CN104170845A - Application and preparation method for piperine substances in pepper extract - Google Patents
Application and preparation method for piperine substances in pepper extract Download PDFInfo
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Abstract
The invention relates to the technical field of pesticide application, and in particular relates to application and a preparation method of piperine substances in a pepper extract, and application of the piperine substances in the pepper extract as an insecticide synergist. The piperine substances in the pepper extract disclosed by the invention come from natural plants, is a green and pollution-free product, and has no toxicity to a human body and the environment; the insecticide synergist is the first natural plant-source pesticide synergist in the pesticide history of the world so far, and is an international pioneer; the synergistic effect of the substances on main pesticides is obvious, the insecticidal efficiency of insecticide products with the product disclosed by the invention can be increased by 10.6-30.2% compared with products without the product disclosed by the invention, and the efficacy can be improved by 24.5-30.2% with regard to natural pyrethrin insecticides.
Description
Technical field
The present invention relates to pesticides application technical field, specifically application of pepper alkaloids and preparation method thereof in Fructus Piperis extract.
Background technology
The increase day by day of world population and the continuous minimizing of arable area have determined that agricultural production is to be unable to do without agricultural chemicals within significant period of time from now on.At present, chemical pesticide is the main method of insect control, unfortunately, more and more fact proved, the use of chemical pesticide brings many catastrophic results to the mankind and environment.Over nearly 30 years, the combine result of common development of biotechnology and Pesticide Science has produced multiple and biological material relevant, that have agricultural chemicals function, Here it is biopesticide.Botanical biological pesticide is efficient with it, wide spectrum, and safety, low toxicity and noresidue become a wherein most important class, are known as nuisanceless environmentally friendly machine by the whole world, and are put into first of the agricultural chemicals that international food and agricultural organization recommends use to the utmost.
Botanical biological pesticide toxicity active ingredient extracts from specified plant, this chemical substance is little at plant corpus intensive amount, generally in 5% left and right, some even still less, if the content of chrysanthemum ester composition in Dalmatian chrysanthemum kind is only in 1% left and right, this has just caused such agricultural chemicals use cost high, the situation that is difficult to large scale application.The usage amount that reduces active ingredient in tradition pesticide producing by adding the method for synergist, reduces agricultural chemicals use cost.Pesticide synergistic agent can suppress or weaken the removing toxic substances deactivation of insect to pesticide activity component, and drug effect is brought into play more fully, has promoted the availability of agricultural chemicals main component in insect bodies, thereby reaches the effect that strengthens insecticidal effect.But, up to the present, in pesticide producing, synergist used is artificial synthetic chemical products, some of them have been proved to be environment and human health have been worked the mischief, as used Butacide (Piperonyl Butoxide for many years as broad spectrum activity synergist, PBO), be proved to be as possibility carcinogenic substance, high dose contact can be lethal, since on January 1st, 2006, some countries as Australia, America & Canada etc. are successively forbidden the use of PBO in organic farming, crowd residential area and food processing operation region.Select as early as possible a kind of Nantural non-toxic synergist to substitute the synthetic synergist of traditional chemical industry and become a significant task of modern research field.
Summary of the invention
The present invention, in order to solve the problem of needing at present a kind of Nantural non-toxic synergist badly and substitute the synthetic synergist of traditional chemical industry, provides application of pepper alkaloids in a kind of Fructus Piperis extract and preparation method thereof.
The present invention is achieved by the following technical solutions: in Fructus Piperis extract, pepper alkaloids is in the application as in insecticidal synergist.
Pepper of the present invention be the torrid zone and and subtropical zone comprise some Piperaceaies (Piperaceae) Piper (Piper L.) plant of the ground such as Hainan, the Guangxi growth of China, as black pepper (
piper nigrum), long pepper (
piper longum), piper cubeba (
piper cubeba)deng.When concrete use, Fructus Piperis extract of the present invention mixes with natural pyrethrin, pyrethroid-decis, natural insecticide rotenone etc. respectively by the volume ratio of 6～16:1, its insecticidal effect is significantly better than the spray effect of independent main insecticide, the insecticidal effect drug effects of five kinds of Main Agricultural insects is improved to 10.6～30.2%, similar with the insecticidal effect of insecticide that adds traditional Butacide.
