CN118725957A - Extraction and refining method of idesia fruit grease - Google Patents
Extraction and refining method of idesia fruit grease Download PDFInfo
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- CN118725957A CN118725957A CN202410878841.6A CN202410878841A CN118725957A CN 118725957 A CN118725957 A CN 118725957A CN 202410878841 A CN202410878841 A CN 202410878841A CN 118725957 A CN118725957 A CN 118725957A
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- 241001299699 Idesia Species 0.000 title claims abstract description 193
- 235000013399 edible fruits Nutrition 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000000605 extraction Methods 0.000 title claims abstract description 26
- 238000007670 refining Methods 0.000 title claims abstract description 24
- 239000004519 grease Substances 0.000 title claims abstract description 15
- 239000003921 oil Substances 0.000 claims abstract description 166
- 239000010779 crude oil Substances 0.000 claims abstract description 41
- 239000006228 supernatant Substances 0.000 claims abstract description 34
- 239000007788 liquid Substances 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 25
- 239000000839 emulsion Substances 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 21
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- 238000000926 separation method Methods 0.000 claims abstract description 16
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- 238000001035 drying Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 238000010438 heat treatment Methods 0.000 claims description 22
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- 238000005406 washing Methods 0.000 claims description 7
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- 238000006243 chemical reaction Methods 0.000 claims description 5
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- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 2
- 239000005642 Oleic acid Substances 0.000 description 2
- 238000000944 Soxhlet extraction Methods 0.000 description 2
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 2
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- YYGNTYWPHWGJRM-UHFFFAOYSA-N (6E,10E,14E,18E)-2,6,10,15,19,23-hexamethyltetracosa-2,6,10,14,18,22-hexaene Chemical compound CC(C)=CCCC(C)=CCCC(C)=CCCC=C(C)CCC=C(C)CCC=C(C)C YYGNTYWPHWGJRM-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
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- 244000241235 Citrullus lanatus Species 0.000 description 1
- 235000012828 Citrullus lanatus var citroides Nutrition 0.000 description 1
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- 241001048891 Jatropha curcas Species 0.000 description 1
- 235000019483 Peanut oil Nutrition 0.000 description 1
- 235000019484 Rapeseed oil Nutrition 0.000 description 1
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 229930182558 Sterol Natural products 0.000 description 1
- BHEOSNUKNHRBNM-UHFFFAOYSA-N Tetramethylsqualene Natural products CC(=C)C(C)CCC(=C)C(C)CCC(C)=CCCC=C(C)CCC(C)C(=C)CCC(C)C(C)=C BHEOSNUKNHRBNM-UHFFFAOYSA-N 0.000 description 1
- 229930003427 Vitamin E Natural products 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
- 229940076810 beta sitosterol Drugs 0.000 description 1
- LGJMUZUPVCAVPU-UHFFFAOYSA-N beta-Sitostanol Natural products C1CC2CC(O)CCC2(C)C2C1C1CCC(C(C)CCC(CC)C(C)C)C1(C)CC2 LGJMUZUPVCAVPU-UHFFFAOYSA-N 0.000 description 1
- NJKOMDUNNDKEAI-UHFFFAOYSA-N beta-sitosterol Natural products CCC(CCC(C)C1CCC2(C)C3CC=C4CC(O)CCC4C3CCC12C)C(C)C NJKOMDUNNDKEAI-UHFFFAOYSA-N 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
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- 238000001514 detection method Methods 0.000 description 1
- PRAKJMSDJKAYCZ-UHFFFAOYSA-N dodecahydrosqualene Natural products CC(C)CCCC(C)CCCC(C)CCCCC(C)CCCC(C)CCCC(C)C PRAKJMSDJKAYCZ-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
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- 235000019197 fats Nutrition 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
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- 229910052740 iodine Inorganic materials 0.000 description 1
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- 239000004006 olive oil Substances 0.000 description 1
- 235000008390 olive oil Nutrition 0.000 description 1
- 239000000312 peanut oil Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- CASUWPDYGGAUQV-UHFFFAOYSA-M potassium;methanol;hydroxide Chemical compound [OH-].[K+].OC CASUWPDYGGAUQV-UHFFFAOYSA-M 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000005713 safflower oil Nutrition 0.000 description 1
- 239000003813 safflower oil Substances 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 239000008159 sesame oil Substances 0.000 description 1
