CN102080017A - Gallic oil composite and preparation method thereof - Google Patents
Gallic oil composite and preparation method thereof Download PDFInfo
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- CN102080017A CN102080017A CN201010578999XA CN201010578999A CN102080017A CN 102080017 A CN102080017 A CN 102080017A CN 201010578999X A CN201010578999X A CN 201010578999XA CN 201010578999 A CN201010578999 A CN 201010578999A CN 102080017 A CN102080017 A CN 102080017A
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Abstract
The invention relates to a gallic oil composite and a preparation method thereof. The preparation method comprises the following steps: removing impurities in gallnut, performing coarse crushing, adding organic solvent in the obtained gallnut in a weight measurement ratio of 1:3-30g/mL; performing continuous extraction through the hot refluxing method or percolation method for 2-4 times, wherein the extraction time is 0.5-8 hours each time; filtering, and evaporating filtrate to recycle solvent and obtain light brown oily liquid; or performing supercritical CO2 extraction separation on raw material under the conditions that the extraction temperature is from the room temperature to 90 DEG C, the pressure is 5MPa-50MPa and the time is 5-7 hours, and performing reduced pressure separation to produce gallic oil. The oil composite in the invention is mainly composed of unsaturated fatty acid compounds and saturated fatty acid compounds, wherein the content of the unsaturated fatty acid compounds is 25-35%, the content of the saturated fatty acid compounds is 55-63%; the unsaturated fatty acid compounds mainly contain oleic acid compounds, linoleic acid compounds and linolenic acid compounds; and the saturated fatty acid compounds mainly contain capric acid compounds, lauric acid compounds, myristic acid compounds, palmitic acid compounds and stearic acid compounds.
Description
Technical field
The present invention relates to the Turkey-galls tripe doubly is fat or oil composition of raw material extraction and preparation method thereof.
Background technology
Turkey-galls is China's characteristic Forest products, by goitre cotten aphid section (
Pemphigidae) five root section aphid subfamilies (
Fordinae) some aphid, colonize in Anacardiaceae (
Anacardiaceae) Rhus (
Rhus) on the compound leaves of several trees, the general designation of the insect gall of formation.Different times aphid parasitisms have specificity, the gall nut of formation (insect gall), and its face shaping, size, weight and tannin content etc. are all different.A kind of times of aphid only forms a kind of gall nut.China has write down 14 kinds of times of aphids so far altogether, they form 14 kinds of Turkey-galls respectively, be respectively the angle doubly, tripe doubly, circle tripe times, times egg, jujube iron doubly, egg iron doubly, the egg tripe doubly, red little iron jujube doubly, the little iron jujube of yellow hair doubly, rice doubly, doubly flower, red times of flower, iron doubly flower and Zhou Shi doubly spend, " Pharmacopoeia of People's Republic of China (2005 editions) " Chinese medicinal materials portion " Turkey-galls " has recorded tripe wherein down doubly and tripe times.
Tripe doubly mainly is distributed in China Qinling Mountains, on the south the Daba Mountain, to the north of the Changjiang river, causing gall aphid is tripe times aphid, it parasitizes the little leaf back of blue or green bran poplar compound leaf.Stature is bigger, and the maximum is 110mm * 50mm.Times wall is than doubly thick of tripe, and the gall nut smooth surface does not have projection, and is oval to oblong or jujube shape, the blunt point of tip but do not have hook-shaped projection.The ripe explosion phase be late June to mid-July, a bright times water ratio is about 44%.Commodity are doubly best in quality, average 55～81/500g of number of individuals, tannin content (in over dry) 69.0%～72.4%; Total color 0.6～1.6 is one of good gall nut kinds of giving priority to, and output accounts for 25% of national Turkey-galls ultimate production.
Documents and materials report Chinese gall oil can be used for treating diabetes, but it is that raw material extracts Chinese gall oil that existing research report only limits to Turkey-galls Chinese medicinal materials (mixing commodity doubly), do not see that causing the parasitic different Turkey-galls that form of gall aphid with different biotic populations is raw material, produces the Chinese gall oil with specific components.Tripe doubly causes gall aphid, host and the place of production with other times kind and all is not quite similar, and its component purity of Turkey-galls tripe times fat or oil composition of its extraction is higher, and hypoglycemic activity is stronger.
Summary of the invention
The object of the present invention is to provide that a kind of to cause the tripe that goitre forms with tripe times aphid doubly be Turkey-galls tripe times grease of raw material extraction and preparation method thereof.
