CN101781601A - Method for extracting pupa oil from silkworm pupa by using ultrasonic wave - Google Patents
Method for extracting pupa oil from silkworm pupa by using ultrasonic wave Download PDFInfo
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Abstract
The invention relates to a method for extracting pupa oil from silkworm pupas by using ultrasonic wave. The method is formed by silkworm pupa pretreatment, ultrasonic extraction, pupa oil preparation and refining. Compared with solvent extraction method, since the ultrasonic extraction is adopted, the extraction duration is shortened to 30 minutes from 2 hours, the extract rate is improved to 96.3 percent from 81.1 percent and the product yield is improved to 28.9 percent from 24.3 percent. According to the detection of the pupa oil prepared through the method of the invention, all indexes satisfy the pupa oil quality standard reported in literature and the GB15306-2004 rapeseed oil quality standard, and the pupa oil can be used as both edible oil and healthcare food ingredients. The invention has the advantages of simple technological steps, high extraction rate, short extraction duration, low production cost and the like, and can be used for pupa oil preparation from silkworm pupas.
Description
Technical field
The invention belongs to food processing technology field, being specifically related to the silkworm chrysalis is the method that raw material adopts the ultrasonic extraction silkworm chrysalis oil.
Background technology
Natural fats and oils extensively is formed in the bodies of aminal and plant, and is contained in that animal is intravital butter, lard, a sheep wet goods, is contained in that plant is intravital perilla oil, oleum lini, a root of Redsepal Eveningprimrose wet goods.Grease is one of still human essential substance of depending on for existence not, and is important industrial raw material, has purposes widely in technical fields such as food, medicine, makeup, leather industries.Now, world's year per capita oil consumption reach more than 11 kilograms, and China has only 3.1 kilograms, is one of minimum country of oil consumption.China's oil resource wretched insufficiency, domestic soya-bean oil, plam oil, rapeseed oil three big food oils import volumes are all ranked the first in the world, and the import total amount accounts for 18% of global trade amount.Therefore expert call strengthens the grease exploitation, improves the grease extraction yield, strengthens grease yield.
Silkworm chrysalis is a kind of resource of medicine-food two-purpose, it is the main by product of filature industry, 1 ton of raw silk of every production can be produced 1.5 tons of dried silkworm chrysalises, China is the major country of production of silkworm, there is domestic every year more than 200,000 tons the silkworm chrysalis can be for utilizing, but, substantially all is used as feed or fertilizer owing to lack deep process technology, resource utilization is low, causes great waste.Studies show that, contain about 30% fat in the dried silkworm chrysalis, silkworm chrysalis oil can be hydrolyzed into various fatty acid esters, the content of unsaturated fatty acids is very high in the silkworm chrysalis oil, is about 75%, is rich in the linolic acid of needed by human and alpha-linolenic acid etc., its content is about: oleic acid 33%, alpha-linolenic acid 35%, linolic acid 8% contains the unsaponifiables such as β-Gu Zaichun, cholesterol and campesterol more than 1% in addition.The silkworm chrysalis oil nutritive value is abundant; the alpha-linolenic acid that particularly is rich in can be converted into timnodonic acid in human body; be EPA; also can be converted into docosahexenoic acid; be DHA; have improve intelligence, vision protection, delay senility, reducing blood-fat, hypotensive, improve liver function and prevention cardiovascular and cerebrovascular diseases and suppress effects such as senile dementia, can develop and make herbal cuisine homology healthcare products.Simultaneously developing the silkworm chrysalis oil resource energetically can increase domestic grease utilization, alleviates the under-supply present situation of grease.
The method that food oils are produced generally has milling process, organic solvent extraction.In recent years, supercritical carbon dioxide extraction method has been subjected to extensively paying attention to and research as a kind of new extracting process.About the extraction of silkworm chrysalis oil, the organic solvent extractionprocess cost is low, power consumption is little, but has the long and not high shortcoming of extraction yield of extraction time; Supercritical carbon dioxide extraction method extraction yield height, extraction time are short, but big to equipment requirements height, power consumption, and easily cause line clogging when extracting, and the industrial production cost is higher, and problem is more in the technological process; Ultrasonic wave auxiliary extraction method yet there are no report aspect the silkworm chrysalis oil extraction, but the rate of mass transfer and the effect of the sepn process of ultrasonic wave strengthening extraction, thus help greasy extraction.