- 235000011803 sesame oil Nutrition 0.000 description 1
- KZJWDPNRJALLNS-VJSFXXLFSA-N sitosterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CC[C@@H](CC)C(C)C)[C@@]1(C)CC2 KZJWDPNRJALLNS-VJSFXXLFSA-N 0.000 description 1
- 229950005143 sitosterol Drugs 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229940031439 squalene Drugs 0.000 description 1
- TUHBEKDERLKLEC-UHFFFAOYSA-N squalene Natural products CC(=CCCC(=CCCC(=CCCC=C(/C)CCC=C(/C)CC=C(C)C)C)C)C TUHBEKDERLKLEC-UHFFFAOYSA-N 0.000 description 1
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- 238000002604 ultrasonography Methods 0.000 description 1
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- 235000019165 vitamin E Nutrition 0.000 description 1
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- 229940046009 vitamin E Drugs 0.000 description 1
- QUEDXNHFTDJVIY-UHFFFAOYSA-N γ-tocopherol Chemical class OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1 QUEDXNHFTDJVIY-UHFFFAOYSA-N 0.000 description 1
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- Fats And Perfumes (AREA)
Abstract
The invention provides an extraction and refining method of idesia fruit grease, belonging to the technical field of vegetable oil extraction and preparation. The method comprises the following steps: (1) Drying idesia fruits and crushing to obtain idesia fruit powder; (2) Mixing idesia fruit powder with an enzyme solution, carrying out enzymolysis, and carrying out solid-liquid separation after the enzymolysis is finished to obtain supernatant oil and an emulsion layer; (3) Demulsification and solid-liquid separation are carried out on the emulsion layer, and an upper layer oil layer and the supernatant oil are combined to obtain idesia polycarpa crude oil; (4) Sequentially degumming, deacidifying, decoloring and deodorizing the idesia polycarpa crude oil to obtain idesia primary refined oil. The invention provides a novel idesia oil preparation process, which solves the problems of heavy oil gas taste and easy deterioration of idesia to generate harbour taste, and the refined idesia oil is light in color, strong in fluidity, light in plant fragrance and free from harbour taste when stored at normal temperature.
Description
Technical Field
The invention relates to the technical field of vegetable oil extraction and preparation, in particular to an extraction and refining method of idesia fruit grease.
Background
Idesia is a plant of the family Hydnocarpus, which is a deciduous tree, also called as oil grape, water melon, jatropha curcas, etc., and is a dual-purpose tree species for oil materials. Idesia is often referred to as an "oil depot on tree" where the weight of pulp is 62.3% of the total weight and the weight of seeds is 36.7% of the total weight. Researches show that the oil content of idesia fruits is 36.71%, the fatty acid in idesia takes oleic acid, linoleic acid and the like as main components, the content of unsaturated fatty acid in oil reaches 68% -75%, and the content of linoleic acid in seed oil reaches 78%. The idesia oil has the linoleic acid content remarkably higher than that of olive oil, peanut oil, rapeseed oil, sesame oil, safflower oil and the like, has excellent health care effects of reducing blood fat, softening blood vessels and the like, has good immunity and oxidation resistance, and contains very rich natural active substances, wherein the content of beta-sitosterol reaches 28.15 percent by taking homologs of sterols and tocopherols as main components. Therefore, idesia can be applied to industries such as medicines, industrial oil, fertilizers, cosmetics and the like based on the excellent effect of idesia.
The majority of the fatty acids in idesia are in a combined state, and due to the characteristic of the fatty acids in idesia, the extraction of idesia oil by adopting a squeezing method and an organic solution leaching method has a certain problem. The common squeezing method can not completely break the cell wall of idesia polycarpa and release fatty acid; the organic solution leaching method is easy to produce organic reagent residues, thereby affecting the quality of idesia oil. Therefore, the invention tries to extract idesia oil by adopting a water enzyme method, and solves the technical problems of low extraction rate and large solvent residue in the traditional idesia oil preparation method.
Disclosure of Invention
The invention aims to provide an extraction and refining method for idesia fruit grease, which can extract grease in idesia fruits and refine crude oil, and the obtained idesia first-grade refined oil has high quality, clear color and luster, good fluidity and light plant fragrance.
