CN104560381A - Subcritical extraction process of high-quality chaenomeles speciosa seed oil - Google Patents
Subcritical extraction process of high-quality chaenomeles speciosa seed oil Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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Abstract
The invention discloses high-quality chaenomeles speciosa seed oil and a subcritical extraction process of the high-quality chaenomeles speciosa seed oil. The process comprises the following contents: selecting full and mature chaenomeles speciosa seeds, pulverizing and sieving for later use; extracting chaenomeles speciosa seed powder for multiple times by using a subcritical fluid extracting device by using n-butane as an extraction solvent; separating extraction solvent from a target product in a way of desolvation of a compressor and a vacuum pump-compressor combined desolvation to obtain crude oil; and performing refined filtration on the crude oil to obtain the high-quality chaenomeles speciosa seed oil. The method has the characteristics of simplicity in operation, low energy consumption, small pollution, short extraction time, high oil extraction rate and capability of realizing industrial production. By utilizing a subcritical fluid extraction technology, the extraction process is completed at a low temperature, the physicochemical property of the target product can be maintained, and nutritive components can be protected from being damaged; the extracted chaenomeles speciosa oil is high in quality and has low acid values and peroxide values; the polyphenol total content is more than 0.52 mg/g, the proportion of unsaturated fatty acid to fatty acid is more than 85 percent; oleic acid and linoleic acid respectively account for more than 40 percent and the proportions are approximately. The chaenomeles speciosa seed oil subjected to subcritical fluid extraction is simply filtered in a refined mode and can be used as high-grade plant oil and basic oil, so that the refining process is reduced, the industrial cost is reduced, and the high-quality chaenomeles speciosa seed oil has great significance in realizing new resource functional oil industrialization production.
Description
Technical field
The present invention relates to functional plants grease and extract field, specifically a kind of subcritical abstraction technique of high-quality Fructus Chaenomelis seed oil.
Background technology
Fructus Chaenomelis is the dry almost ripe fruit of rosaceous plant chaenomeles lagenaria, is mainly distributed in East China, Central China and southwestern various places.Its nutritive value can compare favourably with Kiwifruit, famous with " hundred benefits fruit ", is one of dietotherapeutic food of announcing in the first batch of health ministry.Modern study finds, main containing chemical compositions such as flavonoid, organic acid, triterpenes, saponins, carbohydrate, tannins in Fructus Chaenomelis, have protect the liver, the multiple pharmacologically active such as gastrointestinal antispasmodic, relieving inflammation and relaxing pain.
Fructus Chaenomelis cultivated area is wide, high containing seed amount.At present, its chemical composition is mainly concentrated on, pharmacology, cultivation technique, the aspects such as processing technology to the research of Fructus Chaenomelis, and less to the research on utilization of waste as Fructus Chaenomelis seed, skin.Fructus Chaenomelis seed crude fat content is high, and lipid acid composition is abundant, if developed as little oil plant by Fructus Chaenomelis seed, produces mixed oil and functional grease, both can turn waste into wealth, and make full use of the natural resources, reduce environmental pollution; Again can prosperity edible oil market, increase economic efficiency and people ' s health level.
The domestic and international method for extracting Vegetable oil lipoprotein mainly contains milling process, lixiviation process and super critical extraction at present.Milling process due to temperature high, grease is oxidizable rotten; There is dissolvent residual in lixiviation process, last handling process is complicated; Supercutical fluid industrial scale is little, and deindustrialization is produced.And subcritical fluid extraction is the emerging isolation technique of one grown up after supercritical extraction, utilize subcritical fluids as extraction agent, carry out in the pressurized vessel of airtight, anaerobic, low pressure, have many advantages compared with other separation method: nontoxic, low-energy environment-friendly, non-thermal technology.Not only can improve grease extraction efficiency, and raw material nutritive value can be retained better and functional ingredient does not destroy, is not oxidized.And running cost is low, can industrialization scale operation, in grease extraction, there is good application prospect.
Summary of the invention
The object of the present invention is to provide the subcritical abstraction technique of high-quality Fructus Chaenomelis seed oil of a kind of high-efficiency environment friendly, industrialization, to solve the problem proposed in above-mentioned background technology.