Summary of the invention
Technical problem to be solved by this invention be to provide a kind of easy and simple to handle, extraction yield is high, extraction time is short, production cost is low extracts the method for silkworm chrysalis oil with ultrasonic wave from silkworm chrysalis.
Solving the problems of the technologies described above the technical scheme that is adopted is that it is made up of following step:
1, silkworm chrysalis pre-treatment
Silkworm chrysalis is put into air dry oven, and 80～120 ℃ of oven dry to its water content are 6%～10%, are ground into powdery with pulverizer, cross 30～80 mesh sieves.
2, ultrasonic extraction
Dried silkworm chrysalis meal is packed in the container, add normal hexane or sherwood oil or cyclohexane extract solvent, dried silkworm chrysalis meal is 1: 3～6 with the mass ratio that extracts solvent, is warming up to 20～50 ℃, with ultrasonic generator power is the ultrasonication 30～40 minutes of 120～150W, collects extracting solution.
3, preparation silkworm chrysalis oil
Extracting solution is collected filtrate with 3～5 layer of 100～250 order filtered through gauze, with centrifugal 10～30 minutes of 1500～4000 rev/mins in whizzer, collects supernatant liquor, in decompression evaporator 40～50 ℃ ,-the 0.08MPa underpressure distillation, reclaim and extract solvent, silkworm chrysalis oil.
4, refining
Prepared silkworm chrysalis oil is heated to 70 ℃, adds to account for silkworm chrysalis oil quality phosphoric acid or citric acid O.05%～0.12%, mixes, and keeps 5 minutes, comes unstuck; When the silkworm chrysalis oil temperature was 45 ℃, the adding massfraction was 14% the NaOH or the KOH aqueous solution, and addition is that 74.4%, 40～60 rev/mins of silkworm chrysalis oil quality stirred 30～40 minutes, and the silkworm chrysalis oil temperature is controlled at 60～65 ℃, and centrifugation oil soap carries out depickling; Add the bleaching clay that accounts for silkworm chrysalis oil quality 4% in the silkworm chrysalis oil after the depickling, the silkworm chrysalis oil temperature is controlled at 40～42 ℃, and 120 rev/mins were stirred 30 minutes, and the filtering separation bleaching clay gets the refining silkworm chrysalis oil.
Above-mentioned bleaching clay is produced by positive Tonghua, Guangzhou worker company limited.
In ultrasonic extraction step 2 of the present invention, dried silkworm chrysalis meal is packed in the container, add normal hexane or sherwood oil or cyclohexane extract solvent, dried silkworm chrysalis meal is 1: 4～6 with the preferred mass ratio that extracts solvent, preferably be warming up to 30～50 ℃, with the preferred power of ultrasonic generator is the ultrasonication 30～40 minutes of 120～150W, collects extracting solution.
In ultrasonic extraction step 2 of the present invention, dried silkworm chrysalis meal is packed in the container, add normal hexane or sherwood oil or cyclohexane extract solvent, dried silkworm chrysalis meal is 1: 4 with the optimum quality ratio that extracts solvent, optimum temperature rise to 40 ℃, with the ultrasonic generator best power is the ultrasonication 30 minutes of 120W, collects extracting solution.
The present invention compares with solvent extraction method, has adopted the ultrasonic extraction step, and extraction time shortened to 30 minutes by 2 hours, and extraction yield brings up to 96.3% by 81.1%, and the product yield brings up to 28.9% by 24.3%.The silkworm chrysalis oil of employing the present invention preparation after testing, the unsaturated fatty acids relative content is 74.7%, especially alpha-linolenic acid content is abundant, and wherein: oleic acid is 37.6%, alpha-linolenic acid is 30.9%, linolic acid is 4.5%, Zoomeric acid is 1.2%, arachidonic acid is 0.5%; Prepared silkworm chrysalis oil presents yellow, and the salted cake fried in sesame oil flavor is arranged, and every index meets the silkworm chrysalis oil quality standard and GB15306-2004 " rapeseed oil " quality standard of bibliographical information, can be used as edible oil, also can be used as the protective foods base-material.The present invention has advantages such as processing step is simple, extraction yield is high, extraction time is short, production cost is low, can be used for preparing from silkworm chrysalis silkworm chrysalis oil.
