CN104839229B - Metasequoia Volatile Oil from Seed micro-capsule water dispersible granular fungicide and its technology of preparing - Google Patents

Metasequoia Volatile Oil from Seed micro-capsule water dispersible granular fungicide and its technology of preparing Download PDF

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Publication number
CN104839229B
CN104839229B CN201410055656.3A CN201410055656A CN104839229B CN 104839229 B CN104839229 B CN 104839229B CN 201410055656 A CN201410055656 A CN 201410055656A CN 104839229 B CN104839229 B CN 104839229B
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volatile oil
metasequoia
micro
added
seed
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CN104839229A (en
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杨俊杰
雷振山
陈利军
叶兆伟
陈月华
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Xinyang Agriculture and Forestry University
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Xinyang Agriculture and Forestry University
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Abstract

5 times of amount water are added in metasequoia seed, volatile oil is extracted by steam distillation.Beta cyclodextrin is measured with 8 10 (g/ml) times, 23 times of amount purified waters is added to stir into paste, volatile oil is added, 45 50 DEG C of constant temperature stir 2 3h, and gained paste is dried in vacuo 3 4h, crushed 200 mesh sieve, micro-capsule inclusion compound is made.Then with micro-capsule inclusion compound 60% (weight ratio, the same below), pull open powder 3%, NNO5%, ammonium sulfate 4%, white carbon 25% feeds intake, sets multi-dimensional movement mixing machine and be uniformly mixed.With 3% dried starch training 10 15% starch slurries of system.Above-mentioned material is set in fluid bed granulator, spray starch slurry bonding is pelletized, dry, is prepared into water dispersible granular.Quality evaluation is carried out according to the relevant criterion (GB) that China formulates, it is qualified.