For achieving the above object, the invention provides following technical scheme:
A subcritical abstraction technique for high-quality Fructus Chaenomelis seed oil, concrete steps are as follows:
(1) raw materials pretreatment: the Fructus Chaenomelis seed that preferred particulates is full, ripe is raw material, is placed in baking oven in 40-50 DEG C of dry 46-50h, more dried Fructus Chaenomelis seed is put into obtain seed benevolence powder after pulverizer pulverizes and sieves for subsequent use;
(2) feed: above-mentioned seed benevolence powder is put into the netted silk fabric of 200-220 object and is fed into subcritical abstraction still, make the vacuum tightness in subcritical abstraction still and separating still be-0.1-0MPa with vacuum pump;
(3) subcritical fluid extraction: inject extraction solvent normal butane to the complete submergence of sample in subcritical abstraction still, adopts hot water cyclesystem to heat extraction kettle, and carries out 3-4 extraction;
(4) precipitation: after extraction terminates, mixture containing Fructus Chaenomelis seed oil and extraction solvent is put into separating still, carry out compressor precipitation and vacuum pump-compressor interlock precipitation, the compressor precipitation time is 25-35min, vacuum pump-compressor interlock precipitation time is 8-12min, open separating still lower end valve after precipitation, collect Fructus Chaenomelis seed crude oil;
(5) crude oil is refined: above-mentioned obtained Fructus Chaenomelis seed crude oil is carried out suction filtration, namely obtains refining Fructus Chaenomelis seed oil.
As the further scheme of the present invention: the dried moisture content of Fructus Chaenomelis seed benevolence in described step (1), lower than 3%, uses 40-50 eye mesh screen during grinding and sieving.
As the further scheme of the present invention: the subcritical abstraction parameter in described step (3) is: extracting pressure is 0.3-0.5MPa, extraction temperature is 45-50 DEG C, and each extraction time is 20-60min.
As the further scheme of the present invention: the subcritical abstraction parameter in described step (3) is: extracting pressure is 0.4MPa, extraction temperature is 50 DEG C, extraction times is four times, extraction time is 60min for the first time, second time extraction time is 30min, third time, extraction time was 30min, and the 4th time extraction time is 20min.
As the further scheme of the present invention: the precipitation first time subcritical fluid extraction product in the second time subcritical fluid extraction in described step (3) and step (4) carries out simultaneously; Released by crude oil after precipitation, then the mixture containing Fructus Chaenomelis seed oil and extraction solvent of second time subcritical fluid extraction is put into separating still, during precipitation, the compressor precipitation time is 30min, and vacuum pump-compressor interlock precipitation time is 10min.
As the further scheme of the present invention: gained Fructus Chaenomelis seed oil unsaturated fatty acid content is 87-89%, and total phenol content is 0.52-0.54mg/g.
As the present invention's further scheme: gained Fructus Chaenomelis seed oil unsaturated fatty acid content is 88.15%, and total phenol content is 0.527mg/g.
Compared with prior art, the invention has the beneficial effects as follows:
Present method have simple to operate, energy consumption is low, it is little to pollute, extraction time is short, oil extracting rate is high, be conducive to realizing the feature of suitability for industrialized production, adopt subcritical fluid extraction technology, complete under cryogenic, extraction solvent low toxicity is harmless, the nutritive ingredient of target product can be kept to be without prejudice, to extract the Fructus Chaenomelis seed oil quality obtained good, only need namely can be used as high-grade vegetable oil and base oil use through simple refining, can refining procedure be reduced, reduce industrial cost.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Fig. 2 is that the Fructus Chaenomelis seed oil fatty acid composition GC-MS that the present invention obtains characterizes collection of illustrative plates.
Embodiment
Be described in more detail below in conjunction with the technical scheme of embodiment to this patent.
