CN105341010B - A kind of Radix Curcumae activity extract, biocide preparation and its application - Google Patents

A kind of Radix Curcumae activity extract, biocide preparation and its application Download PDF

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Publication number
CN105341010B
CN105341010B CN201510900123.5A CN201510900123A CN105341010B CN 105341010 B CN105341010 B CN 105341010B CN 201510900123 A CN201510900123 A CN 201510900123A CN 105341010 B CN105341010 B CN 105341010B
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China
Prior art keywords
radix curcumae
extract
activity
extractant
activity extract
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CN201510900123.5A
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CN105341010A (en
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龙章富
陈琴
刘庆亚
陈次琼
陈子柱
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Sichuan University
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Sichuan University
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/40Liliopsida [monocotyledons]
    • A01N65/48Zingiberaceae [Ginger family], e.g. ginger or galangal

Abstract

The present invention provides a kind of Radix Curcumae activity extract, biocide preparation and its applications, by the Radix Curcumae cauline leaf of drying and crushing or root tuber extractant are extracted 8~for 24 hours, then 0.5~2h is extracted under 30~60Hz frequency ultrasonic waves under the conditions of 30~50 DEG C, collects leaching liquor;Leaching liquor is rotated to evaporation and concentration at 30~55 DEG C, medicinal extract shape Radix Curcumae activity extract is obtained after separation and Extraction agent, then medicinal extract shape Radix Curcumae activity extract is obtained into finished product Radix Curcumae activity extract with extractant extraction and separation again.Medicinal extract shape Radix Curcumae activity extract, the finished product Radix Curcumae activity extract of the present invention is used equally for inhibiting and killing plant pathogenic fungi, and can be used for preparing fungicide.Preparation method of the present invention is simple, can effectively press down and kill various plants disease fungus;Material of germicide source of the present invention is wider, bioactivity is high, contamination-free residual, and with ultrasonic wave extraction, active material discharges more comprehensively.