Embodiment
The present invention is described in more detail below in conjunction with embodiment, but the invention is not restricted to these embodiment.
Embodiment 1
Extracting silkworm chrysalis oil with raw materials used dried silkworm chrysalis meal 100g is that example used other raw materials and extracting method thereof are as follows:
1, silkworm chrysalis pre-treatment
Get silkworm chrysalis and put into air dry oven, 80～120 ℃ of oven dry to its water content are 6%～10%, are ground into powdery with pulverizer, cross 30～80 mesh sieves.
2, ultrasonic extraction
Dried silkworm chrysalis meal 100g packs in the container, adds 400g normal hexane extraction solvent, and dried silkworm chrysalis meal is 1: 4 with the mass ratio that extracts solvent, is warming up to 40 ℃, is the ultrasonication 30 minutes of 120W with ultrasonic generator power, the collection extracting solution.
3, preparation silkworm chrysalis oil
Extracting solution is collected filtrate with 3～5 layer of 100～250 order filtered through gauze, with centrifugal 10～30 minutes of 1500～4000 rev/mins in whizzer, collects supernatant liquor, in decompression evaporator 40～50 ℃ ,-the 0.08MPa underpressure distillation, reclaim and extract solvent, silkworm chrysalis oil.
4, refining
Prepared silkworm chrysalis oil is heated to 70 ℃, adds the phosphoric acid that accounts for silkworm chrysalis oil quality 0.08%, mixes, and keeps 5 minutes, comes unstuck; When the silkworm chrysalis oil temperature was 45 ℃, the adding massfraction was 14% the NaOH aqueous solution, and addition is that 74.4%, 40～60 rev/mins of silkworm chrysalis oil quality stirred 30～40 minutes, and the silkworm chrysalis oil temperature is controlled at 60～65 ℃, and centrifugation oil soap carries out depickling; Add the bleaching clay that accounts for silkworm chrysalis oil quality 4% in the silkworm chrysalis oil after the depickling, the silkworm chrysalis oil temperature is controlled at 40～42 ℃, and 120 rev/mins were stirred 30 minutes, and the filtering separation bleaching clay gets the refining silkworm chrysalis oil.
Embodiment 2
Extracting silkworm chrysalis oil with raw materials used dried silkworm chrysalis meal 100g is that example used other raw materials and extracting method thereof are as follows:
In ultrasonic extraction step 2, dried silkworm chrysalis meal 100g packs in the container, adds 300g normal hexane extraction solvent, and dried silkworm chrysalis meal is 1: 3 with the mass ratio that extracts solvent, and other steps of this step are identical with embodiment 1, are prepared into silkworm chrysalis oil.In refinement step 4, prepared silkworm chrysalis oil is heated to 70 ℃, adds the phosphoric acid that accounts for silkworm chrysalis oil quality 0.05%, mixes, and keeps 5 minutes, comes unstuck, and other steps of this step are identical with embodiment 1.Other steps are identical with embodiment 1, are prepared into the refining silkworm chrysalis oil.
Embodiment 3
Extracting silkworm chrysalis oil with raw materials used dried silkworm chrysalis meal 100g is that example used other raw materials and extracting method thereof are as follows:
In ultrasonic extraction step 2, dried silkworm chrysalis meal 100g packs in the container, adds 600g normal hexane extraction solvent, and dried silkworm chrysalis meal is 1: 6 with the mass ratio that extracts solvent, and other steps of this step are identical with embodiment 1, are prepared into silkworm chrysalis oil.In refinement step 4, prepared silkworm chrysalis oil is heated to 70 ℃, adds the phosphoric acid that accounts for silkworm chrysalis oil quality 0.12%, mixes, and keeps 5 minutes, comes unstuck, and other steps of this step are identical with embodiment 1.Other steps are identical with embodiment 1, are prepared into the refining silkworm chrysalis oil.