Embodiment 1
Refer to Fig. 1, in the embodiment of the present invention, a kind of subcritical abstraction technique of high-quality Fructus Chaenomelis seed oil, concrete steps are as follows:
(1) raw materials pretreatment: the Fructus Chaenomelis seed that preferred particulates is full, ripe is raw material, be placed in baking oven in 40 DEG C of dry 46h, obtain the dry Fructus Chaenomelis seed that moisture content is 2.5%, then cross 40 mesh sieves after dried Fructus Chaenomelis seed being put into pulverizer pulverizing, obtain seed benevolence powder for subsequent use;
(2) feed: take above-mentioned seed benevolence powder 500.3g, put into the netted silk fabric of 200 object and be fed into subcritical abstraction still, make the vacuum tightness in subcritical abstraction still and separating still be-0.05MPa with vacuum pump;
(3) subcritical fluid extraction: inject extraction solvent normal butane to the complete submergence of sample in subcritical abstraction still, hot water cyclesystem is adopted to heat extraction kettle, temperature in extraction kettle is made to be 45 DEG C, extracting pressure is 0.3MPa, carry out three extractions, first time, extraction time was 60min, and second time extraction time is 30min, and extraction time is 30min for the third time;
(4) precipitation: after extraction terminates, mixture containing Fructus Chaenomelis seed oil and extraction solvent is put into separating still, carry out compressor precipitation and vacuum pump-compressor interlock precipitation, the compressor precipitation time is 25min, vacuum pump-compressor interlock precipitation time is 8min, open separating still lower end valve after precipitation, collect Fructus Chaenomelis seed crude oil;
(5) crude oil is refined: above-mentioned obtained Fructus Chaenomelis seed crude oil is carried out suction filtration, namely obtains refining Fructus Chaenomelis seed oil.
In the present embodiment, gained Fructus Chaenomelis seed oil is yellow transparent oily liquids, and through weighing as 84.6g, extraction yield is 16.9%.Main physical and chemical index: acid value: 0.53mgKOH/g, iodine number: 113.2gI2/100g, saponification value: 175.3mgKOH/g, peroxide value: 0.02mmol/kg; Go out containing 8 kinds of lipid acid in gained Fructus Chaenomelis seed oil through GC-MS isolation identification, wherein unsaturated fatty acids accounts for 88.15%, and Fructus Chaenomelis seed oil total phenol content is 0.526mg/g.
Embodiment 2
Refer to Fig. 1, in the embodiment of the present invention, a kind of subcritical abstraction technique of high-quality Fructus Chaenomelis seed oil, concrete steps are as follows:
(1) raw materials pretreatment: the Fructus Chaenomelis seed that preferred particulates is full, ripe is raw material, be placed in baking oven in 45 DEG C of dry 48h, obtain the dry Fructus Chaenomelis seed that moisture content is 2.2%, then cross 45 mesh sieves after dried Fructus Chaenomelis seed being put into pulverizer pulverizing, obtain seed benevolence powder for subsequent use;
(2) feed: take above-mentioned seed benevolence powder 480.6g, put into the netted silk fabric of 210 object and be fed into subcritical abstraction still, make the vacuum tightness in subcritical abstraction still and separating still be-0.08MPa with vacuum pump;
(3) subcritical fluid extraction: inject extraction solvent normal butane to the complete submergence of sample in subcritical abstraction still, adopting hot water cyclesystem to carry out heating to extraction kettle makes temperature in extraction kettle be 50 DEG C, extracting pressure is 0.4MPa, carry out four extractions, extraction time is 60min for the first time, second time extraction time is 30min, and extraction time is 30min for the third time, and the 4th time extraction time is 20min;
(4) precipitation: after extraction terminates, mixture containing Fructus Chaenomelis seed oil and extraction solvent is put into separating still, carry out compressor precipitation and vacuum pump-compressor interlock precipitation, the compressor precipitation time is 30min, vacuum pump-compressor interlock precipitation time is 10min, open separating still lower end valve after precipitation, collect Fructus Chaenomelis seed crude oil;
(5) crude oil is refined: above-mentioned obtained Fructus Chaenomelis seed crude oil is carried out suction filtration, namely obtains refining Fructus Chaenomelis seed oil.
In the present embodiment, gained Fructus Chaenomelis seed oil is yellow transparent oily liquids, and through weighing as 81.2g, extraction yield is 16.3%.Main physical and chemical index: acid value: 0.52mgKOH/g, iodine number: 112.9gI2/100g, saponification value: 176.1mgKOH/g, peroxide value: 0.03mmol/kg; Go out containing 8 kinds of lipid acid in gained Fructus Chaenomelis seed oil through GC-MS isolation identification, wherein unsaturated fatty acids accounts for 87.93%, and Fructus Chaenomelis seed oil total phenol content is 0.523mg/g.
