CN101449686A - Nux vomica or cortex dictamni botanical acaricide and preparation method thereof - Google Patents

Abstract

The invention relates to a plant acaricide suitable for preventing and controlling harmful mites on economic crops such as fruit trees and vegetables, as well as its preparation method and application. Made by adding surfactants, emulsifiers, penetrants, synergists, etc., it has the characteristics of high efficiency, low toxicity, low residue, and harmony with the environment.

Description

Nuxychnium or white fresh bark botanical acaricide and preparation method thereof

technical field

The invention relates to a pesticide and a preparation method thereof, in particular to an acaricide and a preparation method thereof.

Background technique

Herbivorous mites are important harmful mites in agricultural production. Due to their strong drug resistance, they cause serious losses to agricultural production and are difficult to control. The negative effects of chemical control are well known. At present, the research objects of botanical pesticides are mainly insects, and there are few studies on mites; in the current domestic research of the same type, many botanical insecticide products have come out, but the pesticide products of botanical acaricides have not been reported. less. Therefore, research and development of pollution-free botanical acaricides is imminent.

Contents of the invention

The present invention adopts the method of chemical extraction to extract the active ingredients of Strychnos nux-vomica or the whole plant of Dictamnus dasycarpus which have a lethal effect on mites respectively from the whole plant of Strychnos nux-vomica or Dictamnus dasycarpus, And be prepared into plant source acaricide.

The effective part of the whole plant of Nuxychnium in the present invention can be the whole plant extract or extract of Nuxychnium, and the preparation process of the whole plant of Nuxychnya is selected from one of the following methods:

A. Use a multi-functional extraction tank to make the whole plant of Nuxyche chinensis into powder, and the volume ratio to the organic solvent ethanol is 1:2-8, preferably 1:4, 1:5 or 1:6, soaking in warm or cold After 4-24 hours, filter and dry to obtain the whole plant extract of Nuxyche chinensis;

B adopts a multifunctional extraction tank, the volume ratio of the whole plant powder of the plant Nuxychee chinensis and the organic solvent ethanol is 1:2-8, preferably 1:4, 1:5 or 1:6, and the percolation extraction is repeated 2-10 times, Or continuously reflux extraction for 4-24 hours, filter, and dry to obtain the whole plant extract of Nuxebra chinensis.

Nuxychnium whole plant extract preparation process: after the whole plant extract of Nuxychia chinensis of the present invention is dissolved with methanol, placed in a closed extraction tank, use chloroform or petroleum ether solvent with methanol at a ratio of 0.8:1.5 by volume Liquid-liquid distribution method extraction, with solvent polarity from small to large as the extraction order of the solvent, finally collect the chloroform or petroleum ether extract phase and concentrate under reduced pressure to a relative density of 0.78-1g/cm ³ Ointment, preferably relative density of Nuxychnium 0.9546g/cm ³ , to get the whole plant extract of Nuxychon.

The preparation method of the acaricide: dissolving the whole plant extract or extract of Nuxebra Chin Fructus with chloroform, cyclohexane, benzene, xylene or ethanol solvent, adding the extract or extract to dissolve or extract in the following order and proportion Suspended solubilizers, emulsifiers and/or suspending agents, synergists, and penetrating agents are made into acaricides.

Nuxychnium whole plant extract acaricide:

Extract 5-36 parts by weight

Solvent 30-95 parts by weight

Solubilizer 1-40 parts by weight

Emulsifier or suspending agent 2-350 parts by weight

Synergist 0.5-30 parts by weight

Penetrant 0.5-28 parts by weight.

Nuxychnium whole plant extract acaricide:

Extract 3-30 parts by weight

Solvent 30-95 parts by weight

Solubilizer 1-30 parts by weight

Emulsifier or suspending agent 2-32 parts by weight

Penetrant 0.5-28 parts by weight

Synergist 0.5-25 parts by weight.

In addition to ethanol, the organic solvent used in the preparation method of the whole plant extract of Strychnis nuxicae can also be selected from non-limiting: chloroform, 30-90°C petroleum ether, ether, ethyl acetate, n-hexane, cyclohexane, One of benzene, methanol, acetone, cyclohexanone, etc.

In the preparation method of the whole plant extract of Nuxebra chinensis, the organic solvent used can be non-limitingly selected from: chloroform, 30-90°C petroleum ether, ether, ethyl acetate, n-hexane, cyclohexane in addition to ethanol , benzene, methanol, acetone, cyclohexanone, etc.

In the preparation method of the acaricide, the solvent is selected from one of water, ethanol, methanol, acetone, cyclohexanone, toluene, xylene, petroleum ether, petroleum aromatics, and pure benzene; the solubilizing agent is dodecylbenzenesulfonate Any one of sodium dodecylbenzenesulfonate, potassium dodecylbenzenesulfonate, polysorbate, polyethylene glycol, sorbitol polyoxyethyl ether, lignosulfonate, tea dead, and saponin; the synergist is tea Any one of saponin, 2-C1C6H4-N=OCH3SCH3, methylenedioxybenzene derivatives, 6-vinyldecyl aldehyde, octachlorodipropyl ether; emulsifier is C15-17H31-37COONa, stearic acid Sodium, sodium lauryl sulfate, N-dodecyldimethylamine, polyoxyethylene ether, polyoxypropylene ether, p-octylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene Any one of base esters and alkylaryl sulfonates; the penetrating agent is any one of benzylphenol polyoxyethylene ether, azone, and triphenylphosphine.

