CN1084176A - The wartwort saponin extracts, separates and prepares the method for agricultural insecticide with it - Google Patents
The wartwort saponin extracts, separates and prepares the method for agricultural insecticide with it Download PDFInfo
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- CN1084176A CN1084176A CN 93102634 CN93102634A CN1084176A CN 1084176 A CN1084176 A CN 1084176A CN 93102634 CN93102634 CN 93102634 CN 93102634 A CN93102634 A CN 93102634A CN 1084176 A CN1084176 A CN 1084176A
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Abstract
The invention provides a kind of saponin that from wartwort, extracts, and with the method for its preparation agricultural insecticide missible oil, leaching process can also obtain byproduct chlorophyll and Quercetin.
The technology that the present invention extracts saponin only with ethanol or a kind of material of methyl alcohol as solvent, by heat of solution repeatedly, cryoprecipitate, filter the saponin that acquisition will be extracted, raw material sources are wide, and technology is simple, the recovery solvent is convenient, substantially do not have the three wastes and produce, the present invention is dissolved in dimethylbenzene with the wartwort saponin and the trichloromethane mixing solutions adds the emulsifying agent preparation agricultural insecticide that is mixed again, and technology is simple, cost is low, do not change natural component, and killing rate can sweep profit and match in excellence or beauty with going out, considerably beyond SD-1750.
Description
The present invention relates to a kind of saponin that from euphorbia plant wartwort (Euphorbia helioscopia L), extracts, and, in the leaching process of saponin, also can obtain chlorophyll crude product and Quercetin crude product with the method for the wartwort saponin preparation agricultural insecticide that extracts.
From the plant that contains saponin, extract the method more complicated of saponin at present, as the method for introducing in " medicinal herb components chemistry " volume, People's Health Publishers 1985 such as () Beijing medical colleges book be: after the plant that will contain saponin is pulverized, earlier with a kind of (water, ethanol or methyl alcohol) or several (earlier with ethanol or methyl alcohol then with butanols or amylalcohol) solvent extractions, again with ether or acetone or heavy metal or cholesterol precipitation; Perhaps with dialysis, chromatography, methods such as magnesium oxide adsorbing are separated, and solvent or carrier that these methods are required are more, and the recovery of production process and solvent, carrier is complexity all, and corresponding input, equipment, labour are more.
Still be not reported as former powder preparation agricultural insecticide missible oil with saponin, can have thought to open up the frontier of an agricultural insecticide.
For chlorophyllous extraction, to introduce according to " foodstuff additive " (foodstuffs industry teaching and research room of Tianjin light industry institute, light industry press, 1985) and other data, chlorophyll is many to be extracted in the silkworm excrement from spinach, and cost is higher.According to document record and two data accumulative totals of field trip, in 13 provinces, cities and autonomous regions of China a large amount of wartwort growths is arranged at least.Show that through planting experimentally continuously of the ecological observations in 5 years and 3 years wartwort can be grown in the weeds clump, be easy to cultivation so aboundresources.
The objective of the invention is provides to the public:
1, makes solvent with ethanol or methyl alcohol for a kind of, from the plant that contains saponin, extract the method for saponin;
2, a kind of method of preparing new agricultural insecticide with the wartwort saponin.
The objective of the invention is to reach by following measure:
1, the method for extraction separation saponin is from wartwort:
A: dry wartwort herb is pulverized, and implantation concentration is the ethanol (or concentration is 95-99% methyl alcohol) of 90-95%, heats then to 55-82 ℃, and wherein contained saponin is fully dissolved, and uses filter paper filtering while hot;
B: will go up step gained filtrate and leave standstill, and treat abundant post precipitation, and refilter at 0-25 ℃; Then
C: with the alcohol washing of the second more than 90% (or first) below 15 ℃ filter thing;
D: after washing, filter to such an extent that thing is used concentration 90% above second (or first) alcohol again, heat of solution in the time of 55-82 ℃, 0-25 ℃ of cryoprecipitate, filter paper filtering, repeated treatments several, get final product pure white technical pure wartwort saponin.
2, the method with wartwort saponin preparation agricultural insecticide is:
A: pure white wartwort saponin is added the three oxygen methane that 4-20 doubly measures (W/V): in 1: 1 mixed solvent of dimethylbenzene, then
B, the dissolving of in water-soluble more than 60 ℃, heating, thus be made into the wartwort saponin solution (the evaporable solvent is ignored in the process of heating) that concentration is 5-25%.