Further, in natural pyrethrin insecticide interpolation Fructus Piperis extract, pepper alkaloids is the application of synergist in the vegetable insecticide of organic foodstuff production chain use.
When concrete use, Fructus Piperis extract of the present invention mixes with natural pyrethrin by the volume ratio of 6～16:1, its insecticidal effect is significantly better than the spray effect of independent natural pyrethrin, the insecticidal effect drug effect of five kinds of Main Agricultural insects is improved to 24.5～30.2%, similar with the natural pyrethrin insecticidal effect that has added traditional Butacide.
The extraction of pepper alkaloids of the present invention can adopt several in effective plant component extracting process.But traditional extraction process is to utilize polar solvent water, ethanol, methyl alcohol and propyl alcohol etc. mostly, or rely on the fluids such as non-polar solven n-hexane, propane and butane, carry out active ingredient extraction by methods such as dipping, diacolation, decoction, refluxing extraction, the required operating temperature of these techniques all, more than 50 DEG C, easily causes active ingredient thermal degradation; Because operation is to carry out under open state, process is loaded down with trivial details tediously long, and the light degradation of extract is increased the weight of simultaneously, and these all cause the loss of active ingredient in manufacturing process; Another one problem is, the dissolvent residual in extract is high, thereby badly influences quality and the grade of extract, and range of application is restricted, if the Pesticidal products using in organic farming is not allow to contain organic solvent; In addition, all organic solvents belong to explosives, inflammable items more, and production process has potential safety hazard.And in traditional pepper alkaloids extraction system, hot environment causes a large amount of impurity to extract with pepper alkaloids, cause extract purity low, poor product quality, especially be the acid pepper oleoresin of solid or semi-solid state, forming to later stage end product formulation has increased difficulty, therefore must carry out degreasing purification.And the degreasing purification technique of present stage need to be used high-risk chemical reagent and the hot conditions such as strong acid, highly basic, diethyl ether, working environment potential danger increases suddenly, and technological process is loaded down with trivial details, time consumption and energy consumption, and poor operability, is not suitable for carrying out large-scale production.
Therefore, the invention provides the preparation method of pepper alkaloids in a kind of Fructus Piperis extract, the steps include:
(1) pepper immature seed is dried, and being crushed to granularity is 5～40 orders, packs in extractor, starts and stirs, and makes the smooth accumulation of material in still; Open vavuum pump and adjust between interior vacuum to the 0.02～0.08MPa of extractor, inject liquid subcritical fluids R134a as solvent, be uniformly mixed with raw material until liquid level exceeds raw material; Controlling extraction temperature in extractor is 30～60 DEG C, and pressure is 0.3～1.0MPa, and immersion extraction time is 30～180min; When soaking extraction, carry out ultrasonic processing, process 1～7 min, intermittently 2～10 min, so iterative cycles; After having extracted, close ultrasonicly, separate solid, liquid phase, liquid phase mixed liquor is delivered into temporary tank; In solid phase waste residue, add solvent and repeat above-mentioned immersion extraction, ultrasonic and separation solid, liquid phase step, re-extract 3～6 times, each time of soaking extraction is 10～60 min;
(2) rely on pressure and solvent pump, the liquid phase mixed liquor in temporary tank is pressed into one-level extraction-container through self-cleaning filter; Liquid phase mixed liquor is repeatedly by tubular heat exchanger, and under the pressure of 30～60 DEG C and 0.3～1.0MPa, the solvent evaporates in liquid phase mixed liquor enters solvent recovering system, and liquid extract stays in one-level extraction-container; Between Pressure Drop to the 0.1～0.2MPa in one-level extraction-container, complete one-level and resolve;
(3) be delivered to secondary extraction-container through the liquid extract of one-level parsing initial gross separation, spray and diffuse to form tiny liquid pearl through injector at kettle top, under the pressure of 30～60 DEG C and 0.3～1.0MPa, residue in solvent in tiny liquid pearl from top to bottom by the process of jacketed heat exchanger, further evaporated;
(4) extract of secondary extraction-container is delivered to extract holding vessel by sanitary pump, obtains pepper alkaloids extract.