Nuxychnium extract acaricide is preferably:

Extract 18 parts by weight

Toluene 70 parts by weight

Polysorbate 5 parts by weight

Tea saponin 4 parts by weight

Sodium lauryl sulfate 5 parts by weight

Azone 3 parts by weight.

The nuxy seed extract acaricide is preferably:

Extract 14 parts by weight

Xylene 65 parts by weight

Sorbitol polyoxyethyl ether 3.5 parts by weight

Polyoxyethylene ether 4 parts by weight

6-Vinyl decanal 2.5 parts by weight

Benzylphenol polyoxyethylene ether 2.5 parts by weight.

The application of the present invention also discloses an effective part of Dictatoria radiata and its acaricide, which are prepared by the same technical scheme as that of the above-mentioned Nuxychia, wherein the preparation process of the whole plant extract of Dictatoria Finally, the chloroform or petroleum ether extract phase was collected and concentrated under reduced pressure to an ointment with a relative density of 0.8-1 g/cm ³ , preferably a relative density of 0.9128 g/cm ³ , to obtain the whole plant extract of Cortex radix.

The invention provides a novel biopesticide with high efficiency, low toxicity, low residue, and harmony with the environment and other organisms, which has far-reaching significance for environmental protection and for solving the drug resistance of harmful mites. Compared with chemically prepared pesticides, the present invention has the following characteristics and advantages:

(1) Since the whole plant of Strychnos chinensis or the whole plant of B. chinensis is a plant in nature, its extract is easy to decompose under natural conditions, safe for the environment and the surrounding ecosystem, and has no environmental pollution problem; Or the whole plant acaricide of Nymphaeum chinensis is a multi-component mixture, which has multiple action sites on mites, so it is not easy to produce drug resistance; The agent has significant acaricidal effect, and has the characteristics of high efficiency of chemical pesticides; (4) the extraction of effective parts in the whole plant of Nuxychnium or D. chinensis is simple and easy, and is very conducive to industrial production.

The following experimental examples or examples are used to further illustrate but not limit the present invention.

Experimental example 1 Pharmacodynamic research test

The whole plant extract or extract of Semen Nuxicae or Radix Dictatus obtained by the present invention, with reference to the standard method recommended by FAO-slide method, Semen Nuxtrix or Radix Dictica is carried out biological activity assay to harmful mites; Cut the masking tape into 2-3cm long, stick it on one end of the glass slide, use tweezers to peel off the paper on the tape, use a zero brush to select female adult mites with the same size, bright body color, and active actions, and stick them on the back. On the double-sided adhesive tape, stick 3 rows per piece, and stick 10 heads per row; place it in a biochemical incubator at (25±1)°C and RH85% for 4 hours, observe with binoculars, and remove dead or inactive ones. Individual; on the basis of the pre-test, dilute the medicine to 3-5 concentrations, immerse the end of the glass slide with mites in the medicine solution, shake gently for 5 seconds, take it out, and quickly absorb the excess medicine solution around the mite body and its surroundings with absorbent paper Place it in a biochemical incubator, and check the results with binoculars after 24 hours; lightly touch the mite body with a brush, and those who do not move their feet are considered dead; each concentration is repeated 3 times, and the results are shown in the following table 1-2.

Table 1 The acaricidal effect of two plant extracts on Tetranychus cinnabarinus (Teranychus cinnabarinus)

Table 2 The poisonous effect of two plant extracts on Tetranychus cinnabarinus (Teranychus cinnabarinus)

The results showed that: the extracts of the two plants or the extracts of Tetranychus cinnabarinus had an average killing rate and poisoning rate of more than 80%. With the reduction of the extracts or extract concentrations of the two plants, the acaricidal effect and poisonous effect are reduced, but the mortality rate of the mites is still about 45%. It can be seen that the whole plant extract or the extract of the Nuxychnium or Radix Cortex of the present invention has remarkable acaricidal effect.

For the ovicidal effect, refer to the Leaf-residue method recommended by FAO and improve it. Collect fresh ground bean leaves, cut off the petiole by 0.5cm, wrap wet cotton balls on the petiole, and place it on a water culture platform. Pick up 50 female adult mites on each leaf, place them at (25±1)°C and allow them to lay eggs for 24 hours, remove the female adult mites, check and record the number of eggs, and place them in a constant temperature incubator at (25±1)°C. When the age of the eggs reaches 36-48h, the measurement is carried out. The leaves with eggs are immersed in each treatment solution for 5 seconds, then placed on absorbent paper to dry in the shade, and then put back on the water culture platform. After the eggs of the control group hatch and develop to the nymph stage, The mortality rate of each treatment was checked and counted. See Table 3 for the ovicidal effects of the whole plant extracts of Nuxyche, D. chinensis and Amorpha fruticosa.