Embodiment 4
Extracting silkworm chrysalis oil with raw materials used dried silkworm chrysalis meal 100g is that example used other raw materials and extracting method thereof are as follows:
In the ultrasonic extraction step 2 of above embodiment 1～3, dried silkworm chrysalis meal 100g packs in the container, adds the normal hexane extraction solvent and replaces with sherwood oil, and consumption is identical with respective embodiments, and other steps of this step are identical with embodiment 1.Other steps are identical with embodiment 1, are prepared into the refining silkworm chrysalis oil.
Embodiment 5
Extracting silkworm chrysalis oil with raw materials used dried silkworm chrysalis meal 100g is that example used other raw materials and extracting method thereof are as follows:
In the ultrasonic extraction step 2 of above embodiment 1～3, dried silkworm chrysalis meal 100g packs in the container, adds the normal hexane extraction solvent and replaces with hexanaphthene, and consumption is identical with respective embodiments, and other steps of this step are identical with respective embodiments.Other steps are identical with embodiment 1, are prepared into the refining silkworm chrysalis oil.
Embodiment 6
Extracting silkworm chrysalis oil with raw materials used dried silkworm chrysalis meal 100g is that example used other raw materials and extracting method thereof are as follows:
In the refinement step 4 of above embodiment 1～5, used phosphoric acid such as uses to replace at the citric acid of quality, adding massfraction and be 14% the NaOH aqueous solution, the massfraction of quality such as to use be that 14% the KOH aqueous solution is replaced, 40～60 rev/mins were stirred 30～40 minutes, the silkworm chrysalis oil temperature is controlled at 60～65 ℃, centrifugation oil soap carries out depickling, and other steps of this step are identical with embodiment 1.Other steps are identical with respective embodiments, are prepared into the refining silkworm chrysalis oil.
Embodiment 7
Extracting silkworm chrysalis oil with raw materials used dried silkworm chrysalis meal 100g is that example used other raw materials and extracting method thereof are as follows:
In the ultrasonic extraction step 2 of above embodiment 1～6, dried silkworm chrysalis meal 100g packs in the container, used extraction solvent is identical with respective embodiments with consumption, dried silkworm chrysalis meal is warming up to 50 ℃ with the extraction solvent, with ultrasonic generator power is the ultrasonication 40 minutes of 120W, collects extracting solution.Other steps are identical with respective embodiments, are prepared into the refining silkworm chrysalis oil.
Embodiment 8
Extracting silkworm chrysalis oil with raw materials used dried silkworm chrysalis meal 100g is that example used other raw materials and extracting method thereof are as follows:
In the ultrasonic extraction step 2 of above embodiment 1～6, dried silkworm chrysalis meal 100g packs in the container, used extraction solvent is identical with respective embodiments with consumption, dried silkworm chrysalis meal is warming up to 20 ℃ with the extraction solvent, with ultrasonic generator power is the ultrasonication 30 minutes of 150W, collects extracting solution.Other steps are identical with respective embodiments.Be prepared into the refining silkworm chrysalis oil.
In order to determine raw materials used best proportioning and the processing step of the present invention, the contriver has carried out a large amount of laboratory study tests, every kind of test triplicate, and experimental result is the mean value of three revision tests, various test situation are as follows:
Material: silkworm chrysalis: available from Shaanxi Province's Ankang City.
Fatty acid methyl ester standard substance: available from the gloomy biological products in Wal company limited, purity＞99%.
Reagent: normal hexane, sherwood oil, glacial acetic acid isochromatic spectrum reagent are chromatographically pure, and other reagent are analytical pure.
Laboratory apparatus: gas chromatograph, a day island proper Tianjin produces; FW400A type high speed Universalpulverizer, big Yongxing Instr Ltd. of Beijing section produces; LXJ-II type whizzer, the Shanghai medical apparatus is analyzed factory and is produced; 2WAJ type Abbe refractometer, opticinstrument company limited in Shanghai produces; KQ type ultrasonic generator, Kunshan Ultrasonic Instruments Co., Ltd. produces; BS224S type electronic analytical balance (precision 0.1mg), Beijing Sai Duolisi instrument system company limited produces; RE-52AA type Rotary Evaporators, Shanghai Yarong Biochemical Instrument Plant produces; GZX-9146MBE digital display air dry oven, Medical Equipment Plant of Shanghai Boxun Industrial Co., Ltd. produces; SZY-06 type fat test instrument, the production of the special instrument electricity of last sea cowry instrument factory.