The extract output obtaining through above-mentioned preparation method can reach 4.92～25.6%, recovery rate can reach 90～95%, in extract, the content of pepper alkaloids is 11.4～30.8%, extraction rate is 4～6 times of conventional organic solvents extracting method, is independent 2～4 times of adopting subcritical technology (not adding ultrasonic processing) extracting method.The present invention's technique used is to carry out under low temperature, airtight and shading condition, thereby has prevented to a great extent the loss of effective ingredient.
Further, after completing steps (4), pepper alkaloids extract is through CO 2 supercritical purification step.
And, the present invention further provides a kind of CO 2 supercritical purification step, described CO 2 supercritical purification step is: (5) are opened extraction kettle to make its inner pressure decreased be 0MPa, open kettle cover and feed; Material loading completes injection CO in backward still
2, CO
2flow-control is below 30L/h, and regulating extraction temperature in extraction kettle is 20～50 DEG C, and extracting pressure is 5～20MPa, and in separating still, separation temperature is 20～50 DEG C, and separating pressure is 5～20MPa, and extraction time is 30～180min; Collect extract and obtain limpid, transparent, oily liquid pepper alkaloids extract.The content of the pepper alkaloids in the pepper alkaloids extract after above-mentioned purification is 41.2～82.3%.
Pepper alkaloids in Fructus Piperis extract of the present invention, from natural frond, is green non-pollution product, nontoxic to the mankind and environment.Up to the present this be, at world pesticide first historically natural plant pesticide synergistic agent, for initiating the world.This material is obvious to the synergistic effect of main agricultural chemicals, has added that pesticide product of the present invention is comparable not to be added product of the present invention and improve insecticide efficiency 10.6～30.2%, can improve drug effect 24.5～30.2% to natural pyrethrin insecticide.Adding the natural pyrethrin insecticides that pepper alkaloids of the present invention is synergist is unique a kind of vegetable insecticide that can use at organic foodstuff production chain.And traditional synergist is artificial synthetic chemical products, harm and potential hazard that environment and the mankind are caused are huge, and some of them are prohibited from using.The present invention makes the large scale application of modern plants source biological pesticide become possibility, the generation of this Novel non-toxic natural synergic agent, can improve on the one hand the physical property of former medicine, not only extend the service life of original agricultural chemicals, better the effect of performance medicine, reduces dosage, expands range of application, reduce costs, save manpower etc.On the other hand, can bring into play to greatest extent pesticide active ingredient drug effect, decline, improve user's safety, minimizing environmental pollution for drug effect raising, toxicity, there is significant economic benefit and social benefit.
the test of pesticide effectiveness:
Select natural pyrethrin as main insecticide, test is processed and is comprised:
Experimental group: mix with natural pyrethrin with the volume ratio of 6-16:1 as synergist, insecticide working concentration (volumetric concentration) is 0.02% to spray;
Contrast 1: the natural pyrethrin that does not add any synergist sprays with 0.02%;
Contrast 2: traditional Butacide PBO mixes with natural pyrethrin with 10:1 ratio, insecticide working concentration is 0.02% to spray;
Contrast 3: water.
1. flight class pest-mosquito
Experiment is carried out in 5 worm cages, and 20 adult mosquitoes of each processing, after three days, record experimental result (table 1), and experimental group reaches 97.7% to the lethality rate of mosquito, improves 25.6% than the product drug effect of contrast 1, improves 1.9% than the product drug effect of control group 2.