Table 3 The effect of two plant extracts on the eggs of spider mite (Teranychus cinnabarinus)

The results show that the poisonous killing rate of the two plant extracts to the eggs of Tetranychus cinnabarinus can reach 65%, and the poisonous killing rate of the extract of Nuxychia cinnabarinus on the eggs of Tetranychus cinnabarinus can reach more than 70%, which proves that the two plant extracts The poisonous effect on mite eggs is remarkable.

Antifeedant Activity Test After the leaves of Glycyrrhiza sativa were washed and blotted dry, the sample to be tested was applied on the back side along the midrib of the leaf (about 0.01ml/cm ² ), and distilled water was used as a control on the other side. 30 spider mites were attached to the back of the leaf, and then covered with a glass ring with a diameter of 5 cm, so that the treated area on both sides of the leaf midrib was equal to the control area. After 24 hours, the number of spider mites inhabiting on both sides of the leaf midrib was checked, and the spider mites inhabiting on the leaf midrib and glass circle wall were not counted. 30 test insects were treated each time, repeated three times;

Feed resistance rate (%)=[(number of spider mites in control area-number of spider mites in treatment area)/total number]×100%, the results are shown in Table 4.

Table 4 Antifeedant activity of two plant extracts against spider mite (Teranychus cinnabarinus)

The result shows: two kinds of plant extracts have obvious antifeedant activity effect to Tetranychus cinnabarinus, the antifeedant rate to nymph is slightly stronger than the antifeedant rate to adult mites, all can reach about 70%, prove that two kinds of plant extracts of the present invention have antifeedant effect Both nymphs and adults had strong antifeedant activity.

Experimental Example 2 Compared with the disclosed extraction process, the effective fractions extracted by this process have better ovicidal and antifeedant activities, and the results are shown in Table 5.

Table 5 Comparison of different extraction processes on the active substances of Tetranychus cinnabarinus from two plants

Note: A: the effect of the effective part proposed by this process, B: the effect of the effective part proposed by the disclosed process

The results show that: compared with the disclosed existing technology, the extracts or extracts of the two plants prepared by the extraction process of the present invention have significant effects on the poisoning and antifeedant effects of Tetranychus cinnabarinus, and the extraction of the present invention is effective. The ovum killing rate of the parts can reach about 70%, while the acaricidal rate of the effective parts extracted by the disclosed process is only about 35%; the antifeedant rate of the effective parts extracted by the process of the present invention can reach twice the antifeedant rate of the effective parts extracted by the disclosed process , which proves that the effective part prepared by the extraction process of the present invention has a significant rate of killing acarids and resisting food.

The following embodiments can all achieve the effects of the above experimental examples.

Detailed ways

Example 1:

Wash the whole plant of St. Chinensis, dry in the shade in a ventilated place, and pass through a 40-60 mesh sieve after grinding; put the crushed plant powder into a multifunctional extraction tank, and extract with petroleum ether with 5 times the volume of the plant powder. Collect the petroleum ether extract phase, concentrate under reduced pressure to obtain the extract; take 18 kg of the extract and add 70 kg of toluene, add it to a mixing kettle with a stirrer and a thermometer, mix for 1.5 hours at 50 ° C, add Tween (polysorbate) 5kg, 6-vinyl decanal 4kg, sodium lauryl sulfate 5kg, benzylphenol polyoxyethylene ether 3kg, mix homogeneously, obtain the whole plant extract of Nuxychia chinensis acaricide emulsifiable concentrate. Example 2:

As in the method of Example 1, the fresh bark extract acaricide emulsifiable concentrate was prepared.

Example 3:

Wash the whole plant of St. Chinensis, dry it at 45°C, grind it and pass it through a 60-mesh sieve; put the crushed plant powder into a multifunctional extraction tank, extract with 4 times the volume of chloroform, and collect the chloroform for extraction. phase, concentrated under reduced pressure to obtain the extract; take 14kg of the extract, add 65kg of xylene, add it to a mixing kettle with a stirrer and a thermometer, mix for 3 hours at 60°C, add 3.5kg of polyethylene glycol, tea saponin 4kg, p-octylphenol polyoxyethylene ether 2.5kg, azone 2.5kg, mix homogeneously, obtain the whole plant extract of Nuxychia chinensis acaricide emulsifiable concentrate.

Example 4:

As in the method of Example 3, the fresh bark extract acaricide emulsifiable concentrate was prepared.

Example 5:

Wash the whole plant of Nuxyche chinensis, dry it at 40°C, grind it and pass it through a 60-mesh sieve; put the crushed plant powder into a multifunctional extraction tank, extract with 6 times the volume of chloroform, and collect the chloroform for extraction phase, concentrated under reduced pressure to obtain the extract; take 15kg of the extract, add 70kg of xylene, add it to a mixing kettle with a stirrer and a thermometer, mix for 2 hours at 60°C, add 8kg of sodium dodecylbenzenesulfonate, 4kg of 6-vinyldecyl aldehyde, 5kg of p-octylphenol polyoxyethylene ether, and 3kg of azone were mixed uniformly to obtain the acaricide emulsifiable concentrate of the whole plant extract of Nuxychia chinensis.

Embodiment 6:

As in the method of Example 5, the acaricide emulsifiable concentrate of the fresh bark extract was prepared.