Embodiment 3
Refer to Fig. 1, in the embodiment of the present invention, a kind of subcritical abstraction technique of high-quality Fructus Chaenomelis seed oil, concrete steps are as follows:
(1) raw materials pretreatment: the Fructus Chaenomelis seed that preferred particulates is full, ripe is raw material, be placed in baking oven in 50 DEG C of dry 50h, obtain the dry Fructus Chaenomelis seed that moisture content is 2%, then cross 50 mesh sieves after dried Fructus Chaenomelis seed being put into pulverizer pulverizing, obtain seed benevolence powder for subsequent use;
(2) feed: take above-mentioned seed benevolence powder 800g, put into the netted silk fabric of 220 object and be fed into subcritical abstraction still, make the vacuum tightness in subcritical abstraction still and separating still be-0.1MPa with vacuum pump;
(3) subcritical fluid extraction: inject extraction solvent normal butane to the complete submergence of sample in subcritical abstraction still, adopting hot water cyclesystem to carry out heating to extraction kettle makes temperature in extraction kettle be 55 DEG C, extracting pressure is 0.5MPa, carry out four extractions, extraction time is 60min for the first time, second time extraction time is 30min, and extraction time is 30min for the third time, and the 4th time extraction time is 20min;
(4) precipitation: after extraction terminates, mixture containing Fructus Chaenomelis seed oil and extraction solvent is put into separating still, carry out compressor precipitation and vacuum pump-compressor interlock precipitation, the compressor precipitation time is 35min, vacuum pump-compressor interlock precipitation time is 12min, open separating still lower end valve after precipitation, collect Fructus Chaenomelis seed crude oil;
(5) crude oil is refined: above-mentioned obtained Fructus Chaenomelis seed crude oil is carried out suction filtration, namely obtains refining Fructus Chaenomelis seed oil.
In the present embodiment, gained Fructus Chaenomelis seed oil is yellow transparent oily liquids, through weighing as 149.6g, and extraction rate reached 18.7%.Main physical and chemical index: acid value: 0.53mgKOH/g, iodine number: 113.5gI2/100g, saponification value: 178.6mgKOH/g, peroxide value: 0.05mmol/kg; Go out containing 8 kinds of lipid acid in gained Fructus Chaenomelis seed oil through GC-MS isolation identification, wherein unsaturated fatty acids accounts for 88.87%, and Fructus Chaenomelis seed oil total phenol content is 0.527mg/g.
Refer to Fig. 2, the Fructus Chaenomelis seed oil that the present invention prepares carries out GC-MS isolation identification, and the lipid acid composition obtained is as shown in table 1:
Fatty acid component and content in table 1 Fructus Chaenomelis seed oil
Present method have simple to operate, energy consumption is low, it is little to pollute, extraction time is short, oil extracting rate is high, be conducive to realizing the feature of suitability for industrialized production, adopt subcritical fluid extraction technology, complete under cryogenic, extraction solvent low toxicity is harmless, the nutritive ingredient of target product can be kept to be without prejudice, to extract the Fructus Chaenomelis seed oil quality obtained good, only need namely can be used as high-grade vegetable oil and base oil use through simple refining, can refining procedure be reduced, reduce industrial cost.
Above the better embodiment of this patent is explained in detail, but this patent is not limited to above-mentioned embodiment, in the ken that one skilled in the relevant art possesses, various change can also be made under the prerequisite not departing from this patent aim.
Claims (7)
1. a subcritical abstraction technique for high-quality Fructus Chaenomelis seed oil, it is characterized in that, concrete steps are as follows:
(1) raw materials pretreatment: the Fructus Chaenomelis seed that preferred particulates is full, ripe is raw material, is placed in baking oven in 40-50 DEG C of dry 46-50h, more dried Fructus Chaenomelis seed is put into obtain seed benevolence powder after pulverizer pulverizes and sieves for subsequent use;
(2) feed: above-mentioned seed benevolence powder is put into the netted silk fabric of 200-220 object and is fed into subcritical abstraction still, make the vacuum tightness in subcritical abstraction still and separating still be-0.1-0MPa with vacuum pump;
(3) subcritical fluid extraction: inject extraction solvent normal butane to the complete submergence of sample in subcritical abstraction still, adopts hot water cyclesystem to heat extraction kettle, and carries out 3-4 extraction;
(4) precipitation: after extraction terminates, mixture containing Fructus Chaenomelis seed oil and extraction solvent is put into separating still, carry out compressor precipitation and vacuum pump-compressor interlock precipitation, the compressor precipitation time is 25-35min, vacuum pump-compressor interlock precipitation time is 8-12min, open separating still lower end valve after precipitation, collect Fructus Chaenomelis seed crude oil;
(5) crude oil is refined: above-mentioned obtained Fructus Chaenomelis seed crude oil is carried out suction filtration, namely obtains refining Fructus Chaenomelis seed oil.