Description

Metasequoia Volatile Oil from Seed micro-capsule water dispersible granular fungicide and its technology of preparing
Technical field
The present invention relates to a kind of botanical fungicides, more particularly to a kind of metasequoia Volatile Oil from Seed micro-capsule water dispersible granular Fungicide and its technology of preparing.
Background technology
China is that agricultural pest endangers more serious country, it was reported that 1648 kinds of China Main Agricultural harmful organism, Wherein 724 kinds of disease, 838 kinds of worm (mite) evil, 64 kinds of weeds, 22 kinds of bandicoot.According to statistics, average every under conditions of not preventing Year causes the cereal crops underproduction 15% or so, 20% or more the cotton underproduction, the damage of outbreak year part due to the harm of harmful organism Mistake substantially exceeds throughout the year.Chemical pesticide has played important function in terms of control agricultural pest, protection agricultural production security. But there are disadvantages such as " 3R " (drug resistance resistance remain residue, then ferocious sticks up resurgence) in chemical pesticide End, and grow in intensity.The exploitation of botanical pesticide can be to avoid the generation of the above problem.Antifungal activity is screened from plant Substance is the important directions of current fungicide research and development.
Metasequoia is single kind of metasequoia (Metasequoia glyptostroboides of Gymnospermae taxodiaceae plant metasequoia Hu et Cheng), it is the rare few survivors's species in the world.According to《Chinese medicine resource will is wanted》Record its leaf, seed have it is clearing heat and detoxicating, The effect of anti-inflammatory analgetic, swells and ache for ulcerative carbuncle, the diseases such as moss sore,《Mingyi Bielu》Middle product are classified as, meaning cooking is washed, and ulcer on the shank can be controlled.《This Careless detailed outline is picked up any lost article from the road》It carries san-mou oil and controls all stubborn dermatitis.The antifungic action of metasequoia is not only applied in medicine, is agriculturally also being had Wide application prospect.Identification and its Determination of Antibacterial Activity of the author to metasequoia seed volatile substance, the results showed that metasequoia seed Volatile oil all has certain inhibiting rate to 8 kinds of plant pathogenic fungis such as Pear black spot bacterium, to garlic leaf blight bacterium, gibberella saubinetii Germ, Pestallozzia theae bacteriostasis rate 60% or more.Metasequoia Volatile Oil from Seed is not yet formulation at present, can be with by its microencapsulation The influence of the external conditions such as light, oxygen, temperature, pH value is avoided, the lasting period is extended.Water dispersion granule belongs to environmentally friendly dose Type, non-target organism and environment are influenced in use it is small, carry out pesticide micro-capsule water dispersion granule research have compared with Big social value and economic value.
Invention content
The problems such as in order to solve short general chemical fungicide lasting period, environmental hazard, the present invention provides a kind of metasequoia kinds The micro-capsule water dispersion granule and its technology of preparing of sub- volatile oil, this method is simple and practicable, at low cost, and effect on environment is small, and medicine The agent lasting period is long.
The technical solution adopted by the present invention is:
5 times of amount water are added in metasequoia seed, volatile oil is extracted by steam distillation.β-ring is measured with 8-10 (g/ml) times Dextrin adds 2-3 times to measure purified water and stirs into paste, and volatile oil is added, and 45-50 DEG C of constant temperature stirs 2-3h, and gained paste vacuum is dry Dry 3-4h crushed 200 mesh sieve, micro-capsule inclusion compound be made.Then it with micro-capsule inclusion compound 60% (weight ratio, the same below), pulls open Powder 3%, NNO5%, ammonium sulfate 4%, white carbon 25% feed intake, and set multi-dimensional movement mixing machine and are uniformly mixed.With 3% dried starch Training 10-15% starch slurries processed.Above-mentioned material is set in fluid bed granulator, spray starch slurry bonding is pelletized, dry, is prepared into moisture Scattered seed.Quality evaluation is carried out according to the relevant criterion (GB) that China formulates, it is qualified.
The beneficial effects of the invention are as follows:This product no chemical residues have controlled-release function, when extending the effect of volatile oil Between, it can be to avoid the influence of the external conditions such as light, oxygen, temperature, pH value.Water dispersion granule belongs to environmentally friendly dosage form, Non-target organism and environment are influenced during use small.
Specific implementation mode
Volatile oil extracting:Fetch water China fir seed 400g, sets in 3000ml round-bottomed flasks, and 2000ml purified waters are added, and installation is waved Hair oil extractor, extracts 2h, and repetitive operation 5 times obtains faint yellow volatile oil 60ml.
It is prepared by Benexate Hydrochloride:600g beta-cyclodextrins are weighed, 1800ml purified waters are added and stir into paste, by volatile oil It is gradually added into wherein, sets constant temperature in 50 DEG C of water-baths and stir 2h.Gained paste sets YZG-600, and (Nanjing martial prowess pharmaceutical equipment is limited Company) vacuum drying, vacuum degree 0.05MPa, 50 DEG C of temperature control, time 3.5h.Lump material sets the WKF130 Universalpulverizers (Weihe River Mill city north pharmaceutical equipment Manufacturing Co., Ltd) crushing of 200 mesh, obtain the powdered inclusion compound 520g of yellow-white.
Dispensing mixes:Benexate Hydrochloride is taken, pull open powder 26g, NNO43g, ammonium sulfate 35g, white carbon 217g are weighed. Above-mentioned material is set into SHB-10 Multidimensionblenders (Changzhou Hai Jiangyaohua machinery plants), rotating speed 10rpm, 3min.
Binder is prepared:26g cornstarch is weighed, 50ml purified waters are added, stirs into paste, sets on electronic scale, boiling is added Water stirs evenly while hot to 200g.
Granulation drying:Dispensing is added in FL-3 fluid bed granulators, peristaltic pump is added in binder by 60 DEG C of set temperature, Rotating speed 40rpm.After adhesive has sprayed, continue the 40min that boils, discharging.