Each group of contrast of the insecticidal effect to mosquito of table 1
2. reptiles insect A-Potato Aphid
Experiment is carried out on field planting Kidney bean, arrangement of time is encroached on plant season without restraint aphid, for 9 strains of examination plant, every leaf has 100 aphids at least, after three days, record result (in table 2), experimental group is 93.5% to the lethality rate of Potato Aphid, improves 22.9% than the product drug effect of contrast 1, improves 2.6% than the product drug effect of control group 2.
Each group of contrast of the insecticidal effect to Potato Aphid of table 2
3. the larva of reptiles insect B-potato ladybug
Test on the 9 strain tomato plants of planting in the courtyard of being in and carry out, after plucking infringement blade, spray medicine, after three days, record experimental result (as table 3), experimental group reaches 98.27% to the lethality rate of ladybug larva, improve 26.9% than the product drug effect of contrast 1, improve 10.06% than the product drug effect of control group 2.
Each group of contrast of the insecticidal effect to potato ladybug of table 3
4. reptiles insect C-Oeobia undalis caterpillar
Experiment is carried out on the green soya bean of field planting, there is the plant tissue of caterpillar to be collected, concentrate and spray medicine experiment, after three days, record experimental result (in table 4), experimental group reaches 98.3% to the lethality rate of Oeobia undalis caterpillar, improves 26.6% than the product drug effect of contrast 1, improves 14.8% than the product drug effect of control group 2.
Each group of contrast of the insecticidal effect to Oeobia undalis caterpillar of table 4
5. reptiles insect D-ant
Tested summer and carry out on silky ant, ant is collected in wide-mouth bottle, every bottle of 10 ants, then spray medicine experiment, after three days, record experimental result (in table 5), experimental group reaches 100% to the lethality rate of ant, improves 26.6% than the product drug effect of contrast 1, improves 14.8% than the product drug effect of control group 2.
Each group of contrast of the insecticidal effect to ant of table 5
Embodiment
embodiment 1
The preparation method of pepper alkaloids in Fructus Piperis extract, described pepper be black pepper (
piper nigrum), the steps include:
(1) black pepper immature seed is dried, and being crushed to granularity is 5 orders, packs in extractor, starts and stirs, and makes the smooth accumulation of material in still; Open vavuum pump and adjust between interior vacuum to the 0.02～0.08MPa of extractor, inject liquid subcritical fluids R134a as solvent, be uniformly mixed with raw material until liquid level exceeds raw material; Controlling extraction temperature in extractor is 40 DEG C, and pressure is 1.0MPa, and immersion extraction time is 100min; When soaking extraction, carry out ultrasonic processing, process 1 min, intermittently 6 min, so iterative cycles; After having extracted, close ultrasonicly, separate solid, liquid phase, liquid phase mixed liquor is delivered into temporary tank; In solid phase waste residue, add solvent and repeat above-mentioned immersion extraction, ultrasonic and separation solid, liquid phase step, re-extract 6 times, each time of soaking extraction is 30 min;
(2) rely on pressure and solvent pump, the liquid phase mixed liquor in temporary tank is pressed into one-level extraction-container through self-cleaning filter; Liquid phase mixed liquor is repeatedly by tubular heat exchanger, and under the pressure of 30 DEG C and 0.7MPa, the solvent evaporates in liquid phase mixed liquor enters solvent recovering system, and liquid extract stays in one-level extraction-container; Between Pressure Drop to the 0.1～0.2MPa in one-level extraction-container, complete one-level and resolve;
(3) be delivered to secondary extraction-container through the liquid extract of one-level parsing initial gross separation, spray and diffuse to form tiny liquid pearl through injector at kettle top, under the pressure of 60 DEG C and 1.0MPa, residue in solvent in tiny liquid pearl from top to bottom by the process of jacketed heat exchanger, further evaporated;
(4) extract of secondary extraction-container is delivered to extract holding vessel by sanitary pump, obtains pepper alkaloids extract.The extract output obtaining through above-mentioned preparation method can reach 25.6%, and in extract, the content of pepper alkaloids is 30.2%.