1, ultrasonic extraction choice of Solvent
Get the dried silkworm chrysalis meal 300g that pulverized 30～80 mesh sieves, be divided into 3 parts, be respectively charged in the container, taking by weighing hexanaphthene, sherwood oil, each 400g of normal hexane joins in the container for extracting solvent, be warming up to 40 ℃, with ultrasonic generator power is the ultrasonication 30 minutes of 120W, collect extracting solution, with 3～5 layer of 100～250 order filtered through gauze, collect filtrate, centrifugal 10～30 minutes with 1500～4000 rev/mins in whizzer, collect supernatant liquor, in decompression evaporator 40～50 ℃ ,-the 0.08MPa underpressure distillation, reclaim to extract solvent, silkworm chrysalis oil.The yield of silkworm chrysalis oil is calculated by following formula:
η＝G2/G1×100??????????????????????????????(1)
η is silkworm chrysalis oil yield (%) in the formula, and G1 is the quality (g) of dried silkworm chrysalis meal, and G2 is the quality (g) of silkworm chrysalis oil.
Experiment and calculation result see Table 1.
Table 1 extracts the influence of solvent to the silkworm chrysalis oil yield
| Extract solvent | Yield (%) |
| Hexanaphthene | ??27.1 |
| Extract solvent | Yield (%) |
| Sherwood oil | ??28.1 |
| Normal hexane | ??28.9 |
By table 1 as seen, normal hexane, sherwood oil, hexanaphthene are that the yield of silkworm chrysalis oil is higher when extracting solvent, and normal hexane is for extracting solvent, and the yield of silkworm chrysalis oil is the highest.Selective extraction solvent of the present invention is normal hexane or sherwood oil or hexanaphthene, and the best is a normal hexane.
2, the mass ratio of dried silkworm chrysalis meal and extraction solvent is to the influence of silkworm chrysalis oil yield
Taking by weighing dried silkworm chrysalis meal 500g is divided into 5 parts and is respectively charged in the container, with the normal hexane is to extract solvent, taking by weighing normal hexane 200g, 300g, 400g, 500g, 600g joins respectively in 5 containers, other steps are identical with experiment 1, get silkworm chrysalis oil, by formula (1) calculates the yield of silkworm chrysalis oil, and experiment and calculation result see Table 2.
Table 2 dried silkworm chrysalis meal and the influence of the mass ratio that extracts solvent to the silkworm chrysalis oil yield
| Dried silkworm chrysalis meal and the mass ratio that extracts solvent | Yield (%) |
| ??1∶2 | ??14.3 |
| ??1∶3 | ??22.3 |
| ??1∶4 | ??28.1 |
| ??1∶5 | ??28.4 |
| ??1∶6 | ??28.7 |
By table 2 as seen, the yield of silkworm chrysalis oil increases with the increase of dried silkworm chrysalis meal with the mass ratio that extracts solvent, dried silkworm chrysalis meal all can reach the higher extracted yield with the mass ratio 1: 3～6 that extracts solvent, the mass ratio of dried silkworm chrysalis meal and extraction solvent was greater than 1: 4 o'clock, the silkworm chrysalis oil yield increases slowly, consider cost factor, the present invention selects dried silkworm chrysalis meal and the mass ratio 1: 3～6 that extracts solvent, and the best is 1: 4.
3, ultrasonic power is to the influence of silkworm chrysalis oil yield
Taking by weighing dried silkworm chrysalis meal 500g is divided into 5 parts and is respectively charged in the container, with the normal hexane is to extract solvent, taking by weighing normal hexane 2000g is divided into 5 parts and joins respectively in 5 containers, be warming up to 40 ℃, with ultrasonic generator power be respectively 30,60,90,120, the ultrasonication of 150W 30 minutes, other steps are identical with experiment 1, silkworm chrysalis oil, by formula (1) calculates the yield of silkworm chrysalis oil, and experiment and calculation result see Table 3.