Quality examination
(1) content inspection:100g granules are taken, is added in 1000ml volatile oil extractors (proportion is less than 1), distillation is added Water 500ml, electric jacket heat slightly boiling 2h, collect volatile oil, weigh.Volatile oil content is calculated as follows, and no less than 5.0%.
(2) thin layer inspection:The absolute ethyl alcohol of equivalent is used to dissolve respectively the volatile oil recycled in volatile oil and granule, point Sample is unfolded by petroleum ether (30~60 DEG C)-acetone (8: 2) of solvent on silica gel thin-layer plate, flings to solvent, lamellae is set It smokes in iodine cylinder, observes under visible light, the volatile oil recycled in volatile oil and granule puts on display 5 brown color spots, Rf It is worth almost the same, it was demonstrated that chemical composition of volatile oil is unchanged in buccal tablet.
(3) measurement of wetability:It is measured, is as follows according to GB/5451 methods:Add the 342mg/L of 500ml In standard hard water 500ml measuring graduates.With weighing disk, quickly the sample of falling 1.0g does not stir in graduated cylinder, and stop-watch records at once 99% sample sinks to the time of graduated cylinder bottom.It is qualification less than 1min.
(4) disintegration measures:100ml tool plug graduated cylinders equipped with 90ml distilled water are placed in 25 DEG C of water-baths, are added 0.5 gram Sample clamps the middle part of graduated cylinder, clogs nozzle, is rotated around center with the speed of 8r/min, until sample is disintegrated completely in water, Disintegration time is recorded, it is qualification to be less than 3min.
(5) suspensibility measures:The measurement of preparation suspensibility is with reference to GB/T14825-2006 agricultural-chemical suspension rate assay methods.Greatly It is qualification in 80%.
(6) dispersibility measures:The dispersibility that preparation is estimated using graduated cylinder method, when redispersibility, the last number of reversals is less than 10 times are qualification.
(7) wet screening residual volume measures:With reference to the wet screening analysis method of CIPAC/MT167 water dispersible granules, it is less than 0.3% It is qualified.
The test of pesticide effectiveness
In order to preferably verify the practical application effect of the present invention, illustrate effect of the present invention with experiment below.
(1) bacteriostasis of metasequoia Volatile Oil from Seed
For trying fungicide:Metasequoia Volatile Oil from Seed
For trying strain:Garlic leaf blight bacterium (Stemphylium botryosum), wheat scab (Fusarium graminearum)
Assay method:Growth rate method
The PDA culture medium of 15mL50 DEG C or so thawing is accurately added at the culture dish ware bottom of diameter 90mm, shakes up and thickness is made Thin uniform tablet, tablet center are inoculated with the plant pathogenic fungi bacteria cake of one piece of a diameter of 5mm.Then it is xeothermic that one is placed in ware lid The diameter 11mm circular filter paper pieces of sterilizing draw a certain amount of metasequoia Volatile Oil from Seed using 10 μ L micro syringes and are added drop-wise to filter On the scraps of paper.The dosage of volatile oil sets 8 processing, respectively 0.5,1.0,1.5,2.0,2.5,5.0,10.0,20.0 μ L, with only altogether It is control to put a filter paper and volatile oil is not added dropwise.It is repeated 3 times.Ware bottom ware lid make-up, sealed membrane sealing, 25 DEG C are inverted culture, 3d After measure colony diameter, right-angled intersection takes the average value of 2 data, calculates bacteriostasis rate.
Bacteriostasis rate=(control colony growth diameter-processing colony growth diameter)/control colony growth diameter × 100%
The bacteriostasis of 1 metasequoia Volatile Oil from Seed of table
The toxicity test result of 2 metasequoia Volatile Oil from Seed of table
Test result shows that metasequoia Volatile Oil from Seed has garlic leaf blight bacterium and wheat scab and inhibits to make well With.
(2) field control effectiveness test
In order to preferably verify the practical application effect of the present invention, illustrate that the field efficacy of the present invention tries with example below Test effect.
The application of fungicide of the present invention is to prevent crop disease as the main purpose, according to different diseases type and plant size Determine that the administration dosage of unit area, generally per hectare apply 100-150g.
Reagent agent:Microcapsule product, 40% pyrimethanil prepared by the present invention
Subjects:Garlic leaf blight bacterium, wheat scab
Experiment grouping:20 cells are randomly choosed in field, are individual protecting field per cell per plot area 50m2, 20 cells are randomly divided into 4 groups, every group of 5 repetitions, every group of fungicide 100g/hm2 prepared respectively using the present invention is used A indicates that 120g/hm2 is indicated with B, and 40% pyrimethanil sprays 150g/hm2, is indicated with C, and clear water control is indicated with D, Dispenser when field starts morbidity, sprays once every 7d, applies altogether 3 times, and spray value is according to each group of design concentration with the leaf that sprays Until piece liquid drips.
Investigation method:7d and 14d are investigated after last time dispenser.Per cell using 5 points of samplings, every investigation 5 Strain, record morbidity severity, and calculate each cell disease index.Control effect is calculated according to following formula:
Control effect (%)=(check plot disease refer to-treatment region disease refer to)/check plot disease refers to × 100.
Preventive effect of the 3 metasequoia seed hair oil microcapsule formulations of table to garlic leaf blight bacterium and kind wheat scab
As it can be seen that 2 of bactericide of the present invention handle A and B, to garlic leaf blight bacterium, wheat scab from table Preventive effect be above common chemical bactericide C.And 2 processing of fungicide of the present invention are to garlic leaf blight bacterium, gibberella saubinetii The preventive effect of disease extends and increases at any time;And the extension of the preventive effect of common chemical bactericide processing C at any time reduces.Thus may be used See that fungicide release of the present invention is slow, the lasting period is long, can reduce the dispenser frequency of pesticide, cost-effective.