Embodiment 7:

Using a multi-functional extraction tank, use the volume ratio of the whole plant of Nuxychonzi and the organic solvent ethanol as 1:4, cold soak for 10 hours, filter, and dry to obtain the whole plant extract of Nuxychonzi; After the methanol is dissolved, it is placed in a closed extraction tank, and the petroleum ether solvent is extracted with methanol at a volume ratio of 0.7:1.5 by liquid-liquid distribution method. The ether extraction phase was concentrated under reduced pressure to an ointment, with a relative density of 0.9546g/cm ³ , to obtain the whole plant extract of Nuxychium chinensis; after taking 10kg of the whole plant extract of Nuxychium chinensis and dissolving it with 60kg of petroleum ether, inject it with a stirring In a mixing kettle with a thermostat and a thermometer, mix for 2 hours at 30°C, add 4kg of polysorbate, 3kg of sodium stearate, 2kg of tea saponin and 3kg of azone in the following order and proportion to make whole nux. Strain extract acaricide emulsifiable concentrate.

Embodiment 8:

Using a multi-functional extraction tank, use the volume ratio of the whole plant of Dinosauria to the organic solvent ethanol as 1:4, soak in cold for 10 hours, filter, and dry to obtain the whole plant extract of Dinosauria; After methanol is dissolved, it is placed in a closed extraction tank, and petroleum ether solvent is used to extract methanol at a volume ratio of 0.7:1.5 by liquid-liquid distribution method. The extraction order of the solvent is from small to large solvent polarity, and finally oil The ether extraction phase was concentrated under reduced pressure to an ointment, with a relative density of 0.9128g/cm ³ , to obtain the whole plant extract of D. chinensis; after dissolving 10kg of the whole plant extract of D. chinensis with 60kg of petroleum ether, inject it with a stirring In a mixing kettle with a thermometer and a thermometer, mix for 2 hours at 30°C, add 4kg of polysorbate, 3kg of sodium stearate, 2kg of tea saponin and 3kg of azone in the following order and proportion to make whole white fresh skin Strain extract acaricide emulsifiable concentrate.

Embodiment 9:

The preparation of the whole plant extract of Nuxychia chinensis

Using a multi-functional extraction tank, the whole plant of Nuxychnium chinensis is made into powder, and the volume ratio to the organic solvent ethanol is 1:4, soaked in temperature for 10 hours, filtered, and dried to obtain the whole plant of Nuxychon chinensis extract.

Example 10:

Preparation of the whole plant extract of Cortex alba

The whole plant extract of Cortex radix L. was prepared as in Example 9.

Example 11:

The preparation of the whole plant extract of Nuxychia chinensis

Using a multi-functional extraction tank, use the volume ratio of the whole plant powder of Nuxychnium chinensis to the organic solvent n-hexane as 1:4, perform repeated percolation extraction for 8 times, filter, and dry to obtain the whole plant extract of Nuxychia chinensis.

Example 12:

Preparation of the whole plant extract of Cortex alba

The whole plant extract of Cortex radix was prepared as in Example 11.

Example 13:

The preparation of the whole plant extract of Nuxychia chinensis

After dissolving the whole plant extract of Nuxebra chinensis obtained in Examples 9 and 11 with methanol, place it in a closed extraction tank, use chloroform solvent to extract with methanol in a ratio of 0.7:1.5 by volume and by liquid-liquid distribution method, and use solvent The order of solvent extraction is from small to large polarity, and finally the chloroform extract phase is collected and concentrated under reduced pressure to an ointment with a relative density of 0.9546g/cm ³ , to obtain the whole plant extract of Nuxychia chinensis.

Example 14:

Preparation of the whole plant extract of Cortex radix

Dissolve the extracts of the whole plant of Cortex radix obtained in Examples 10 and 12 with methanol, place them in a closed extraction tank, and use chloroform solvent to extract with methanol at a volume ratio of 0.7:1.5 by liquid-liquid distribution method. The order of solvent extraction is from small to large polarity, and finally the chloroform extract phase is collected and concentrated under reduced pressure to an ointment with a relative density of 0.9128g/cm ³ to obtain the whole plant extract of D.

Example 15:

The preparation of the whole plant extract of Nuxychia chinensis

Using a multifunctional extraction tank, the volume ratio of the whole plant powder of Nuxychia Chin to the organic solvent ethyl acetate is 1:6, and the extraction is continuously refluxed for 20 hours, filtered, and dried to obtain the whole plant extract of Nuxychia Chin.

Embodiment 16: Preparation of the whole plant extract of Radix Cortex Radix

As in the method of Example 15, the whole plant extract of Cortex radix L. was prepared.

Example 17: Preparation of Nuxychnium whole plant extract

After dissolving the whole plant extract of Nuxebra chinensis obtained in Example 15 with methanol, place it in a closed extraction tank, use chloroform solvent to extract with methanol in a volume ratio of 0.7:1.5 by liquid-liquid distribution method, and use a solvent pole The order of solvent extraction is from small to large, and finally the petroleum ether extract phase is collected and concentrated under reduced pressure to an ointment, with a relative density of 0.9546g/cm ³ , to obtain the whole plant extract of Nuxychnium.