Description

A kind of Radix Curcumae activity extract, biocide preparation and its application
Technical field
The invention belongs to a kind of plant pesticide technology more particularly to Radix Curcumae activity extract, biocide preparation and its applications.
Background technology
Pesticide be for the importance of agricultural production it is unquestionable, pesticide can be used for kill insect, fungi and other The biology of damage to crops growth.The pesticide used earliest has DDT, six six six etc., and they can largely eliminate pest, still, it Stability it is good, can long-term existence in the environment, and constantly accumulate in animals and plants and human body, be eliminated thus.
It used organophosphorus pesticide, such as DDVP instead later, and substituted initial pesticide.However they contain P elements, are easy Cause aquatic organism eutrophication.
It can be seen that the use of pesticide, on the one hand brings economic benefit to the mankind really, but on the other hand also gives the mankind The environment of Lai Yi existence brings huge harm.
According to the literature, pesticide utilization rate is generally 10%, and about 90% pesticide residue is caused to environment in the environment Pollution.Largely lost pesticide is evaporate into air, is flowed into water body, and sedimentation aggregation in the soil, pollutes farming animals fishing fruit product, And human body is transferred to by the enrichment of food chain, serious harm is generated to health.
Therefore, it is comparatively ideal method that appliable plant source biological pesticide, which carrys out controlling plant diseases, and one side plant resources are rich Richness can provide huge material base for exploitation;On the other hand, botanical pesticide stems purely from plant, and compound has formd The cyclic metabolic pathway of oneself, nonhazardous, noresidue more will not generate pollution to environment.
Invention content
The primary purpose of the present invention is that providing a kind of Radix Curcumae activity extract, it is intended to solve chemical pesticide residual to environment Endanger big problem.
It is still another object of the present invention to provide the application of the Radix Curcumae activity extract in terms of inhibiting and killing plant pathogenic fungi.
It is still another object of the present invention to provide a kind of biocide preparations prepared by above-mentioned Radix Curcumae activity extract.
The invention is realized in this way a kind of Radix Curcumae activity extract, which passes through following steps system It is standby to obtain:
(1) the Radix Curcumae cauline leaf of drying and crushing or root tuber extractant are extracted 8~for 24 hours, then under the conditions of 30~50 DEG C 0.5~2h is extracted under 30~60KHz frequency ultrasonic waves, collects extracting solution;Wherein, the quality volume of the Radix Curcumae and extractant Than for 1g:(5~20) ml;The extractant is 35~100wt% methanol, 85~98wt% ethyl alcohol and 85~98wt% acetone At least one of;
(2) leaching liquor for obtaining step (1) rotates evaporation and concentration at 30~55 DEG C, and medicinal extract is obtained after separation and Extraction agent Shape Radix Curcumae activity extract.
Preferably, in step (1), the extractant is the ethyl alcohol of 85~98wt%.
Preferably, further include step after step (2):
(3) the medicinal extract shape Radix Curcumae activity extract that step (2) obtains is obtained into finished product Radix Curcumae with extractant extraction and separation again Activity extract;Wherein, the mass volume ratio of medicinal extract shape Radix Curcumae activity extract and extractant is 1g:(5~20) ml, the extraction It is at least one of n-hexane, petroleum ether and acetone to take agent.
Preferably, in step (3), the extractant is at least one of n-hexane and acetone.
Invention further provides application of the above-mentioned Radix Curcumae activity extract in terms of inhibiting and killing plant pathogenic fungi.
Preferably, the plant pathogenic fungi includes that gibberella saubinetii, horseradish ink enter bacterium, capsicum botrytis cinerea, rape sclerotium Bacterium, tobacco black shank, rice blast fungus, rapeseed clubroot bacterium and botrytis cinerea.
Invention further provides above-mentioned Radix Curcumae activity extracts in the biocide preparation for preparing inhibiting and killing plant pathogenic fungi The application of aspect.
Preferably, the dosage form of the biocide preparation includes aqua, soluble powder, wettable powder, granula and suspension Agent.
Preferably, the plant pathogenic fungi includes that gibberella saubinetii, horseradish ink enter bacterium, capsicum botrytis cinerea, rape sclerotium Bacterium, tobacco black shank, rice blast fungus, rapeseed clubroot bacterium and botrytis cinerea.
Invention further provides the sterilization aqua of above-mentioned inhibiting and killing plant pathogenic fungi, which includes pressing below The each component of mass parts meter:
The organic acid is propionic acid;
The solubilizer is N,N-dimethylformamide;
The auxiliary agent is dodecyl sodium sulfate, diisobutyl sodium naphthalene sulfonate, sldium lauryl sulfate, di-2-ethylhexylphosphine oxide naphthalene sulfonic acids Sodium and to one or more in methoxyl group fatty acyl amido benzene sulfonic acid sodium salt.
The present invention overcomes the deficiencies of the prior art and provide a kind of Radix Curcumae activity extract, fungicide and its application.The present invention Alcohol extract (medicinal extract shape Radix Curcumae activity extract), extract (finished product Radix Curcumae work are obtained by being extracted from Radix Curcumae root tuber and cauline leaf Property extract).Alcohol extract is the Radix Curcumae total extract obtained as extractant using ethyl alcohol or methanol, and extract is with n-hexane or stone Oily ether is the essence extract that alcohol extract is further obtained by extraction in extractant.Alcohol extract and extract may be incorporated for suppression and kill plant Disease fungus has killed preferable activity to the suppression of plant pathogenic fungi.In contrast, the effect of extract inhibiting and killing plant pathogenic fungi Fruit is more preferable.