In order to achieve the above object, the present invention provides the following technical solutions:
The invention provides a idesia fruit grease extraction and refining method which is characterized by comprising the following steps:
(1) Drying idesia fruits and crushing to obtain idesia fruit powder;
(2) Mixing idesia fruit powder with water, adding enzyme for enzymolysis, and performing solid-liquid separation after enzymolysis to obtain supernatant oil and emulsion layer;
(3) Demulsification and solid-liquid separation are carried out on the emulsion layer, and an upper layer oil layer and the supernatant oil are combined to obtain idesia polycarpa crude oil;
(4) Sequentially degumming, deacidifying, decoloring and deodorizing the idesia polycarpa crude oil to obtain idesia primary refined oil.
Preferably, in the step (2), the feed liquid ratio of idesia polycarpa fruit powder to water is 1g: 4.5-5.5 mL, and regulating the pH value to 4-5 after mixing;
The enzyme is pectase, the enzyme activity is 50u/mg, and the addition amount is 2-3%; the enzymolysis time is 4-5 h, and the temperature is 40-60 ℃.
Preferably, in the step (3), the demulsification is performed on the emulsion layer for 0.4-0.6 h, and the power of the ultrasound is 110-130W.
Preferably, the solid-liquid separation in the steps (2) and (3) is performed by centrifugation, wherein the rotation speed of the centrifugation is 4000-5000 r/min, and the time is 15-25 min.
Preferably, in the step (4), water with the temperature of 85-95 ℃ is added into idesia polycarpa crude oil with the temperature of 45-50 ℃ and then a degumming agent is added for reaction for 30-40 min, solid-liquid separation is carried out, and supernatant oil is taken to obtain idesia polycarpa degummed oil;
the addition amount of the water is 8-12% of the mass of the idesia polycarpa crude oil;
The degumming agent is obtained by mixing 0.12-0.13 mol/L EDTA-2Na solution and 0.05-0.07 mol/L SDS according to the volume ratio of 1.5-2.5:0.8-1.2;
the solid-liquid separation mode is centrifugation, the rotation speed of the centrifugation is 7500-8500 rpm, and the time is 5-15 min;
The degumming is carried out by adopting a degumming kettle, a stirring device is arranged in the degumming kettle, and the introduced idesia polycarpa crude oil and the degumming agent are mixed and stirred by the stirring device.
Preferably, in the step (4), sodium hydroxide solution is added into idesia polycarpa degummed oil at 35-45 ℃ to react for 35-45 min, standing and solid-liquid separation are carried out, and the supernatant oil is taken to be washed and dehydrated to obtain idesia polycarpa deacidified oil;
the concentration of the sodium hydroxide solution is 0.10-0.20 g/mL, and the addition amount is 8-12% of the mass of the idesia polycarpa degummed oil; adding the sodium hydroxide solution, and then adding excessive alkali with the quality of 0.20-0.30% of idesia degumming oil; the excessive alkali still adopts sodium hydroxide solution with the concentration of 0.10-0.20 g/mL;
the solid-liquid separation mode is centrifugation, the rotation speed of the centrifugation is 4500-5000 r/min, and the time is 15-25 min;
The water washing is to add water with the temperature of 55-65 ℃ accounting for 15-20% of the mass of the idesia polycarpa degummed oil, and react for 1h; the dehydration is carried out under vacuum, the vacuum degree is 0.08-0.09 MPa, and the time is 3-4 hours;
the washing is performed in a cleaning kettle, a heating device and a stirring device are arranged in the cleaning kettle, the oil temperature and the water temperature are kept by the heating device, and the oil and the hot water are fully and uniformly mixed by the stirring device;
The dehydration is carried out in a steam tank, and the water in the idesia oil is evaporated to obtain the high-quality idesia deacidification oil.