Example 18: Preparation of the whole plant extract of Cortex radix

Dissolve the whole plant extract of Cortex ditsiformis obtained in Example 16 with methanol, place it in a closed extraction tank, and use chloroform solvent to extract with methanol at a volume ratio of 0.7:1.5 by liquid-liquid partitioning method. The order of solvent extraction is from small to large, and finally the petroleum ether extract phase is collected and concentrated under reduced pressure to an ointment, with a relative density of 0.9128g/cm ³ of Cortex radix, and the whole plant extract of Cortex punctatus is obtained.

Example 19: Preparation of Nuxychnium Extract

Using a multi-functional extraction tank, use the volume ratio of the whole plant powder of Nuxychnium chinensis and the organic solvent ether as 1:5, cold soak for 10 hours, filter, and dry to obtain the whole plant of Nuxychia chinensis extract.

Embodiment 20: the preparation of white fresh bark extract

As in the method of Example 19, the whole plant extract of Cortex radix L. was prepared.

Example 21: Preparation of Nuxychnium whole plant extract

Using a multi-functional extraction tank, use the volume ratio of the whole plant powder of Nuxychia Chin to the organic solvent methanol as 1:6, soak in warm for 20 hours, filter, and dry to obtain the extract of the whole plant of Nuxychia Chin.

Example 22: Preparation of Cortex Dictica Extract

As in the method of Example 21, the whole plant extract of Cortex radix L. was prepared.

Example 23: Preparation of Nuxychnium whole plant extract

Using a multi-functional extraction tank, use the volume ratio of the whole plant powder of Nuxychia Chin to the organic solvent ethyl acetate at a volume ratio of 1:6, soak in temperature for 10 hours, filter, and dry to obtain the extract of the whole plant of Nuxychia Chin.

Example 24: Preparation of Cortex Dictica Extract

As in the method of Example 23, the whole plant extract of Cortex radix L. was prepared.

Preparation of whole plant extract

Example 25: Preparation of Nuxychnium whole plant extract

Using a multifunctional extraction tank, use the volume ratio of the whole plant powder of Nuxychnium chinensis to the organic solvent benzene as 1:4, perform repeated percolation extraction for 5 times, filter, and dry to obtain the whole plant of Nuxychnium chinensis extract.

Embodiment 26: the preparation of the extract of Radix Cortex

As in the method of Example 25, the whole plant extract of Cortex radix L. was prepared.

Example 27: Preparation of Nuxychnium whole plant extract

Using a multi-functional extraction tank, use the volume ratio of the whole plant powder of Nuxychia Chin to the organic solvent acetone at a volume ratio of 1:5, continuously reflux extraction for 10 hours, filter, and dry to obtain the extract of the whole plant of Nuxychia Chin.

Example 28: Preparation of Radix Cortex Extract

As in the method of Example 27, the whole plant extract of Cortex radix L. was prepared.

Example 29: Preparation of Nuxychnium whole plant extract

Using a multi-functional extraction tank, use the volume ratio of the whole plant powder of Nuxychia Chin to the organic solvent n-hexane at a volume ratio of 1:6, perform repeated percolation extraction for 3 times, filter, and dry to obtain the whole plant extract of Nuxychia Chin.

Example 30: Preparation of Radix Cortex Cortex Extract

As in the method of Example 29, the whole plant extract of Cortex radix L. was prepared.

Example 31: Preparation of Nuxychnium whole plant extract

Using a multi-functional extraction tank, use the volume ratio of the whole plant powder of Nuxychia Chin to the organic solvent ethyl acetate at a volume ratio of 1:5, continuously reflux extraction for 18 hours, filter, and dry to obtain the whole plant extract of Nuxychia Chin.

Example 32: Preparation of Radix Cortex Cortex Extract

According to the method of Example 31, the whole plant extract of Cortex radix L. was prepared.

Example 33: Preparation of Nuxychnium whole plant extract

Dissolve the extract of the whole plant of St. Chinensis obtained in Example 19 with 30-90°C petroleum ether, put it in a closed extraction tank, and use petroleum ether solvent with a volume ratio of 0.7:1.5 to 30-90°C petroleum ether. Extraction by liquid-liquid partitioning Finally, the petroleum ether extract phase was collected and concentrated under reduced pressure to an oily paste with a relative density of 0.9546 g/cm ³ , to obtain the whole plant extract of Nuxica chinensis.

Example 34: Preparation of Cortex Vertex Extract

Dissolve the whole plant extract of Cortex radix obtained in Example 20 with petroleum ether at 30-90°C, put it in a closed extraction tank, and use petroleum ether solvent at a volume ratio of 0.7:1.5 to petroleum ether at 30-90°C Extraction by liquid-liquid distribution method Finally, the petroleum ether extract phase was collected and concentrated under reduced pressure to an ointment with a relative density of 0.9128g/cm ³ , to obtain the whole plant extract of Cortex alba.