C, adding while hot are equivalent to the mixed matching emulsifying agent of wartwort saponin solution amount 5-60%, and continue to heat in water-bath, make till its fully mutual dissolving.
The present invention extracts saponin from wartwort, resource is very abundant, leaching process is only with ethanol or a kind of solvent thermal dissolving of methyl alcohol, cryoprecipitate, the flushing of second (or first) alcohol, technology is very simple, convenient solvent reclaiming, and also can obtain chlorophyll crude product and two kinds of byproducts of Quercetin crude product, the raw material availability height in the process of extracting, economy, the essentially no three-waste pollution of leaching process.The agricultural insecticide cost of preparing with the wartwort saponin of the present invention's extraction is low, pollution-free substantially, natural components, and killing rate reaches as high as 92-97%.
Further specify the present invention below in conjunction with embodiment.
Fig. 1 is the process flow sheet of extraction separation saponin from wartwort
One, from wartwort, extracts saponin
Referring to Fig. 1, dry wartwort herb is pulverized, cross 10 mesh sieves, adding 8 times of amounts (W/V) concentration is 90-95% ethanol, heat to 55-82 ℃, optimum temps is 60 ± 2 ℃, and keeps 30 minutes, uses filter paper filtering while hot, get the filtrate and the dregs of a decoction, this step 3 times repeatedly, can make full use of starting material; Filtrate was left standstill 12-24 hour under 0-25 ℃ (optimum temps is 10-20 ℃), used filter paper filtering; Filter thing when still containing more ethanol and being scattered paste shape, implantation concentration is 90% above cold ethanol below 15 ℃, keep in the funnel, wait to filter the thing temperature at 5-15 ℃, and be interrupted to stir and wait to filter thing or jiggle funnel, meal in the funnel is scattered in the cold ethanol, till the funnel content is yellowish green; Again the above-mentioned mashed prod that is yellowish green through flushing is poured in the container, added the ethanol of several times amount more than 90%, add temperature jointly, be maintained to most of solids dissolving to 60-82 ℃; Only surplus a little the pale brown look precipitation of container bottom, filtered while hot; Filtrate was left standstill 12-24 hour at 10-20 ℃, used filter paper filtering; Filter to such an extent that thing is used ethanol heat of solution more than 90% again, cryoprecipitate, filter paper filtering, repeated treatments for several times, pure white technical pure wartwort saponin.
Etoh solvent in the above extraction process can change the methyl alcohol that concentration is 95-99% into.
Above-mentionedly from wartwort, extract, separate in the process of saponin, can also produce two kinds of byproducts, after all alcoholic solutions reclaim second (or first) alcohol behind the filtering saponin, get final product the chlorophyll crude product.
With the above-mentioned dregs of a decoction through ethanol-extracted, add the water of 6 times of amounts (W/V), boil; Under agitation slowly add milk of lime to PH8-9; Little with this understanding boiling about 20 minutes; Filter, make during filtration and treat on the filter paper that the filtrate temperature remains on more than 70 ℃; In filtrate, drip concentrated hydrochloric acid, transfer to PH3-5, leave standstill a few hours, see that promptly the Quercetin crude product settles out.
Two, the preparation of agricultural insecticide (missible oil)
Embodiment 1, and the mixed matching emulsifying agent is joined ABS-Ca No. 100 for peaceful breast
C missible oil: 10% wartwort saponin (dimethylbenzene: solution 2.8ml trichloromethane=1: 1)
No. 100, peaceful breast: 60%ABS-Ca alcoholic solution (1: 1.6V/V) 2.08ml
D missible oil: 10% wartwort saponin (dimethylbenzene: solution 1.0ml trichloromethane 1: 1)
No. 100 0.48ml of peaceful breast
The saponin solution of C missible oil and emulsifying agent are packed in the C bottle, the saponin solution of D missible oil and emulsifying agent are packed in the D bottle, in water-bath, heat, make the dissolving fully mutually of saponin solution and emulsifying agent.It is sterilant that the quantity that indicates by subordinate list 1 is made into ultimate missible oil.C in the table
3D
2Expression adds C missible oil 0.3ml, and D missible oil 0.2ml is made into sterilant ... C
9D
1Then expression adds C missible oil 0.9ml; D missible oil 0.1ml is made into sterilant.In water-bath, heat, C, D composition are fully dissolved each other.Ultimate missible oil (being sterilant) is becoming the semi-fluid shape below 25 ℃, face the time spent and heat in water-bath and make it to become liquid state, draws and is made into 1: 2000 emulsion an amount of the adding in 30 ℃ of hot water, carries out insecticidal test with indoor pickling process.