Table 3 ultrasonic power is to the influence of silkworm chrysalis oil yield
| Ultrasonic power (W) | Yield (%) |
| ??30 | ??23.5 |
| Ultrasonic power (W) | Yield (%) |
| ??60 | ??25.4 |
| ??90 | ??26.8 |
| ??120 | ??28.6 |
| ??150 | ??27.2 |
By table 3 as seen, ultrasonic power is that 120～150W handles dried silkworm chrysalis meal and extracts solvent, and the silkworm chrysalis oil yield is higher, and ultrasonic power is at 120W, and the silkworm chrysalis oil yield is the highest.It is 120～150W that the present invention selects ultrasonic extraction power, and the best is 120W.
4, ultrasonic treatment time is to the influence of silkworm chrysalis oil yield
Taking by weighing dried silkworm chrysalis meal 400g is divided into 4 parts and is respectively charged in the container, with the normal hexane is to extract solvent, taking by weighing normal hexane 1600g is divided into 4 parts and joins respectively in 4 containers, be warming up to 40 ℃ of ultrasonic temperature, with ultrasonic generator power is that the ultrasonic wave of 120W was handled respectively 10,20,30,40 minutes, and other steps are identical with experiment 1, silkworm chrysalis oil, by formula (1) calculates the yield of silkworm chrysalis oil, and experiment and calculation result see Table 4.
Table 4 ultrasonic treatment time is to the influence of silkworm chrysalis oil yield
| Ultrasonic treatment time (minute) | Yield (%) |
| ??10 | ??25.1 |
| ??20 | ??25.8 |
| ??30 | ??28.4 |
| ??40 | ??26.8 |
By table 4 as seen, ultrasonication 30～40 minutes, the yield of silkworm chrysalis oil is higher, ultrasonication 30 minutes, the yield of silkworm chrysalis oil is the highest.It is 30～40 minutes that the present invention selects ultrasonic treatment time, and the best is 30 minutes.
5, extract the influence of temperature to the silkworm chrysalis oil yield
Taking by weighing dried silkworm chrysalis meal 400g and be divided into 4 parts and be respectively charged in the container, is to extract solvent with the normal hexane, takes by weighing normal hexane 1600g and is divided into 4 parts and joins respectively in 4 containers, is warming up to 20,30,40,50 ℃.Other steps are identical with experiment 1, get silkworm chrysalis oil, and by formula (1) calculates the yield of silkworm chrysalis oil, and experiment and calculation result see Table 5.
Table 5 extracts the influence of temperature to the silkworm chrysalis oil yield
| The extraction temperature (℃) | Yield (%) |
| ??20 | ??25.9 |
| The extraction temperature (℃) | Yield (%) |
| ??30 | ??26.8 |
| ??40 | ??28.2 |
| ??50 | ??27.3 |
By table 5 as seen, when the extraction temperature was 20～50 ℃, the yield of silkworm chrysalis oil was higher, and the yield of silkworm chrysalis oil was the highest when the extraction temperature was 40 ℃.Selective extraction temperature of the present invention is 20～50 ℃, and the best is 40 ℃.
6, the silkworm chrysalis oil yield of ultrasonic extraction preparation and extraction yield and solvent method contrast
Be the reliability of check optimum result of the present invention, adopt above-mentioned optimal conditions to carry out three repeated authentication experiments, i.e. it is that 120W, ultrasonic treatment time are 30 minutes, to extract temperature be 40 ℃ that ultrasonication power is adopted in three repeated authentication experiments.
The silkworm chrysalis oil of ultrasonic extraction and solvent-extraction process extract yield (1) calculating by formula of silkworm chrysalis oil, and extraction yield is calculated as follows:
P(％)＝η/M×100????????????????????????????(2)
P is silkworm chrysalis oil extraction yield (%) in the formula, and η is silkworm chrysalis oil yield (%), and M is a grease total content (%) in the dried silkworm chrysalis meal.
Experiment and calculation result see Table 6.
The silkworm chrysalis oil of table 6 solvent-extraction process and ultrasonic extraction preparation relatively
| Extracting method | Solvent-extraction process | Ultrasonic extraction |
| Oil yield (yield) (%) | ??24.3±0.134 | ??28.9±0.156 |
| Extraction yield (%) | ??81.1±1.035 | ??96.3±1.106 |
By table 6 as seen, the present invention compares with solvent-extraction process, and the present invention extracts the yield of silkworm chrysalis oil and brings up to 28.9% by 24.33%, and extraction yield brings up to 96.3% by 81.1%, and extraction time shortened to 30 minutes by 2 hours.