After completing steps (4), pepper alkaloids extract is through CO 2 supercritical purification step, and described CO 2 supercritical purification step is: (5) are opened extraction kettle to make its inner pressure decreased be 0MPa, open kettle cover and feed; Material loading completes injection CO in backward still
2, CO
2flow-control is below 30L/h, and regulating extraction temperature in extraction kettle is 20 DEG C, and extracting pressure is 13MPa, and in separating still, separation temperature is 50 DEG C, and separating pressure is 13MPa, and extraction time is 30min; Collect extract and obtain limpid, transparent, oily liquid pepper alkaloids extract.The content of the pepper alkaloids in the pepper alkaloids extract after above-mentioned purification is 82.3%.
When concrete enforcement, Fructus piperis nigrum extract of the present invention is pressed the volume ratio of 10:1 and is mixed with natural pyrethrin, its insecticidal effect is significantly better than the spray effect of independent natural pyrethrin, the insecticidal effect drug effect of five kinds of Main Agricultural insects is improved to 30.2%, similar with the natural pyrethrin insecticidal effect that has added traditional Butacide.
embodiment 2
The preparation method of pepper alkaloids in Fructus Piperis extract, described pepper for long pepper (
piper longum), the steps include:
(1) grow pepper immature seed and dry, being crushed to granularity is 20 orders, packs in extractor, starts and stirs, and makes the smooth accumulation of material in still; Open vavuum pump and adjust between interior vacuum to the 0.02～0.08MPa of extractor, inject liquid subcritical fluids R134a as solvent, be uniformly mixed with raw material until liquid level exceeds raw material; Controlling extraction temperature in extractor is 60 DEG C, and pressure is 0.7MPa, and immersion extraction time is 30min; When soaking extraction, carry out ultrasonic processing, process 4 min, intermittently 10 min, so iterative cycles; After having extracted, close ultrasonicly, separate solid, liquid phase, liquid phase mixed liquor is delivered into temporary tank; In solid phase waste residue, add solvent and repeat above-mentioned immersion extraction, ultrasonic and separation solid, liquid phase step, re-extract 5 times, each time of soaking extraction is 10 min;
(2) rely on pressure and solvent pump, the liquid phase mixed liquor in temporary tank is pressed into one-level extraction-container through self-cleaning filter; Liquid phase mixed liquor is repeatedly by tubular heat exchanger, and under the pressure of 50 DEG C and 1.0MPa, the solvent evaporates in liquid phase mixed liquor enters solvent recovering system, and liquid extract stays in one-level extraction-container; Between Pressure Drop to the 0.1～0.2MPa in one-level extraction-container, complete one-level and resolve;
(3) be delivered to secondary extraction-container through the liquid extract of one-level parsing initial gross separation, spray and diffuse to form tiny liquid pearl through injector at kettle top, under the pressure of 30 DEG C and 0.7MPa, residue in solvent in tiny liquid pearl from top to bottom by the process of jacketed heat exchanger, further evaporated;
(4) extract of secondary extraction-container is delivered to extract holding vessel by sanitary pump, obtains pepper alkaloids extract.The extract output obtaining through above-mentioned preparation method can reach 18.7%, and in extract, the content of pepper alkaloids is 24.9%.
After completing steps (4), pepper alkaloids extract is through CO 2 supercritical purification step, and described CO 2 supercritical purification step is: (5) are opened extraction kettle to make its inner pressure decreased be 0MPa, open kettle cover and feed; Material loading completes injection CO in backward still
2, CO
2flow-control is below 30L/h, and regulating extraction temperature in extraction kettle is 40 DEG C, and extracting pressure is 20MPa, and in separating still, separation temperature is 30 DEG C, and separating pressure is 5MPa, and extraction time is 100min; Collect extract and obtain limpid, transparent, oily liquid pepper alkaloids extract.The content of the pepper alkaloids in the pepper alkaloids extract after above-mentioned purification is 67.1%.