Preferably, in the step (4), activated clay is added into idesia polycarpa deacidified oil at the temperature of 85-95 ℃, the mixture is heated for reaction for 0.5-1 h, cooled to the temperature of 65-75 ℃ and filtered to obtain idesia polycarpa deacidified oil;
the addition amount of the activated clay is 8-12% of the mass of idesia polycarpa deacidified oil;
Preferably, the deodorization in the step (4) is to add a deodorant into the idesia polycarpa decolorized oil, react for 15-25 min at 20-30 ℃ and then remove the deodorant, repeat for 2-3 times, and concentrate in vacuum for 1.5-2.5 h to obtain idesia polycarpa deodorized oil, namely idesia polycarpa first-grade refined oil;
The deodorant consists of absolute methanol and absolute ethanol, and the mass ratio of the absolute methanol to the absolute ethanol is 0.5-1.5: 0.5 to 1.5 times of idesia oil removal quantity which is 1.5 to 2.5 times of idesia oil removal quantity, wherein the deodorization agent is removed by adopting a heating evaporation mode, and the heating temperature is 45 to 55 ℃.
The invention has the following beneficial effects:
The invention applies the aqueous enzymatic method to the extraction of idesia fruit grease, releases a large part of fatty acid in a combined state, effectively reduces impurities in idesia crude oil, such as idesia residues and the like, and improves the fluidity of idesia crude oil. The invention further refines idesia crude oil, sequentially carries out degumming, deacidification, decoloration and deodorization treatment, has lower temperature in the refining process and mild treatment condition, avoids long-time high-temperature treatment, can better retain the nutritional value of idesia oil, reduces the oxidation loss of natural lipid such as squalene, vitamin E and the like in idesia oil, and delays the oxidation speed of linoleic acid in idesia oil to oleic acid. The invention solves the problems of heavy oil gas taste and easy deterioration of idesia to generate harbour taste, the refined idesia oil has light color, strong fluidity and light plant fragrance, and has the advantages of simple process, environmental protection, health, convenient operation and the like, reduces the consumption of chemical auxiliary agents and energy sources in oil refining, and has wide prospect in the processing application of idesia oil.
Detailed Description
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Determining the feed-liquid ratio
Cleaning fresh mature idesia polycarpa, drying at 45 ℃ for 48 hours, removing branches and crushing to obtain idesia polycarpa powder. And detecting the grease content of idesia powder by adopting a Soxhlet extraction method to obtain the theoretical idesia crude oil weight.
The idesia powder is divided into 3 groups according to the feed liquid ratio of 1: 4. 1: 5. 1:6, mixing with water, adjusting pH to 4.5, adding pectase with enzyme activity of 50u/mg and accounting for 2.5% of the weight of idesia polycarpa powder, performing enzymolysis at 50deg.C for 4.5 hr, centrifuging at 4500r/min for 20min, and separating supernatant and emulsion layer. After the emulsion layer is subjected to ultrasonic treatment (the power is 120W) for 0.5h, centrifuging for 10min at the rotating speed of 4500r/min, separating out the supernatant oil in the emulsion layer, combining the two supernatant oils to obtain idesia polycarpa crude oil, weighing to obtain the actual idesia polycarpa crude oil weight, and respectively calculating the extraction rates of three groups of idesia polycarpa crude oils.
Table 1 extraction rates of idesia polycarpa crude oil of each feed liquid ratio group
| Feed-to-liquid ratio | 1：4 | 1：5 | 1：6 |
| Extraction rate | 78.6％ | 82.96％ | 77.21％ |
As can be seen from table 1, the feed-to-liquid ratio is 1: the extraction rate of idesia crude oil is highest in the step 5, so the feed liquid ratio is selected as 1:5.
Example 2
Determination of enzyme preparation type
Cleaning fresh mature idesia polycarpa, drying at 45 ℃ for 48 hours, removing branches and crushing to obtain idesia polycarpa powder. And detecting the grease content of idesia powder by adopting a Soxhlet extraction method to obtain the theoretical idesia crude oil weight.
The idesia powder is divided into 2 groups, and the two groups are respectively mixed according to a feed liquid ratio of 1:5, mixing with water, regulating pH to 4.5, respectively adding pectase and cellulase with the enzyme activity of 50u/mg and accounting for 2.5% of the mass of idesia polycarpa powder, carrying out enzymolysis for 4.5 hours at 50 ℃, centrifuging for 20 minutes at 4500r/min after the enzymolysis is finished, separating supernatant oil and emulsion layer, carrying out ultrasonic (power is 120W) treatment on the emulsion layer for 0.5 hours, centrifuging for 10 minutes at the rotating speed of 4500r/min, separating the supernatant oil of the emulsion layer, combining the two supernatant oils to obtain idesia polycarpa crude oil, weighing to obtain the actual idesia polycarpa crude oil weight, and respectively calculating the idesia polycarpa crude oil extraction rates of the two groups.