In order to verify beneficial effect of the present invention, the contriver adopts the silkworm chrysalis oil of the embodiment of the invention 1 preparation to test, and various tests are as follows:
1, Organoleptic Inspection
Color and luster: yellow.
Smell: salted cake fried in sesame oil flavor.
Outward appearance: evenly, no foreign matter and throw out.
2, the silkworm chrysalis oil physical and chemical index of ultrasonic extraction preparation and national standard contrast
According to GB/T 5530-2005 " animal-plant oil acid number and acid test ", GB/T 5532-2008 " mensuration of animal-plant oil iodine number ", GB/T5527-1985 " Vegetable oil lipoprotein check refractive index assay method ", GB5526-1985 " Vegetable oil lipoprotein check measurement of specific gravity ", carried out the analysis of silkworm chrysalis oil physical and chemical index, measurement result and relatively see Table 7 with the rapeseed oil national standard.
Table 7 silkworm chrysalis oil quality and rapeseed oil national standard are relatively
| Index name | The rapeseed oil national standard | The silkworm chrysalis oil of bibliographical information | The silkworm chrysalis oil of the present invention's preparation |
| Outward appearance | Faint yellow transparent | Faint yellow transparent | Golden transparent |
| Smell | Normal free from extraneous odour | Normal free from extraneous odour | Normal free from extraneous odour |
| Acid number (mgKOH/g) | ≤ 0.20 (one-level) | ??≤0.2 | ??0.2 |
| Iodine value (gI 2/100g) | ??94～120 | ??130～138 | ??138 |
| Proportion (20/4 ℃) | ??0.910～0.920 | ??0.914～0.918 | ??0.919 |
| Refractive index | ??1.465～1.469 | ??1.4670 |
By table 7 as seen, the silkworm chrysalis oil of employing the present invention preparation and the silkworm chrysalis oil standard of bibliographical information and approaching with the every quality index in the rapeseed oil national standard reach GB1536-2004 " rapeseed oil " quality standard.
3, the silkworm chrysalis oil fatty acid component is analyzed:
Adopt the silkworm chrysalis oil of the embodiment of the invention 1 preparation the lipid acid composition to be analyzed with vapor-phase chromatography.Chromatographic condition: PEG-20M capillary column (30m * 0.25mm * 0.25 μ m); Column temperature: 195 ℃ of constant temperature kept 50 minutes; Input mode is no split stream sampling, and sample size is 1 μ L; Carrier gas is Ne, flow velocity 30mL/min; 225 ℃ of injector temperatures; 300 ℃ of fid detector temperature.
Test-results sees Table 8.
Table 8 silkworm chrysalis oil lipid acid is formed
| Lipid acid | Content (%) |
| Palmitinic acid (C16:0) | ??21.8 |
| Zoomeric acid (C16:1) | ??1.2 |
| Stearic acid (C18:0) | ??2.4 |
| Oleic acid (C18:1) | ??37.6 |
| Linolic acid (C18:2) | ??4.5 |
| Linolenic acid (C18:3) | ??30.9 |
| Arachidonic acid (C20:4) | ??0.5 |
| Other | ??1.1 |
By table 8 as seen, the unsaturated fatty acids relative content is 74.7%, and visible silkworm chrysalis oil contains a large amount of polyunsaturated fatty acids, and nutritive value is abundant.
Shown that by above experimental study the present invention compares with existing silkworm chrysalis oil extracting method, the silkworm chrysalis oil recovery rate obviously improves, and asks during extraction greatly and shortens, and technical process is simple, stable, is suitable for suitability for industrialized production. Adopt the present invention to extract the silkworm chrysalis oil product and present yellow, has the peculiar salted cake fried in sesame oil flavor of silkworm chrysalis oil, because silkworm chrysalis oil is at present without state quality standard, contrast with vegetable seed wet goods edible oil, indices meets GB1536-2004 " rapeseed oil " quality standard, polyunsaturated fatty acid, especially alpha-linolenic acid rich content are rich in the fatty acid compositional analysis demonstration, are a kind of nutrition and health care greases that better nutritivity is worth that has.