Example 35: Preparation of Nuxychnium whole plant extract

After dissolving the extract of the whole plant of St. Chinensis obtained in Example 21 with ethanol, place it in a closed extraction tank, use chloroform solvent to extract with ethanol in a volume ratio of 0.7:1.5 by liquid-liquid distribution method, and use solvent polarity The order of extraction is from small to large solvents, and finally the chloroform extract phase is collected and concentrated under reduced pressure to an ointment with a relative density of 0.9546g/cm ³ , to obtain the whole plant extract of Nuxica chinensis.

Example 36: Preparation of the whole plant extract of Cortex radix

Dissolve the whole plant extract of Cortex radix obtained in Example 22 with ethanol, place it in a closed extraction tank, and use chloroform solvent to extract with ethanol at a ratio of 0.7:1.5 by volume ratio by liquid-liquid distribution method. The order of extraction is from small to large solvents, and finally the chloroform extract phase is collected and concentrated under reduced pressure to an ointment with a relative density of 0.9128g/cm ³ , to obtain the whole plant extract of Cortex alba.

Example 37: Preparation of Nuxychnium whole plant extract

Dissolve the whole plant extract of Nuxebra chinensis obtained in Example 23 with ethyl acetate, put it in a closed extraction tank, and use petroleum ether solvent to extract with ethyl acetate at a volume ratio of 0.7:1.5 by liquid-liquid distribution method Finally, the petroleum ether extract phase was collected and concentrated under reduced pressure to an ointment with a relative density of 0.9546 g/cm ³ to obtain the whole plant extract of Nuxychia chinensis.

Example 38: Preparation of the whole plant extract of Cortex radix

Dissolve the whole plant extract of Cortex radix obtained in Example 24 with ethyl acetate, put it in a closed extraction tank, and use petroleum ether solvent to extract with ethyl acetate at a volume ratio of 0.7:1.5 by liquid-liquid distribution method Finally, the petroleum ether extract was collected and concentrated under reduced pressure to an ointment with a relative density of 0.9128g/cm ³ , to obtain the whole plant extract of Cortex alba.

Example 39: Preparation of Nuxychnium whole plant extract

Dissolve the whole plant extract of Nuxebra chinensis obtained in Example 25 with methanol, put it in a closed extraction tank, use chloroform solvent to extract with methanol at a volume ratio of 0.7:1.5 by liquid-liquid distribution method, and finally collect the chloroform extraction phase and concentrated under reduced pressure to an ointment, with a relative density of 0.9546g/cm ³ , to obtain the whole plant extract of Strychnis chinensis.

Example 40: Preparation of the whole plant extract of Cortex radix

Dissolve the whole plant extract of Cortex radix obtained in Example 26 with methanol, put it in a closed extraction tank, use chloroform solvent to extract with methanol at a volume ratio of 0.7:1.5 by liquid-liquid distribution method, and finally collect chloroform for extraction phase and concentrated under reduced pressure to an ointment, with a relative density of 0.9128g/cm ³ , to obtain the whole plant extract of Cortex alba.

Example 41: Preparation of Nuxychnium Extract Acaricide

The whole plant extract of Fructus Nuxychia of embodiment 9, 11, 15 or 19 prepares acaricide according to the following ratio

Extract 18kg

Toluene 70kg

Polysorbate 5kg

Tea saponin 4kg

Sodium Lauryl Sulfate 5kg

Azone 3kg.

Example 42: Preparation of acaricide from Cortex radix L.

The whole plant extract of Radix Cortex Cortex of embodiment 10, 12, 16 or 20 prepares acaricide according to the following ratio

Extract 18kg

Toluene 70kg

Polysorbate 5kg

Tea saponin 4kg

Sodium Lauryl Sulfate 5kg

Azone 3kg.

Example 43: Preparation of Nuxychnium Extract Acaricide

Embodiment 21, 23, 25, 27, 29 or 31 The whole plant extract of Nuxebra chinensis is prepared in the following proportions as acaricide

Extract 30kg

Acetone 70kg

Polyethylene glycol 15kg

6-Vinyldecanal 14kg

p-Octylphenol polyoxyethylene ether 18kg

Benzylphenol polyoxyethylene ether 12kg.

Example 44: Preparation of acaricide from Cortex radix L.

Example 22, 24, 26, 28, 30 or 32 Radix Cortex whole plant extract prepares acaricide according to the following ratio

Extract 30kg

Acetone 70kg

Polyethylene glycol 15kg

6-Vinyldecanal 14kg

p-Octylphenol polyoxyethylene ether 18kg

Benzylphenol polyoxyethylene ether 12kg.

Example 45: Preparation of Nuxychnium Extract Acaricide

Embodiment 13, 17 or 33 Nuxychnium whole plant extract prepares acaricide according to the following ratio

Extract 14kg

Xylene 65kg

Sorbitol polyoxyethyl ether 3.5kg

Polyoxyethylene ether 4kg

6-Vinyldecanal 2.5kg

Benzylphenol polyoxyethylene ether 2.5kg.

Example 46: Preparation of acaricide from the fresh bark extract

Embodiment 14, 18 or 34 Radix Cortex whole plant extract prepares acaricide according to the following ratio

Extract 14kg

Xylene 65kg

Sorbitol polyoxyethyl ether 3.5kg

Polyoxyethylene ether 4kg

6-Vinyldecanal 2.5kg

Benzylphenol polyoxyethylene ether 2.5kg.

