
| CN107788325A (en) | A kind of safety and environmental protection food preservative and preparation method thereof | |
| Santos et al. | Conventional and emerging techniques for extraction of bioactive compounds from fruit waste | |
| JP6557102B2 (en) | Method for producing polyisoprene | |
| CN1285152A (en) | High-active tawny agent and productive method thereof | |
| CN108929770A (en) | A method of utilizing enzyme assisted extraction soybean grease | |
| CN109054992A (en) | A method of extracting Seabuckthorm Seed Oil | |
| CN112725063A (en) | Subcritical tea seed oil extraction method | |
| CN106065036B (en) | A kind of method of hydro-thermal method extraction tea polysaccharide | |
| CN107125371A (en) | A kind of tealeaves high efficiency extraction and the technique utilized | |
| CN104327943A (en) | Method for extracting antrodia camphorata oil from antrodia camphorata sporophore | |
| CN111960981B (en) | Preparation method of lutein extract with good smell | |
| CN108117558B (en) | Method for separating teddenox A and teddenox B from fermented tea | |
| CN105622353B (en) | The method of supercritical carbon dioxide extracting strand Ka Kele aldehydes matters | |
| CN107349430B (en) | Phyllanthus emblica polysaccharide-EGCG compound and preparation method thereof | |
| CN112898444A (en) | Method for preparing muramyl polysaccharide by using ganoderma lucidum spore powder raffinate, product and application thereof | |
| CN112226281A (en) | Method for combined extraction of essential oil, flavone, pectin and cellulose from citrus peel |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210430 |
|
| RJ01 | Rejection of invention patent application after publication |