When concrete enforcement, long Fructus Piperis extract of the present invention is pressed the volume ratio of 16:1 and is mixed with pyrethroid-decis, its insecticidal effect is significantly better than the spray effect of independent pyrethroid-decis, the insecticidal effect drug effect of five kinds of Main Agricultural insects is improved to 27.8%, similar with the pyrethroid-decis insecticidal effect that has added traditional Butacide.
embodiment 3
The preparation method of pepper alkaloids in Fructus Piperis extract, described pepper be piper cubeba (
piper cubeba), the steps include:
(1) piper cubeba immature seed is dried, and being crushed to granularity is 40 orders, packs in extractor, starts and stirs, and makes the smooth accumulation of material in still; Open vavuum pump and adjust between interior vacuum to the 0.02～0.08MPa of extractor, inject liquid subcritical fluids R134a as solvent, be uniformly mixed with raw material until liquid level exceeds raw material; Controlling extraction temperature in extractor is 30 DEG C, and pressure is 0.3MPa, and immersion extraction time is 180min; When soaking extraction, carry out ultrasonic processing, process 7 min, intermittently 2 min, so iterative cycles; After having extracted, close ultrasonicly, separate solid, liquid phase, liquid phase mixed liquor is delivered into temporary tank; In solid phase waste residue, add solvent and repeat above-mentioned immersion extraction, ultrasonic and separation solid, liquid phase step, re-extract 3 times, each time of soaking extraction is 60 min;
(2) rely on pressure and solvent pump, the liquid phase mixed liquor in temporary tank is pressed into one-level extraction-container through self-cleaning filter; Liquid phase mixed liquor is repeatedly by tubular heat exchanger, and under the pressure of 60 DEG C and 0.3MPa, the solvent evaporates in liquid phase mixed liquor enters solvent recovering system, and liquid extract stays in one-level extraction-container; Between Pressure Drop to the 0.1～0.2MPa in one-level extraction-container, complete one-level and resolve;
(3) be delivered to secondary extraction-container through the liquid extract of one-level parsing initial gross separation, spray and diffuse to form tiny liquid pearl through injector at kettle top, under the pressure of 50 DEG C and 0.3MPa, residue in solvent in tiny liquid pearl from top to bottom by the process of jacketed heat exchanger, further evaporated;
(4) extract of secondary extraction-container is delivered to extract holding vessel by sanitary pump, obtains pepper alkaloids extract.The extract output obtaining through above-mentioned preparation method can reach 4.92%, and in extract, the content of pepper alkaloids is 11.4%.
After completing steps (4), pepper alkaloids extract is through CO 2 supercritical purification step, and described CO 2 supercritical purification step is: (5) are opened extraction kettle to make its inner pressure decreased be 0MPa, open kettle cover and feed; Material loading completes injection CO in backward still
2, CO
2flow-control is below 30L/h, and regulating extraction temperature in extraction kettle is 50 DEG C, and extracting pressure is 5MPa, and in separating still, separation temperature is 20 DEG C, and separating pressure is 20MPa, and extraction time is 180min; Collect extract and obtain limpid, transparent, oily liquid pepper alkaloids extract.The content of the pepper alkaloids in the pepper alkaloids extract after above-mentioned purification is 41.2%.
When concrete enforcement, piper cubeba extract of the present invention is pressed the volume ratio of 6:1 and is mixed with natural insecticide rotenone, its insecticidal effect is significantly better than the spray effect of independent natural insecticide rotenone, the insecticidal effect drug effect of five kinds of Main Agricultural insects is improved to 24.5%, similar with the natural insecticide rotenone insecticidal effect that has added traditional Butacide.
Claims (5)
- In Fructus Piperis extract pepper alkaloids in the application as in insecticidal synergist.