Invention further provides a kind of biocide preparation prepared by Radix Curcumae activity extract, it can be used for preparing suppression and kill Plant pathogenic fungi and mushroom disease fungus preparation, are especially used to prepare suppression and kill gibberella saubinetii (Fusarium Graminearum), Sclerotinia sclerotiorum (Phoma wasabiae), horseradish ink enter bacterium (Sclerotinia sclerotiorum) With the preparation of capsicum botrytis cinerea (Botrytis cinerea) etc..The present invention utilizes Radix Curcumae activity extract, is equipped in the art A variety of dosage forms of the present invention, the agent of preparation can be made in auxiliary agent known in technical staff (including solubilizer, filler, synergist etc.) Type can be the dosage form of the forms such as aqua, soluble powder, wettable powder, granula or suspending agent.Further, of the invention A kind of fungicide is provided, active constituent content is:0.1~90 part of Radix Curcumae extract, 0.01~5 part of propionic acid, auxiliary agent (12 Sodium alkyl sulfonate, diisobutyl sodium naphthalene sulfonate, sldium lauryl sulfate, sodium methylene bis-naphthalene sulfonate and to methoxyl group fatty acyl amido It is one or more in benzene sulfonic acid sodium salt) 0.01~1 part.
Compared with the prior art the shortcomings that and deficiency, the invention has the advantages that:
(1) Radix Curcumae activity extract preparation method of the present invention is simple, can effectively press down and kill various plants disease fungus, such as wheat Gibberella, horseradish ink enter bacterium etc., and botanical pesticide is prepared using Radix Curcumae, not only have in terms of Agriculture Ecological Environment Protection important Meaning, and the comprehensive utilization to Radix Curcumae resource can be expanded, production cost is reduced, makes this industry that there is broader development Foreground;
(2) material of germicide source of the invention is wider, bioactivity is high, contamination-free residual, with ultrasonic wave extraction, Active material discharges more comprehensively.
(3) present invention is in the comprehensive development and utilization of Radix Curcumae stalk, the production cost for reducing its natural products fungicide, resource Recycle etc., there is important theory significance and potential application value.
Description of the drawings
Fig. 1 is the blank control group before bacteriostatic experiment in effect example 3 of the present invention;
Fig. 2 is in effect example 3 of the present invention using the fungistatic effect figure after sterilization aqua 3.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and It is not used in the restriction present invention.
Embodiment 1
(1) the fresh Radix Curcumae cauline leafs of 1g are dried in the shade and extracts 8h with 20ml 98wt% methanol after crushing, then under the conditions of 40 DEG C 2h is extracted under 60KHz frequency ultrasonic waves, with Buchner funnel negative pressure filtration, removes residue, obtains leaching liquor;
(2) leaching liquor for obtaining step (1) is concentrated under 45 DEG C of water-baths with Rotary Evaporators rotary evaporation, detaches methanol After obtain medicinal extract shape Radix Curcumae activity extract Isosorbide-5-Nitrae DEG C preservation.
Embodiment 2
(1) residue that 1 step of embodiment (1) obtains is used to the first for the 98wt% for being equivalent to about 6 times of volumes of material quality again Alcohol futher stirs, and 1.0h is extracted under 60KHz frequency ultrasonic waves under the conditions of 40 DEG C, and the active constituent in Radix Curcumae is made fully to carry Go out, with Buchner funnel negative pressure filtration, removes residue, collect leaching liquor;
(2) leaching liquor that 1 step of embodiment (1) obtains is merged with the leaching liquor in the present embodiment step (1), will be merged Leaching liquor under 35 DEG C of water-baths with Rotary Evaporators rotary evaporation concentrate, detach methanol after obtain medicinal extract shape Radix Curcumae activity extraction Object 2.
Embodiment 3
(1) the fresh Radix Curcumae root tubers of 1g are dried in the shade and uses 5ml 85wt% alcohol steeps for 24 hours after crushing, then under the conditions of 40 DEG C 0.5h is extracted under 30KHz frequency ultrasonic waves, with Buchner funnel negative pressure filtration, removes residue, obtains root tuber leaching liquor;
(2) leaching liquor for obtaining step (1) is concentrated under 35 DEG C of water-baths with Rotary Evaporators rotary evaporation, separating alcohol After obtain medicinal extract shape Radix Curcumae activity extract 3.
Embodiment 4
(1) the fresh Radix Curcumae cauline leafs of 1g are dried in the shade after crushing, takes the ethyl alcohol for the 95wt% for being equivalent to about 7 times of volumes of material quality About 10h is impregnated at room temperature;
(2) ultrasonic-leaching 0.5h under the conditions of 40 DEG C;With Buchner funnel negative pressure filtration, remove residue, obtains leaching liquor 1.
(3) residue is futher stirred with the ethyl alcohol for the 95wt% for being equivalent to about 6 times of volumes of material quality again, 50 DEG C of conditions Lower ultrasonic-leaching 1.0h, makes the active constituent in Radix Curcumae fully propose, with Buchner funnel negative pressure filtration, removes residue, must soak Extract 2.
(4) merge leaching liquor 1 and leaching liquor 2, filtrate concentrated under 45 DEG C of water-baths with Rotary Evaporators with Rotary Evaporators, Obtain 4, the 4 DEG C of preservations of medicinal extract shape Radix Curcumae activity extract.
Embodiment 5