Embodiment of the present invention are: a kind of Turkey-galls tripe times fat or oil composition, make by the method that may further comprise the steps: tripe is doubly removed impurity elimination doubly, coarse crushing, crossing 10 mesh sieves and remove worm dung and dust in the goitre, is the ratio adding organic solvent of 1:3 ~ 30g/mL in doubly spending with the weightmeasurement ratio of organic solvent, heat reflow method or percolation continuous extraction 2 ~ 4 times, each 0.5 ~ 8 hour, filter, solvent is reclaimed in the filtrate evaporation, gets shallow pale brown oily liquids.
Described organic solvent is sherwood oil, 6# solvent or hexane.
The present invention also can be made by following method: with the raw material supercritical CO
2Extracting and separating, extraction temperature are room temperature to 90 ℃, pressure 5Mpa ~ 50Mpa, and 5 ~ 7 hours time, decompression separation is produced doubly oil of tripe.
The grease obtained composition of the present invention contains unsaturated fatty acids 25-35%, saturated fatty acid 55-63%, unsaturated fatty acids mainly contains oleic acid, linolic acid, linolenic acid compounds, and saturated fatty acid mainly comprises capric acid, lauric acid, tetradecanoic acid, palmitinic acid, stearic acid compound.
Embodiment
Embodiment 1:Get tripe times 100g, and the adding sherwood oil (60 ~ 90 ℃, boiling range, down together) 500 mL, and be heated to 60 ℃ of backflow 2h, filter; Filter residue adds sherwood oil (60 ~ 90 ℃) 500 mL secondary thermal backflow lixiviate 2h, filters; Merging filtrate reclaims sherwood oil, makes Turkey-galls tripe times grease 1.3g.
Embodiment 2:Get tripe times 100g, add sherwood oil (30 ~ 60 ℃) 500 mL, be heated to 60 ℃ of backflow 2h, filter; Filter residue adds sherwood oil (30 ~ 60 ℃) 500 mL secondary thermal backflow lixiviate 2h, filters; Merging filtrate reclaims sherwood oil, makes Turkey-galls tripe times grease 1.1g.
Embodiment 3:Get tripe times 100g, add sherwood oil (30 ~ 60 ℃) 500 mL, be heated to 40 ℃ of backflow 6h, filter; Filter residue adds sherwood oil (30 ~ 60 ℃) 500 mL secondary thermal backflow lixiviate 6h, filters; Merging filtrate reclaims sherwood oil, makes Turkey-galls tripe times grease 0.9g.
Embodiment 4: get tripe times 100g, add 6# solvent 500 mL, be heated to 40 ℃ of backflow 2h, filter; Filter residue adds 6# solvent 500 mL secondary thermal backflow lixiviate 2h, filters; Merging filtrate reclaims the 6# solvent, makes Turkey-galls tripe times grease 1.0g.
Embodiment 5: get tripe times 100g, add 6# solvent 500mL, be heated to 40 ℃ of backflow 2h, filter; Filter residue adds 6# solvent 500mL secondary thermal backflow lixiviate 2h, filters; Filter residue adds three thermal backflow lixiviates of No. 6 solvent 500mL 2h, filters; Merging filtrate reclaims the 6# solvent, makes Turkey-galls tripe times grease 1.1g.
Embodiment 6: get tripe times 100g, add 6# solvent 1400 mL, be heated to 70 ℃ of backflow 4h, filter, reclaim the 6# solvent, make Turkey-galls times caul-fat fat 1.4g.
Embodiment 7: get tripe times 100g, add normal hexane 500 mL, be heated to 40 ℃ of backflow 6h, filter; Filter residue adds normal hexane 500 mL secondary thermal backflow lixiviate 6h, filters; Merging filtrate reclaims normal hexane, makes Turkey-galls tripe times grease 1.1g.
Embodiment 8:Get tripe times 100g, add normal hexane 500 mL, be heated to 60 ℃ of backflow 6h, filter; Filter residue adds normal hexane 500 mL secondary thermal backflow lixiviate 6h, filters; Merging filtrate reclaims normal hexane, makes Turkey-galls tripe times grease 1.2g.
Embodiment 9:Get tripe times 100g, add ethyl acetate 500 mL, be heated to 60 ℃ of backflow 6h, filter; Filter residue adds ethyl acetate 500 mL secondary thermal backflow lixiviate 6h, filters; Merging filtrate reclaims ethyl acetate, makes Turkey-galls tripe times grease 2.2g.