Embodiment 2 mixed matching emulsifying agents are joined ABS-Ca No. 33 with peaceful breast
A missible oil: 5% wartwort saponin (dimethylbenzene: solution 1.0ml trichloromethane 1: 1)
No. 33, peaceful breast: 60%ABS-Ca ethanolic soln (1: 1.6V/V) 0.72ml
B missible oil: 5% wartwort saponin (dimethylbenzene: solution 1.0ml trichloromethane 1.1)
No. 33 0.48ml of peaceful breast
Method by embodiment 1 is mixed with the listed A of table 2
1B
4A
4B
1The ultimate missible oil of various compositions is sterilant, and dilutes 1000 times and make insecticidal test.
Embodiment 3 mixed matching emulsifying agents are joined ABS-Ca No. 601 with peaceful breast
E missible oil: 5% wartwort saponin (dimethylbenzene: solution 1.0ml trichloromethane 1: 1)
No. 601, peaceful breast: 60%ABS-Ca alcoholic solution (1: 1.6) 0.72ml
F missible oil: 5% wartwort saponin (dimethylbenzene: solution 1.0ml trichloromethane 1: 1)
No. 601 0.48ml of peaceful breast
Press the method for embodiment 1, the ultimate missible oil that is mixed with the listed various compositions of table 3 is sterilant, and dilutes 1000 times and do insecticidal test.
Embodiment 4: the mixed matching emulsifying agent is joined the ABS-Ca example No. 700 for peaceful breast
G missible oil: 5% wartwort saponin (dimethylbenzene: solution 1.0ml trichloromethane 1: 1)
No. 700, peaceful breast: 60%ABS-Ca ethanolic soln (1: 1.6) 0.36ml
H missible oil: 5% wartwort saponin (dimethylbenzene: solution 1.0ml trichloromethane 1: 1)
No. 700 0.24ml of peaceful breast
Press the method for embodiment 1, the ultimate missible oil that is mixed with the listed various compositions of table 4 is sterilant, and dilutes 1000 times and do insecticidal test.
Embodiment 5 mixed matching emulsifying agents are EL
-140Join ABS-Ca
I missible oil: 5% wartwort saponin (dimethylbenzene: solution 1.0ml trichloromethane 1: 1)
EL
-140: 60%ABS-Ca ethanolic soln (1: 1.6) 0.36ml
J missible oil: 5% wartwort saponin (dimethylbenzene: solution 1.0ml trichloromethane 1: 1)
EL
-1400.24ml
Press the method for embodiment 1, the ultimate missible oil that is mixed with the listed various compositions of table 5 is sterilant, and dilutes 1000 times and do insecticidal test.
Table 1-table 5 is an embodiment killing rate table look-up.
Illustrate: DDV is 80% DDT EC, and MTHR 20% goes out and sweeps sharp missible oil.When making insecticidal test, the extension rate of the two is identical with the ultimate missible oil that contrasts.
Claims (10)
1, a kind of method of extraction separation wartwort saponin is characterized in that:
A: dry wartwort herb is pulverized, and implantation concentration is the ethanol (or concentration is 95-99% methyl alcohol) of 90-95%, heats then to 55-82 ℃, and wherein contained saponin is fully dissolved, and uses filter paper filtering while hot;
B: will go up step gained filtrate and leave standstill, and treat abundant post precipitation, and refilter at 0-25 ℃; Then
C: with the alcohol washing of the second more than 90% (or first) below 15 ℃ filter thing;
D: after washing, filter to such an extent that thing is used concentration 90% above second (or first) alcohol again, heat of solution in the time of 55-82 ℃, 0-25 ℃ of cryoprecipitate, filter paper filtering, repeated treatments several, get final product pure white technical pure wartwort saponin.
2, extraction according to claim 1, the method for separating the wartwort saponin is characterized in that: the heat of solution temperature the best of heating is 60 ± 2 ℃.