Example 47: Preparation of Nuxychnium Extract Acaricide

Embodiment 35, 37 or 39 The whole plant extract of Semen Nuxychia is prepared as acaricide according to the following ratio

Extract 25kg

Petroleum ether 60kg

Potassium dodecylbenzenesulfonate 10kg

Octachlorodipropyl ether 7kg

Polyoxypropylene ether 8kg

Azone 5kg.

Example 48: Preparation of Acaricide from Cortex Dictica Extract

Embodiment 36, 38 or 40 The whole plant extract of Cortex radix is prepared in the following proportions as acaricide

Extract 25kg

Petroleum ether 60kg

Potassium dodecylbenzenesulfonate 10kg

Octachlorodipropyl ether 7kg

Polyoxypropylene ether 8kg

Azone 5kg.

Claims (24)

1, plant vomiting nut active component is characterized in that this active component is to be made by one of following method:

A adopts multi-function extractor, and the volume ratio of plant vomiting nut complete stool powder and organic solvent ethanol is 1:2-8, and temperature is soaked or cold soaking 4-24 hour, filters, and drying gets the vomiting nut whole strain extract;

B adopts multi-function extractor, and the volume ratio of plant vomiting nut complete stool powder and organic solvent ethanol is 1:2-8, and diacolation extracts 2-10 time repeatedly, or continuous backflow extracted 4-24 hour, filters, and drying must the vomiting nut whole strain extract.

2, vomiting nut active component as claimed in claim 1 is characterized in that making that the volume ratio of vomiting nut powder and ethanol is 1:4,1:5 or 1:6 in the vomiting nut active component method.

3, vomiting nut active component as claimed in claim 1 or 2 is characterized in that this vomiting nut active component is to be made by following method:

With the vomiting nut whole strain extract with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with chloroform or benzinum solvent with ratio and the methyl alcohol of volume ratio 0.8:1.5, with solvent polarity is the extraction order of solvent from small to large, and finally collecting chloroform or petroleum ether extraction phase and being evaporated to relative density is 0.78-1g/cm ³The vomiting nut complete stool extract of ointment shape.

4, vomiting nut active component as claimed in claim 1 or 2 is made acaricidal preparation method, it is characterized in that this method is: vomiting nut whole strain extract or extract are dissolved with chloroform, cyclohexane, benzene, dimethylbenzene or alcohol solvent, add solubilizer, emulsifier and/or the suspending agent, synergist, the bleeding agent that promote extract or extract to dissolve or suspend therein with ratio in the following order and make miticide;

Extract 5-36 weight portion

Solvent 30-95 weight portion

Solubilizer 1-40 weight portion

Emulsifier or suspending agent 2-350 weight portion

Synergist 0.5-30 weight portion

Bleeding agent 0.5-28 weight portion;

Among the acaricidal preparation method, solvent is selected from a kind of in water, ethanol, methyl alcohol, acetone, cyclohexanone, toluene, dimethylbenzene, benzinum, petroleum aromatic, the purified petroleum benzin; Solubilizer be neopelex, Potassium dodecylbenzenesulfonate, polysorbate, polyethylene glycol, sorbierite polyoxy ether, lignosulfonates, tea withered, take any in the Chinese honey locust; Synergist is any in Tea Saponin, 2-C1C6H4-N=OCH3SCH3, methylenedioxy benzene derivative, 6-vinyl capraldehyde, the Octachlorodipropyl Ether; Emulsifier is any in C15-17H31-37COONa, odium stearate, lauryl sodium sulfate, N-domiphen, APEO, polyethenoxy ether, paraoctyl phenol APEO, aliphatic alcohol polyethenoxy base ether, aliphatic acid polyethenoxy base ester, the alkylaryl sulfonates; Bleeding agent is any in emulsifier BP, azone, the triphen phosphorus.

5, make acaricidal preparation method as vomiting nut active component as described in the claim 3, it is characterized in that this method is: the full pearl extract of vomiting nut with chloroform, cyclohexane, benzene, dimethylbenzene or the dissolving of ethanol equal solvent, is added solubilizer, emulsifier and/or suspending agent, synergist with ratio, the bleeding agent auxiliary material is made the extract miticide in the following order therein;

Extract 3-30 weight portion

Solvent 30-95 weight portion

Solubilizer 1-30 weight portion

Emulsifier or suspending agent 2-32 weight portion

Bleeding agent 0.5-28 weight portion

Synergist 0.5-25 weight portion;

Among the acaricidal preparation method, solvent is selected from a kind of in water, ethanol, methyl alcohol, acetone, cyclohexanone, toluene, dimethylbenzene, benzinum, petroleum aromatic, the purified petroleum benzin; Solubilizer be neopelex, Potassium dodecylbenzenesulfonate, polysorbate, polyethylene glycol, sorbierite polyoxy ether, lignosulfonates, tea withered, take any in the Chinese honey locust; Synergist is any in Tea Saponin, 2-C1C6H4-N=OCH3SCH3, methylenedioxy benzene derivative, 6-vinyl capraldehyde, the Octachlorodipropyl Ether; Emulsifier is any in C15-17H31-37COONa, odium stearate, lauryl sodium sulfate, N-domiphen, APEO, polyethenoxy ether, paraoctyl phenol APEO, aliphatic alcohol polyethenoxy base ether, aliphatic acid polyethenoxy base ester, the alkylaryl sulfonates; Bleeding agent is any in emulsifier BP, azone, the triphen phosphorus.