Claims (1)

1. a kind of metasequoia Volatile Oil from Seed micro-capsule water dispersible granular fungicide, it is characterized in that:By metasequoia Volatile Oil from Seed β-ring Dextrin is made micro-capsule inclusion compound, micro-capsule inclusion compound 60% (weight ratio, the same below), pull open powder 3%, NNO5%, ammonium sulfate 4%, White carbon 25%, feeds intake, and is placed in multi-dimensional movement mixing machine and is uniformly mixed, and a concentration of 10-15% starch is made with 3% dried starch training Slurry, above-mentioned material is placed in fluid bed granulator, and spray starch slurry bonding is pelletized, dry, is prepared into water dispersion granule.
CN201410055656.3A 2014-02-14 2014-02-14 Metasequoia Volatile Oil from Seed micro-capsule water dispersible granular fungicide and its technology of preparing Expired - Fee Related CN104839229B (en)

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CN108096291B (en) * 2017-12-27 2021-05-04 信阳农林学院 Injection prepared from volatile oil of Cunninghamiae Lanceolatae and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996039822A1 (en) * 1995-06-07 1996-12-19 Zeneca Limited Dry water-dispersible compositions of microencapsulated pesticides
CN101647431A (en) * 2009-09-18 2010-02-17 华南师范大学 Pesticide microcapsule granule and preparation method thereof
CN101743960A (en) * 2010-02-01 2010-06-23 吴学民 Thiacloprid microcapsule powder agent, suspending agent and preparation method and application thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996039822A1 (en) * 1995-06-07 1996-12-19 Zeneca Limited Dry water-dispersible compositions of microencapsulated pesticides
CN101647431A (en) * 2009-09-18 2010-02-17 华南师范大学 Pesticide microcapsule granule and preparation method thereof
CN101743960A (en) * 2010-02-01 2010-06-23 吴学民 Thiacloprid microcapsule powder agent, suspending agent and preparation method and application thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
水杉种子挥发物质的鉴定及其抗菌活性测定;杨俊杰 等;《中国生态农业学报》;20100915;第18卷(第5期);第1018-1021页;第1021页表2以及右栏最后一段 *

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