2. the subcritical abstraction technique of high-quality Fructus Chaenomelis seed oil according to claim 1, is characterized in that, the dried moisture content of Fructus Chaenomelis seed benevolence in described step (1), lower than 3%, uses 40-50 eye mesh screen during grinding and sieving.
3. the subcritical abstraction technique of high-quality Fructus Chaenomelis seed oil according to claim 1, it is characterized in that, subcritical abstraction parameter in described step (3) is: extracting pressure is 0.3-0.5MPa, and extraction temperature is 45-50 DEG C, and each extraction time is 20-60min.
4. the subcritical abstraction technique of the high-quality Fructus Chaenomelis seed oil according to claim 1,3, it is characterized in that, subcritical abstraction parameter in described step (3) is: extracting pressure is 0.4MPa, extraction temperature is 50 DEG C, extraction times is four times, and extraction time is 60min for the first time, and second time extraction time is 30min, third time, extraction time was 30min, and the 4th time extraction time is 20min.
5. the subcritical abstraction technique of high-quality Fructus Chaenomelis seed oil according to claim 1, is characterized in that, the precipitation first time subcritical fluid extraction product in the second time subcritical fluid extraction in described step (3) and step (4) carries out simultaneously; Released by crude oil after precipitation, then the mixture containing Fructus Chaenomelis seed oil and extraction solvent of second time subcritical fluid extraction is put into separating still, during precipitation, the compressor precipitation time is 30min, and vacuum pump-compressor interlock precipitation time is 10min.
6. the subcritical abstraction technique of the high-quality Fructus Chaenomelis seed oil according to claim 1-5, is characterized in that, gained Fructus Chaenomelis seed oil unsaturated fatty acid content is 87-89%, and total phenol content is 0.52-0.54mg/g.
7. the subcritical abstraction technique of the high-quality Fructus Chaenomelis seed oil according to claim 1-6, is characterized in that, gained Fructus Chaenomelis seed oil unsaturated fatty acid content is 88.15%, and total phenol content is 0.527mg/g.
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| CN106047476A (en) * | 2016-08-02 | 2016-10-26 | 岳西县光圣茶油有限公司 | Low-temperature squeezing-subcritical extraction process of walnut brain-nourishing tea oil |
| 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 |
| 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 |
| CN106833881A (en) * | 2017-03-02 | 2017-06-13 | 中国林业科学研究院林产化学工业研究所 | A kind of method that utilization subcritical fluid extraction technology prepares high-quality Ginkgo oil |
| CN107129863A (en) * | 2017-05-24 | 2017-09-05 | 中国农业大学 | A kind of extracting method of melon seeds in August oil |
| CN108251218A (en) * | 2018-02-11 | 2018-07-06 | 安阳工学院 | A kind of method of highly selective extraction north Chinese mugwort essential oil |
| CN111518615A (en) * | 2020-04-28 | 2020-08-11 | 武汉轻工大学 | Method for preparing shea butter by adopting subcritical propane extraction technology, shea butter and application |
| CN112450283A (en) * | 2020-11-17 | 2021-03-09 | 江苏鸿祺生物科技有限公司 | Peony seed blend oil based on supercritical extraction and preparation method thereof |
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| CN108251218A (en) * | 2018-02-11 | 2018-07-06 | 安阳工学院 | A kind of method of highly selective extraction north Chinese mugwort essential oil |
| CN108251218B (en) * | 2018-02-11 | 2021-06-15 | 安阳工学院 | Method for extracting artemisia vulgaris essential oil with high selectivity |
| CN111518615A (en) * | 2020-04-28 | 2020-08-11 | 武汉轻工大学 | Method for preparing shea butter by adopting subcritical propane extraction technology, shea butter and application |
| CN112450283A (en) * | 2020-11-17 | 2021-03-09 | 江苏鸿祺生物科技有限公司 | Peony seed blend oil based on supercritical extraction and preparation method thereof |
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