6, vomiting nut active component as claimed in claim 1 or 2 is characterized in that wherein said organic solvent ethanol is by a kind of replacement in chloroform, 30-90 ℃ benzinum, ether, n-hexane, cyclohexane, benzene, ethyl acetate, methyl alcohol, acetone or the cyclohexanone.

7, as vomiting nut active component as described in the claim 3, it is characterized in that wherein said organic solvent methyl alcohol is by a kind of replacement in chloroform, 30-90 ℃ benzinum, ether, n-hexane, cyclohexane, benzene, ethyl acetate, acetone or the cyclohexanone.

8, a kind of preparation method of vomiting nut active component is characterized in that this method is one of following method:

A adopts multi-function extractor, and the volume ratio of plant vomiting nut complete stool powder and organic solvent ethanol is 1:2-8, and temperature is soaked or cold soaking 4-24 hour, filters, and drying gets the vomiting nut whole strain extract;

B adopts multi-function extractor, and the volume ratio of plant vomiting nut complete stool powder and organic solvent ethanol is 1:2-8, and diacolation extracts 2-10 time repeatedly, or continuous backflow extracted 4-24 hour, filters, and drying must the vomiting nut whole strain extract.

9,, it is characterized in that the volume ratio of vomiting nut powder and ethanol is 1:4,1:5 or 1:6 in this method as the preparation method of vomiting nut active component as described in the claim 8.

10, as the preparation method of vomiting nut active component as described in claim 8 or 9, it is characterized in that this preparation method is: with the vomiting nut whole strain extract with dissolve with methanol after, place airtight extractor, adopt liquid-liquid apportion design extraction with chloroform or benzinum solvent with ratio and the methyl alcohol of volume ratio 0.8:1.5, with solvent polarity is the extraction order of solvent from small to large, and finally collecting chloroform or petroleum ether extraction phase and being evaporated to relative density is 0.78-1g/cm ³The vomiting nut complete stool extract of ointment shape.

11, as the preparation method of vomiting nut active component as described in claim 8 or 9, it is characterized in that wherein said organic solvent except that ethanol by a kind of replacement in chloroform, 30-90 ℃ benzinum, ether, ethyl acetate, n-hexane, cyclohexane, benzene, methyl alcohol, acetone or the cyclohexanone.

12, as the preparation method of vomiting nut active component as described in the claim 10, it is characterized in that wherein said organic solvent except that ethanol by a kind of replacement in chloroform, 30-90 ℃ benzinum, ether, ethyl acetate, n-hexane, cyclohexane, benzene, methyl alcohol, acetone or the cyclohexanone.

13, the application of vomiting nut active component as claimed in claim 1 or 2 in the preparation miticide.

14, the application of vomiting nut active component as claimed in claim 3 in the preparation miticide.

15, the application of the full pearl of vomiting nut in the preparation miticide farm chemical.

16, the active component of vomiting nut as claimed in claim 1 or 2 is characterized in that wherein the raw material vomiting nut is replaced by the root bark of shaggy-fruited dittany.

17, the active component of vomiting nut as claimed in claim 3 is characterized in that wherein the raw material vomiting nut is replaced by the root bark of shaggy-fruited dittany, and finally collecting chloroform or petroleum ether extraction phase and being evaporated to relative density is 0.8-1g/cm ³The root bark of shaggy-fruited dittany complete stool extract of ointment shape.

18, vomiting nut active component as claimed in claim 4 is made acaricidal preparation method, it is characterized in that wherein the raw material vomiting nut is replaced by the root bark of shaggy-fruited dittany.

19, vomiting nut active component as claimed in claim 5 is made acaricidal preparation method, it is characterized in that wherein the raw material vomiting nut is replaced by the root bark of shaggy-fruited dittany.

20, the preparation method of vomiting nut active component as claimed in claim 8 or 9 is characterized in that wherein the raw material vomiting nut is replaced by the root bark of shaggy-fruited dittany.

21, as the preparation method of vomiting nut active component as described in the claim 10, it is characterized in that wherein the raw material vomiting nut is replaced by the root bark of shaggy-fruited dittany, finally collect chloroform or petroleum ether extraction mutually and to be evaporated to relative density be 0.8-1g/cm ³The root bark of shaggy-fruited dittany complete stool extract of ointment shape.

22, the application of vomiting nut active component as claimed in claim 13 in the preparation miticide is characterized in that wherein the raw material vomiting nut is replaced by the root bark of shaggy-fruited dittany.

23, the application of vomiting nut active component as claimed in claim 14 in the preparation miticide is characterized in that wherein the vomiting nut raw material is replaced by the root bark of shaggy-fruited dittany.

24, the application of vomiting nut complete stool as claimed in claim 15 in the preparation miticide farm chemical is characterized in that wherein the raw material vomiting nut is replaced by the root bark of shaggy-fruited dittany.