(1) the fresh Radix Curcumae cauline leafs of 1g are dried in the shade after crushing, take be equivalent to about 7 times of volumes of material quality 100wt% methanol, 98wt% ethyl alcohol and 85wt% acetone impregnate about 10h at room temperature;Methanol, ethyl alcohol, acetone are by isometric than mixing.
(2) ultrasonic-leaching 0.5h under the conditions of 30 DEG C;With Buchner funnel negative pressure filtration, remove residue, obtains leaching liquor 1.
(3) residue is futher stirred with the ethyl alcohol for the 95wt% for being equivalent to about 6 times of volumes of material quality again, 40 DEG C of conditions Lower ultrasonic-leaching 1.0h, makes the active constituent in Radix Curcumae fully propose, with Buchner funnel negative pressure filtration, removes residue, must soak Extract 2.
(4) merge leaching liquor 1 and leaching liquor 2, filtrate concentrated under 30 DEG C of water-baths with Rotary Evaporators with Rotary Evaporators, Obtain 4, the 4 DEG C of preservations of medicinal extract shape Radix Curcumae activity extract.
Embodiment 6
By the medicinal extract shape Radix Curcumae activity extract 2 obtained in 1g embodiments 2 with 5ml n-hexane extractions to gained extract liquor without Until color, up to higher active finished product Radix Curcumae activity extract 1 after extract liquor concentration, and recycle as extractant just oneself Alkane.
Embodiment 7
By the medicinal extract shape Radix Curcumae activity extract 3 obtained in 1g embodiments 3 20ml petroleum ether extractions to gained extract liquor Until colourless, up to higher active finished product Radix Curcumae activity extract 2 after extract liquor concentration, and the stone as extractant is recycled Oily ether.
Embodiment 8
The medicinal extract shape Radix Curcumae activity extract 1 obtained in 1g embodiments 1 is extracted with 10ml n-hexanes and acetone mixture Until gained extract liquor is colourless, up to higher active finished product Radix Curcumae activity extract 3 after extract liquor concentration, and extraction is recycled Solvent.
Embodiment 9
Medicinal extract shape Radix Curcumae activity extract 4,0.01g propionic acid, 0.001g dodecyl sodium sulfonates prepared by 90g embodiments 4 Sodium, the mixing of 20g n,N-Dimethylformamide, add water to be settled to 100ml, and sterilization aqua 1 is obtained after mixing.
Embodiment 10
Finished product Radix Curcumae activity extract 3,5g propionic acid, 0.001g dodecyl sodium sulfates prepared by 0.01g embodiments 7, 0.24g diisobutyl sodium naphthalene sulfonates, the mixing of 0.1g n,N-Dimethylformamide, add water to be settled to 100ml, are killed after mixing Bacterium aqua 2.
Embodiment 11
Medicinal extract shape Radix Curcumae activity extract 4,1g propionic acid, the 0.5g diisobutyl naphthalene sulfonic acids that will be obtained in 50g embodiments 4 Sodium, 0.5g mix methoxyl group fatty acyl amido benzene sulfonic acid sodium salt, 15g n,N-Dimethylformamide, add water to be settled to 100ml, mix Sterilization aqua 3 is obtained after even.
Effect example 1
The medicinal extract shape Radix Curcumae activity extract 4 prepared in a small amount of embodiment 4 is taken, a concentration of 50mg is configured to clear water ml-1Solution is as following experiment ready sample.
The measurement of bioactivity:In in vitro, the antibacterial work of Radix Curcumae extract is measured using mycelial growth rate method Property.Experiment ready sample (mass concentration 50mgmL is taken respectively-1) culture medium is prepared, 5 concentration gradients, i.e. 8mg is made mL-1、4mg·mL-1、2mg·mL-1、1mg·mL-1、0.5mg·mL-1.In plate center, access has been cultivated after tablet solidification The horseradish ink good, growth is consistent enters bacterium bacteria cake (d=5.0mm).A bacteria cake is connect per ware, sterile aqueous media inoculation is added It is used as blank control (CK), each handle to set 3 repetitions, cultivated in constant incubator at 26 DEG C afterwards, until control culture dish bacterium colony Data are recorded when will cover with culture dish.Each bacterium colony measures twice according to crossing method, its bacterium colony is represented with average The calculation formula of size, bacteriostasis rate is as follows:
Colony diameter (mm)=bacterium colony average diameter-bacteria cake diameter (5.0mm)
Bacteriostasis rate (%)=(control colony diameter-processing colony diameter) ÷ compares colony diameter × 100%
Experimental result is as shown in table 1.
1 medicinal extract shape Radix Curcumae activity extract of table enters horseradish ink the inhibition of bacterium
Effect example 2
The finished product Radix Curcumae activity extract 3 prepared in a small amount of embodiment 8 is taken to be configured to a concentration of 20mgml-1Solution conduct The experiment ready sample tested below.
Experiment ready sample (mass concentration 20mgmL is taken respectively-1) culture medium is prepared, 5 concentration gradients are made, i.e., 2mg·mL-1、1mg·mL-1、0.5mg·mL-1、0.25mg·mL-1、0.125mg·mL-1, the assay method ginseng of bioactivity According to effect example 1.The fungistatic effect of Radix Curcumae cauline leaf extract is shown in Table 2.
Inhibition of the 2 finished product Radix Curcumae activity extract of table to gibberella saubinetii
Effect example 3
The sterilization aqua 3 prepared in Example 10 carries out bacteriostatic experiment to gibberella saubinetii, as a concentration of 200 μ of medicine base G/mL (i.e. 0.2mgml-1) (shown in Fig. 1~2, Fig. 1 is the blank control group before bacteriostatic experiment, Fig. 2 to inhibiting rate nearly 100% It is using the fungistatic effect figure after sterilization aqua 3).It can be clearly seen that from table 3, the present invention sterilizes the EC50 of aqua 3 about For 31 μ g/mL (i.e. 0.031mgml-1), before not compounding compared with the EC50 values of (such as effect example 2), the aqua 3 of compounding Its EC50 value reduces 10 times, that is to say, that its dosage can be reduced greatly.
Table 3 sterilizes aqua 3 and carries out bacteriostatic experiment to gibberella saubinetii
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.