- 2. in natural pyrethrin insecticide interpolation Fructus Piperis extract, pepper alkaloids is the application of synergist in the vegetable insecticide of organic foodstuff production chain use.
- 3. the preparation method of pepper alkaloids in Fructus Piperis extract as claimed in claim 1 or 2, is characterized in that, the steps include:(1) pepper immature seed is dried, and being crushed to granularity is 5～40 orders, packs in extractor, starts and stirs, and makes the smooth accumulation of material in still; Open vavuum pump and adjust between interior vacuum to the 0.02～0.08MPa of extractor, inject liquid subcritical fluids R134a as solvent, be uniformly mixed with raw material until liquid level exceeds raw material; Controlling extraction temperature in extractor is 30～60 DEG C, and pressure is 0.3～1.0MPa, and immersion extraction time is 30～180min; When soaking extraction, carry out ultrasonic processing, process 1～7 min, intermittently 2～10 min, so iterative cycles; After having extracted, close ultrasonicly, separate solid, liquid phase, liquid phase mixed liquor is delivered into temporary tank; In solid phase waste residue, add solvent and repeat above-mentioned immersion extraction, ultrasonic and separation solid, liquid phase step, re-extract 3～6 times, each time of soaking extraction is 10～60 min;(2) rely on pressure and solvent pump, the liquid phase mixed liquor in temporary tank is pressed into one-level extraction-container through self-cleaning filter; Liquid phase mixed liquor is repeatedly by tubular heat exchanger, and under the pressure of 30～60 DEG C and 0.3～1.0MPa, the solvent evaporates in liquid phase mixed liquor enters solvent recovering system, and liquid extract stays in one-level extraction-container; Between Pressure Drop to the 0.1～0.2MPa in one-level extraction-container, complete one-level and resolve;(3) be delivered to secondary extraction-container through the liquid extract of one-level parsing initial gross separation, spray and diffuse to form tiny liquid pearl through injector at kettle top, under the pressure of 30～60 DEG C and 0.3～1.0MPa, residue in solvent in tiny liquid pearl from top to bottom by the process of jacketed heat exchanger, further evaporated;(4) extract of secondary extraction-container is delivered to extract holding vessel by sanitary pump, obtains pepper alkaloids extract.
- 4. the preparation method of pepper alkaloids in Fructus Piperis extract according to claim 3, is characterized in that, after completing steps (4), pepper alkaloids extract is through CO 2 supercritical purification step.
- 5. the preparation method of pepper alkaloids in Fructus Piperis extract according to claim 4, is characterized in that, described CO 2 supercritical purification step is:(5) opening extraction kettle, to make its inner pressure decreased be 0MPa, opens kettle cover and feed; Material loading completes injection CO in backward still 2, CO 2flow-control is below 30L/h, and regulating extraction temperature in extraction kettle is 20～50 DEG C, and extracting pressure is 5～20MPa, and in separating still, separation temperature is 20～50 DEG C, and separating pressure is 5～20MPa, and extraction time is 30～180min; Collect extract and obtain limpid, transparent, oily liquid pepper alkaloids extract.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104928020A (en) * | 2015-06-12 | 2015-09-23 | 山西鑫中大生物科技有限公司 | Subcritical production method for peony seed oil extraction |
| CN106417300A (en) * | 2016-09-27 | 2017-02-22 | 海南博士威农用化学有限公司 | Insecticide synergia aid |
| CN107803049A (en) * | 2017-11-22 | 2018-03-16 | 中国科学院兰州化学物理研究所 | The method for preparing papper oil and pepper oleoresin using ultrasonic subcritical fluid extraction technology |
| CN113730959A (en) * | 2021-09-30 | 2021-12-03 | 晨光生物科技集团股份有限公司 | Method for removing pesticide residues in pepper oleoresin |
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| CN113730959A (en) * | 2021-09-30 | 2021-12-03 | 晨光生物科技集团股份有限公司 | Method for removing pesticide residues in pepper oleoresin |
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