TABLE 2 extraction rates of idesia crude oil from different enzyme groups
| Enzyme species | Pectase enzyme | Cellulase enzymes |
| Extraction rate | 82.96％ | 74.28％ |
As is clear from Table 2, the extraction rate of idesia polycarpa crude oil was highest when the enzymolysis was performed with pectase, so pectase was used as an enzyme preparation for extracting idesia polycarpa oil.
Example 3
The extraction and refining method of idesia fruit grease specifically comprises the following steps:
(1) Treating idesia fruits: cleaning mature idesia fruits, drying at 45 ℃ for 48 hours, removing branches and crushing to obtain idesia powder;
(2) Enzymolysis: mixing idesia fruit powder and water according to a feed liquid ratio of 1:5, mixing, regulating pH to 4.5, adding pectase with enzyme activity of 50u/mg and accounting for 2.5% of the mass of idesia polycarpa powder, performing enzymolysis at 50deg.C for 4.5h, and centrifuging at 4500r/min for 20min after the enzymolysis is completed to obtain supernatant oil and emulsion layer;
(3) Demulsification: after carrying out ultrasonic treatment (power is 120W) on the emulsion layer for 0.5h, centrifuging for 10min at the rotating speed of 4500r/min, separating out supernatant oil of the emulsion layer, and combining the two supernatant oils to obtain idesia polycarpa crude oil;
(4) Degumming: heating idesia polycarpa crude oil to 50deg.C, maintaining for 2min, adding deionized water with the temperature of 90deg.C, and mixing for 1min. Adding degumming agent with the quality of 30% of crude oil (0.125 mol/L EDTA-2Na solution and 0.06mol/L SDS are mixed according to the volume ratio of 1:1), stirring and reacting for 30min, centrifuging at 8000rpm for 10min, and taking supernatant oil to obtain idesia polycarpa degummed oil;
(5) Deacidifying: heating idesia polycarpa degummed oil to 40 ℃, adding sodium hydroxide solution with the concentration of 0.15g/mL and with the mass of 10% of degummed oil, adding excessive alkali with the weight of 0.25% of degummed oil, stirring for 30min, standing and cooling to room temperature, centrifuging for 20min at the rotating speed of 5000r/min, taking supernatant oil, placing the supernatant oil into a cleaning kettle, adding water with the temperature of 60 ℃ and with the mass of 20% of degummed oil into the cleaning kettle, washing for 3h, keeping the temperature of oil and water by a heating device, fully and uniformly mixing the oil and the hot water by a stirring device, and dehydrating for 3.5h under the vacuum (the vacuum degree is 0.085 MPa) at 70 ℃ to obtain idesia polycarpa deacidified oil;
(6) Decoloring: heating idesia polycarpa deacidified oil to 90 ℃, adding activated clay with 15% of deacidified oil weight at constant temperature, stirring and heating for 0.5h, cooling to 70 ℃, and filtering to obtain idesia polycarpa deacidified oil;
(7) Deodorizing: to the idesia oil was added a deodorant (absolute methanol: absolute ethanol=1:1) twice the mass of the decolorized oil. Regulating the temperature to 25 ℃, stirring for 20min, steaming for 25min at 50 ℃ to remove the deodorant, deodorizing for three times, and concentrating at 40 ℃ in vacuum for 2h to obtain idesia polycarpa deodorized oil, namely idesia polycarpa first-stage refined oil.
The method has the advantages that the degumming rate of the idesia oil is 87% and the deacidification rate is 90% through detecting the phospholipid content and the oil acid value of the idesia oil before and after refining, so that the idesia oil has a more thorough color and luster, and can meet the edible requirement.