Claims (1)

1. a kind of sterilization aqua of inhibiting and killing plant pathogenic fungi, which is characterized in that the sterilization aqua includes in parts by mass Each component:
The organic acid is propionic acid;
The solubilizer is N,N-dimethylformamide;
The auxiliary agent is 0.001 part of dodecyl sodium sulfate and 0.24 part of diisobutyl sodium naphthalene sulfonate;
The described finished product Radix Curcumae activity extract is prepared by following steps:
(1) the Radix Curcumae root tuber of drying and crushing extractant is extracted for 24 hours, then in 30KHz frequency ultrasonic waves under the conditions of 40 DEG C Lower extraction 0.5h collects extracting solution;Wherein, the mass volume ratio of the Radix Curcumae and extractant is 1g:5mL;The extractant is 85wt% ethyl alcohol;
(2) leaching liquor for obtaining step (1) rotates evaporation and concentration at 30~55 DEG C, and it is strongly fragrant that medicinal extract shape is obtained after separation and Extraction agent Golden activity extract;
(3) the medicinal extract shape Radix Curcumae activity extract that step (2) obtains is obtained into finished product Radix Curcumae activity with extractant extraction and separation again Extract;Wherein, the mass volume ratio of medicinal extract shape Radix Curcumae activity extract and extractant is 1g:20ml, the extractant are stone Oily ether.
CN201510900123.5A 2015-12-09 2015-12-09 A kind of Radix Curcumae activity extract, biocide preparation and its application Expired - Fee Related CN105341010B (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101053332A (en) * 2007-05-08 2007-10-17 四川大学 Active constituent of curcuma longa for inhibiting and killing plant pathogenic fungi and its preparation and application

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101053332A (en) * 2007-05-08 2007-10-17 四川大学 Active constituent of curcuma longa for inhibiting and killing plant pathogenic fungi and its preparation and application

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