3, extraction according to claim 1 and 2, the method for separating the wartwort saponin, it is characterized in that: filtrate is left standstill, and impelling the wartwort saponin optimum temps that cryoprecipitate is separated out from ethanol (methyl alcohol) is 10-20 ℃.
4, the method for extraction separation wartwort saponin according to claim 1 and 2 is characterized in that: from all alcoholic solutions of filtering wartwort saponin, behind the recovery alcohol, can get the chlorophyll crude product.
5, the method for extraction separation wartwort saponin according to claim 3 is characterized in that: from all alcoholic solutions of filtering wartwort saponin, behind the recovery alcohol, can get the chlorophyll crude product.
6, the method for extraction separation wartwort saponin according to claim 1 and 2 is characterized in that adding limewater extraction in the dregs of a decoction behind second (or first) the ethanol-extracted wartwort saponin, drips concentrated hydrochloric acid then in extracting solution, is settled out the Quercetin crude product.
7, the method for extraction separation wartwort saponin according to claim 3 is characterized in that adding limewater extraction in the dregs of a decoction behind second (or first) the ethanol-extracted wartwort saponin, drips concentrated hydrochloric acid then in extracting solution, is settled out the Quercetin crude product.
8, a kind of wartwort saponin that utilizes claim 1 to obtain is prepared the method for agricultural insecticide, it is characterized in that:
A: pure white wartwort saponin is added the trichloromethane that 4-20 doubly measures (W/V): in the mixed solvent of dimethylbenzene preparation in 1: 1, then
B, the dissolving of in water-soluble more than 60 ℃, heating, thus be made into the wartwort saponin solution that concentration is 5-25%;
C, adding while hot are equivalent to the mixed matching emulsifying agent of wartwort saponin solution amount 5-60%, and continue to heat in water-bath, make till its fully mutual dissolving.
9, the method for preparation agricultural insecticide according to claim 8 is characterized in that: the mixed matching emulsifying agent is that peaceful breast is joined ABS-Ca No. 33; Perhaps peaceful breast is joined ABS-Ca No. 601, and perhaps peaceful breast is joined ABS-Ca No. 700; Perhaps EL
-140Join ABS-Ca; Perhaps peaceful breast is joined ABS-Ca No. 100.
10, the method for preparation agricultural insecticide according to claim 9, it is characterized in that: in the mixed matching emulsifying agent, the collocation scope of ABS-Ca is: 10-55%, promptly do not have pure ABS-Ca weight/(not having pure ABS-Ca weight+nonionic emulsifier capacity) and equal 10-55%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93102634A CN1040614C (en) | 1993-03-08 | 1993-03-08 | Method for extraction and separation glucoside of Euphorbia helioscopia of agricultural insecticide therewith |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93102634A CN1040614C (en) | 1993-03-08 | 1993-03-08 | Method for extraction and separation glucoside of Euphorbia helioscopia of agricultural insecticide therewith |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1084176A true CN1084176A (en) | 1994-03-23 |
| CN1040614C CN1040614C (en) | 1998-11-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN93102634A Expired - Fee Related CN1040614C (en) | 1993-03-08 | 1993-03-08 | Method for extraction and separation glucoside of Euphorbia helioscopia of agricultural insecticide therewith |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1040614C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102342305A (en) * | 2011-08-03 | 2012-02-08 | 甘肃省农业科学院 | Spurge oil emulsion for preventing spider mites of melon and vegetable crops and preparation method thereof |
| CN103081954A (en) * | 2013-02-18 | 2013-05-08 | 青岛农业大学 | Alcoholic solution preparation of wartwort secondary metabolism product and preparation method thereof |
-
1993
- 1993-03-08 CN CN93102634A patent/CN1040614C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102342305A (en) * | 2011-08-03 | 2012-02-08 | 甘肃省农业科学院 | Spurge oil emulsion for preventing spider mites of melon and vegetable crops and preparation method thereof |
| CN102342305B (en) * | 2011-08-03 | 2013-04-10 | 甘肃省农业科学院 | Spurge oil emulsion for preventing spider mites of melon and vegetable crops and preparation method thereof |
| CN103081954A (en) * | 2013-02-18 | 2013-05-08 | 青岛农业大学 | Alcoholic solution preparation of wartwort secondary metabolism product and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN1040614C (en) | 1998-11-11 |
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