Example 4
The extraction and refining method of idesia fruit grease specifically comprises the following steps:
(1) Treating idesia fruits: cleaning mature idesia fruits, drying at 45 ℃ for 48 hours, removing branches and crushing to obtain idesia powder;
(2) Enzymolysis: mixing idesia fruit powder and water according to a feed liquid ratio of 1:5, mixing, regulating pH to 4.5, adding pectase with enzyme activity of 50u/mg and accounting for 2.5% of the mass of idesia polycarpa powder, performing enzymolysis at 50deg.C for 4.5h, and centrifuging at 4500r/min for 20min after the enzymolysis is completed to obtain supernatant oil and emulsion layer;
(3) Demulsification: after carrying out ultrasonic treatment (power is 120W) on the emulsion layer for 0.5h, centrifuging for 10min at the rotating speed of 4500r/min, separating out supernatant oil of the emulsion layer, and combining the two supernatant oils to obtain idesia polycarpa crude oil;
(4) Degumming: heating idesia polycarpa crude oil to 50deg.C, maintaining for 2min, adding deionized water with the temperature of 90deg.C, and mixing for 1min. Adding degumming agent with the quality of 30% of crude oil (0.125 mol/L EDTA-2Na solution and 0.06mol/L SDS are mixed according to the volume ratio of 2:1), stirring and reacting for 35min, centrifuging at 8000rpm for 10min, and taking supernatant oil to obtain idesia polycarpa degummed oil;
(5) Deacidifying: heating idesia polycarpa degummed oil to 40 ℃, adding sodium hydroxide solution with the concentration of 0.15g/mL and with the mass of 10% of degummed oil, adding excessive alkali with the weight of 0.25% of degummed oil, stirring for 45min, standing and cooling to room temperature, centrifuging for 20min at the rotating speed of 5000r/min, taking supernatant oil, putting the supernatant oil into a cleaning kettle, adding water with the temperature of 60 ℃ and with the mass of 20% of degummed oil into the cleaning kettle, washing for 3h, keeping the temperature of oil and water by a heating device, fully and uniformly mixing the oil and the hot water by a stirring device, and dehydrating for 3.5h under the vacuum (the vacuum degree is 0.085 MPa) at 70 ℃ to obtain idesia polycarpa deacidified oil;
(6) Decoloring: heating idesia polycarpa deacidified oil to 90 ℃, adding activated clay with 15% of deacidified oil weight at constant temperature, stirring and heating for 40min, cooling to 70 ℃, and filtering to obtain idesia polycarpa deacidified oil;
(7) Deodorizing: to the idesia oil was added a deodorant (absolute methanol: absolute ethanol=1:1) twice the mass of the decolorized oil. Regulating the temperature to 25 ℃, stirring for 20min, steaming for 25min at 50 ℃ to remove the deodorant, deodorizing for three times, and concentrating at 40 ℃ in vacuum for 2h to obtain idesia polycarpa deodorized oil, namely idesia polycarpa first-stage refined oil.
The method has the advantages that the degumming rate of the idesia oil is 91% and the deacidification rate is 93% through detecting the phospholipid content and the fatty acid value of the idesia oil before and after refining, so that the idesia oil is thorough in color and light yellow in color and can meet the edible requirement.
Example 5
The extraction and refining method of idesia fruit grease specifically comprises the following steps:
(1) Treating idesia fruits: cleaning mature idesia fruits, drying at 45 ℃ for 48 hours, removing branches and crushing to obtain idesia powder;
(2) Enzymolysis: mixing idesia fruit powder and water according to a feed liquid ratio of 1:5, mixing, regulating pH to 4.5, adding pectase with enzyme activity of 50u/mg and accounting for 2.5% of the mass of idesia polycarpa powder, performing enzymolysis at 50deg.C for 4.5h, and centrifuging at 4500r/min for 20min after the enzymolysis is completed to obtain supernatant oil and emulsion layer;
(3) Demulsification: after carrying out ultrasonic treatment (power is 120W) on the emulsion layer for 0.5h, centrifuging for 10min at the rotating speed of 4500r/min, separating out supernatant oil of the emulsion layer, and combining the two supernatant oils to obtain idesia polycarpa crude oil;
(4) Degumming: heating idesia polycarpa crude oil to 50deg.C, maintaining for 2min, adding deionized water with the temperature of 90deg.C, and mixing for 1min. Adding degumming agent with the quality of 30% of crude oil (0.125 mol/L EDTA-2Na solution and 0.06mol/L SDS are mixed according to the volume ratio of 2:1), stirring and reacting for 40min, centrifuging at 8000rpm for 10min, and taking supernatant oil to obtain idesia polycarpa degummed oil;