Claims (3)
1. one kind is extracted the method for silkworm chrysalis oil with ultrasonic wave from silkworm chrysalis, it is characterized in that it is made up of following step:
(1) silkworm chrysalis pre-treatment
Silkworm chrysalis is put into air dry oven, and 80～120 ℃ of oven dry to its water content are 6%～10%, are ground into powdery with pulverizer, cross 30～80 mesh sieves;
(2) ultrasonic extraction
Dried silkworm chrysalis meal is packed in the container, add normal hexane or sherwood oil or cyclohexane extract solvent, dried silkworm chrysalis meal is 1: 3～6 with the mass ratio that extracts solvent, is warming up to 20～50 ℃, with ultrasonic generator power is the ultrasonication 30～40 minutes of 120～150W, collects extracting solution;
(3) preparation silkworm chrysalis oil
Extracting solution is collected filtrate with 3～5 layer of 100～250 order filtered through gauze, with centrifugal 10～30 minutes of 1500～4000 rev/mins in whizzer, collects supernatant liquor, in decompression evaporator 40～50 ℃ ,-the 0.08MPa underpressure distillation, reclaim and extract solvent, silkworm chrysalis oil;
(4) refining
Prepared silkworm chrysalis oil is heated to 70 ℃, adds the phosphoric acid or the citric acid that account for silkworm chrysalis oil quality 0.05%～0.12%, mixes, and keeps 5 minutes, comes unstuck; When the silkworm chrysalis oil temperature was 45 ℃, the adding massfraction was 14% the NaOH or the KOH aqueous solution, and addition is that 74.4%, 40～60 rev/mins of silkworm chrysalis oil quality stirred 30～40 minutes, and the silkworm chrysalis oil temperature is controlled at 60～65 ℃, and centrifugation oil soap carries out depickling; Add the bleaching clay that accounts for silkworm chrysalis oil quality 4% in the silkworm chrysalis oil after the depickling, the silkworm chrysalis oil temperature is controlled at 40～42 ℃, and 120 rev/mins were stirred 30 minutes, and the filtering separation bleaching clay gets the refining silkworm chrysalis oil.
2. according to the described method of from silkworm chrysalis, extracting silkworm chrysalis oil with ultrasonic wave of claim 1, it is characterized in that: in ultrasonic extraction step (2), dried silkworm chrysalis meal is packed in the container, add normal hexane or sherwood oil or cyclohexane extract solvent, dried silkworm chrysalis meal is 1: 4～6 with the mass ratio that extracts solvent, being warming up to 30～50 ℃, is the ultrasonication 30～40 minutes of 120～150W with ultrasonic generator power, collects extracting solution.
3. according to the described method of from silkworm chrysalis, extracting silkworm chrysalis oil with ultrasonic wave of claim 1, it is characterized in that: in ultrasonic extraction step (2), dried silkworm chrysalis meal is packed in the container, add normal hexane or sherwood oil or cyclohexane extract solvent, dried silkworm chrysalis meal is 1: 4 with the mass ratio that extracts solvent, being warming up to 40 ℃, is the ultrasonication 30 minutes of 120W with ultrasonic generator power, collects extracting solution; In refinement step (4), prepared silkworm chrysalis oil is heated to 70 ℃, adds the phosphoric acid or the citric acid that account for silkworm chrysalis oil quality 0.08%, mixes, and keeps 5 minutes, comes unstuck; When the silkworm chrysalis oil temperature was 45 ℃, the adding massfraction was 14% the NaOH or the KOH aqueous solution, and addition is that 74.4%, 40～60 rev/mins of silkworm chrysalis oil quality stirred 30～40 minutes, and the silkworm chrysalis oil temperature is controlled at 60～65 ℃, and centrifugation oil soap carries out depickling; Add the bleaching clay that accounts for silkworm chrysalis oil quality 4% in the silkworm chrysalis oil after the depickling, the silkworm chrysalis oil temperature is controlled at 40～42 ℃, and 120 rev/mins were stirred 30 minutes, and the filtering separation bleaching clay gets the refining silkworm chrysalis oil.
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