Embodiment 10:Get tripe times 1000g, put supercritical CO
2Extracting and separating is a room temperature in extraction temperature, CO
2Pressure 20Mpa, extracting and separating 6 hours, decompression separation get the doubly oily 16.5g of tripe.
The doubly oily yield of the prepared Turkey-galls tripe of the various embodiments described above is 0.9 ~ 2.2g.Adopt GC-MS(gas chromatography-mass spectrography) to detect oil component and content, its fat or oil composition mainly is made up of unsaturated fatty acids, saturated fatty acid compounds, unsaturated fatty acids 25-35% wherein, saturated fatty acid 55-63%, unsaturated fatty acids mainly contains oleic acid, linolic acid, linolenic acid compounds, and saturated fatty acid mainly comprises capric acid, lauric acid, tetradecanoic acid, palmitinic acid, stearic acid compound.
Claims (5)
1. Turkey-galls tripe times fat or oil composition, it is characterized in that, make by the method that may further comprise the steps: tripe is doubly removed impurity, coarse crushing, cross 10 mesh sieves and remove worm dung and dust in the goitre, in doubly spending with the weightmeasurement ratio of organic solvent is the ratio adding organic solvent of 1:3 ~ 30g/mL, heat reflow method or percolation continuous extraction 2 ~ 4 times, each 0.5 ~ 8 hour, filter, solvent is reclaimed in the filtrate evaporation, gets shallow pale brown oily liquids, and described organic solvent is sherwood oil, 6# solvent, hexane or ethyl acetate.
2. a Turkey-galls tripe times fat or oil composition is characterized in that, by comprising that following method makes: with the raw material supercritical CO
2Extracting and separating, extraction temperature are room temperature to 90 ℃, pressure 5Mpa ~ 50Mpa, and 5 ~ 7 hours time, decompression separation is produced doubly oil of tripe.
3. Turkey-galls tripe times fat or oil composition according to claim 1 and 2, it is characterized in that, contain unsaturated fatty acids 25-35%, saturated fatty acid 55-63%, unsaturated fatty acids contains oleic acid, linoleic acid plus linolenic acid compounds, and saturated fatty acid comprises capric acid, lauric acid, tetradecanoic acid, palmitinic acid and stearic acid compound.
4. the preparation method of a Turkey-galls tripe times fat or oil composition as claimed in claim 1, it is characterized in that, step comprises: tripe is doubly removed impurity elimination doubly, and coarse crushing is crossed 10 mesh sieves and is removed worm dung and dust in the goitre, in doubly spending with the weightmeasurement ratio of organic solvent is the ratio adding organic solvent of 1:3 ~ 30g/mL, heat reflow method or percolation continuous extraction 2 ~ 4 times each 0.5 ~ 8 hour, filter, solvent is reclaimed in the filtrate evaporation, gets shallow pale brown oily liquids.
5. the preparation method of a Turkey-galls tripe times fat or oil composition as claimed in claim 2 is characterized in that, with the raw material supercritical CO
2Extracting and separating, extraction temperature are room temperature to 90 ℃, pressure 5Mpa ~ 50Mpa, and 5 ~ 7 hours time, decompression separation is produced doubly oil of tripe.
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| CN201010578999XA CN102080017A (en) | 2010-12-08 | 2010-12-08 | Gallic oil composite and preparation method thereof |
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| CN201010578999XA CN102080017A (en) | 2010-12-08 | 2010-12-08 | Gallic oil composite and preparation method thereof |
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| CN102080017A true CN102080017A (en) | 2011-06-01 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1232866A (en) * | 1998-04-21 | 1999-10-27 | 李素琼 | Gallnut oil and its extraction process and application in pharmacy |
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2010
- 2010-12-08 CN CN201010578999XA patent/CN102080017A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1232866A (en) * | 1998-04-21 | 1999-10-27 | 李素琼 | Gallnut oil and its extraction process and application in pharmacy |
Non-Patent Citations (2)
| Title |
|---|
| 《中国药学杂志》 20051031 蒲旭峰等 五倍子降血糖有效组分的药理筛选 第1470-1473页 2，3，5 第40卷, 第19期 * |
| 蒲旭峰等: "五倍子降血糖有效组分的药理筛选", 《中国药学杂志》 * |
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Application publication date: 20110601 |