(5) Deacidifying: heating idesia polycarpa degummed oil to 45 ℃, adding sodium hydroxide solution with the concentration of 0.15g/mL and with the mass of 10% of degummed oil, adding excessive alkali with the weight of 0.25% of degummed oil, stirring for 35min, standing and cooling to room temperature, centrifuging for 20min at the rotating speed of 5000r/min, taking supernatant oil, putting the supernatant oil into a cleaning kettle, adding water with the temperature of 60 ℃ and with the mass of 20% of degummed oil into the cleaning kettle, washing for 3h, keeping the temperature of oil and water by a heating device, fully and uniformly mixing the oil and the hot water by a stirring device, and dehydrating for 3.5h under the vacuum (the vacuum degree is 0.085 MPa) at 70 ℃ to obtain idesia polycarpa deacidified oil;
(6) Decoloring: heating idesia polycarpa deacidified oil to 90 ℃, adding activated clay accounting for 10% of the deacidified oil weight at constant temperature, stirring and heating for 1h, cooling to 70 ℃, and filtering to obtain idesia polycarpa deacidified oil;
(7) Deodorizing: to the idesia oil was added a deodorant (absolute methanol: absolute ethanol=1:1) twice the mass of the decolorized oil. Regulating the temperature to 25 ℃, stirring for 20min, steaming for 25min at 50 ℃ to remove the deodorant, deodorizing for three times, and concentrating at 40 ℃ in vacuum for 2h to obtain idesia polycarpa deodorized oil, namely idesia polycarpa first-stage refined oil.
The method has the advantages that the degumming rate of the idesia oil is 90 percent, the deacidification rate is 91 percent, the idesia oil is thorough in color and light yellow in color and can meet the edible requirement by detecting the phospholipid content and the oil acid value of the idesia oil before and after refining.
Example 6
The fatty acid compositions of the idesia polycarpa crude oil and refined oil in example 4 were detected by gas chromatography mass spectrometry (GC-MS method), and the chromatographic peaks were integrated by normalized integration method to obtain the percentage of each fatty acid.
Dissolving 100 μL of grease with 2mL of normal hexane, adding 1mL of 1mol/L KOH-methanol solution, shaking, carrying out water bath at 60 ℃ for 40min, cooling, adding 3mL of saturated saline, shaking, centrifuging at 3500r/min for 10min, taking an upper normal hexane layer, filtering by using a 0.45 μm organic filter membrane, and obtaining a sample for gas chromatography analysis.
Chromatographic reference conditions: chromatographic column Agilent 123-5533DB-5MS (30 m×320 μm×1 μm), sample inlet temperature 250 ℃, flow rate 1.0mL/min, temperature program: the initial temperature was 80℃for 3min, at 8℃per min up to 150℃for 7min, at 10℃per min up to 240℃for 10min. The test results are shown in Table 3.
Physical and chemical index analysis was performed on idesia crude oil and refined oil in example 4 by referring to the national standard method, and the detection results are shown in table 4.
The acid value of idesia oil is measured by referring to GB 5009.229-2016;
the peroxide value of idesia oil is measured by referring to GB 5009.227-2016;
Iodine value of idesia oil is measured according to GB/T5532-2008;
saponification value of idesia oil is measured by referring to GB/T5534-2008.
TABLE 3 fatty acid main composition of idesia crude oil and idesia refined oil
TABLE 4 physicochemical index analysis of idesia crude oil and idesia refined oil
From tables 3 and 4, it is clear that the composition and content of the idesia oil fatty acid obtained by refining according to the invention are the same as those of the crude oil, and it is shown that the refining method of the invention does not affect the composition of the idesia oil fatty acid. Meanwhile, refined idesia oil has no impurities, clear color, good fluidity, high quality and light plant fragrance.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (8)
1. The extraction and refining method of idesia fruit grease is characterized by comprising the following steps:
(1) Drying idesia fruits and crushing to obtain idesia fruit powder;
(2) Mixing idesia fruit powder with water, adding enzyme for enzymolysis, and performing solid-liquid separation after enzymolysis to obtain supernatant oil and emulsion layer;
(3) Demulsification and solid-liquid separation are carried out on the emulsion layer, and an upper layer oil layer and the supernatant oil are combined to obtain idesia polycarpa crude oil;
(4) Sequentially degumming, deacidifying, decoloring and deodorizing the idesia polycarpa crude oil to obtain idesia primary refined oil.
2. The idesia fruit oil extraction and refining method according to claim 1, wherein in the step (2), the feed liquid ratio of idesia fruit powder to water is 1g: 4.5-5.5 mL, and regulating the pH value to 4-5 after mixing;
The enzyme is pectase, the enzyme activity is 50u/mg, and the addition amount is 2-3%; the enzymolysis time is 4-5 h, and the temperature is 40-60 ℃.
3. The idesia fruit oil extraction and refining method according to claim 2, wherein in the step (3), the demulsification is performed on an emulsion layer for 0.4-0.6 h, and the ultrasonic power is 110-130W.
4. The idesia fruit oil extraction and refining method according to claim 3, wherein the solid-liquid separation mode in the steps (2) and (3) is centrifugation, and the rotation speed of the centrifugation is 4000-5000 r/min and the time is 15-25 min.
5. The method for extracting and refining idesia fruit oil according to claim 4, wherein in the degumming in the step (4), water with the temperature of 85-95 ℃ is added into idesia crude oil with the temperature of 45-50 ℃, a degumming agent is added for reaction for 30-40 min, solid-liquid separation is carried out, and supernatant oil is taken to obtain idesia degummed oil;
the addition amount of the water is 8-12% of the mass of the idesia polycarpa crude oil;
The degumming agent is obtained by mixing 0.12-0.13 mol/L EDTA-2Na solution and 0.05-0.07 mol/L SDS according to the volume ratio of 1.5-2.5:0.8-1.2;
the solid-liquid separation mode is centrifugation, the rotation speed of the centrifugation is 7500-8500 rpm, and the time is 5-15 min.
6. The method for extracting and refining idesia fruit oil according to claim 5, wherein in the step (4), sodium hydroxide solution is added into idesia degumming oil at 35-45 ℃ for reaction for 35-45 min, standing, solid-liquid separation is carried out, and the supernatant oil is taken for water washing and dehydration to obtain idesia deacidification oil;
the concentration of the sodium hydroxide solution is 0.10-0.20 g/mL, and the addition amount is 8-12% of the mass of the idesia polycarpa degummed oil; adding the sodium hydroxide solution, and then adding excessive alkali with the quality of 0.20-0.30% of idesia degumming oil; the excessive alkali still adopts sodium hydroxide solution with the concentration of 0.10-0.20 g/mL;
the solid-liquid separation mode is centrifugation, the rotation speed of the centrifugation is 4500-5000 r/min, and the time is 15-25 min;
The water washing is to add water with the temperature of 55-65 ℃ accounting for 15-20% of the mass of the idesia polycarpa degummed oil, and react for 1h; the dehydration is carried out under vacuum, the vacuum degree is 0.08-0.09 MPa, and the time is 3-4 h.
7. The method for extracting and refining idesia fruit oil and fat according to claim 6, wherein in the step (4), activated clay is added into idesia deacidification oil at 85-95 ℃, the heating reaction is carried out for 0.5-1 h, the cooling is carried out to 65-75 ℃ and the idesia is filtered, so that idesia oil is obtained;
the addition amount of the activated clay is 8-12% of the mass of idesia polycarpa deacidified oil.
8. The method for extracting and refining idesia fruit oil and fat according to claim 7, wherein the deodorization in the step (4) is to add a deodorizing agent into idesia decolorized oil, react for 15-25 min at 20-30 ℃ and then remove the deodorizing agent, repeat for 2-3 times, and concentrate in vacuum for 1.5-2.5 h to obtain idesia deodorized oil, namely idesia first-grade refined oil;
The deodorant consists of absolute methanol and absolute ethanol, and the mass ratio of the absolute methanol to the absolute ethanol is 0.5-1.5: 0.5 to 1.5 times of idesia oil removal quantity which is 1.5 to 2.5 times of idesia oil removal quantity, wherein the deodorization agent is removed by adopting a heating evaporation mode, and the heating temperature is 45 to 55 ℃.
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