CN106501413A - A kind of method of inspection of corn Pesticide Residues - Google Patents
A kind of method of inspection of corn Pesticide Residues Download PDFInfo
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- CN106501413A CN106501413A CN201611083571.1A CN201611083571A CN106501413A CN 106501413 A CN106501413 A CN 106501413A CN 201611083571 A CN201611083571 A CN 201611083571A CN 106501413 A CN106501413 A CN 106501413A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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Abstract
The invention discloses a kind of method of inspection of corn Pesticide Residues, by the nicosulfuron spray solution of one group of concentration in gradient distribution in battery of tests soil, after sprinkling on test soil seeding corn；The pore water in situ for collecting all soil in 1 day after sprinkling, determines the nicosulfuron concentration in pore water in situ；After cultivating some days, corn plant height is determined；Nicosulfuron concentration IC50 in pore water in situ when the dose-effect curve equation and corn plant height inhibiting rate that finally fitting obtains nicosulfuron concentration in corn plant height and the pore water in situ is 50%；The nicosulfuron concentration in soil in-situ pore water to be measured is determined, according to the plant height inhibiting rate of described this kind of soil maize planting of dose-effect curve prediction equation.The present invention is simple to operate, quickly, dose-effect curve equation and soil situ hole water concentration to be measured according to nicosulfuron in soil, the phytotoxicity of nicosulfuron in energy fast prediction soil to be measured.
Description
Technical field
The present invention relates to chemistry security evaluates field, and in particular to a kind of inspection party of corn Pesticide Residues
Method.
Background technology
The discovery of Shi Yuan industry companies of Japan of nicosulfuron system, the sulfonylureas that 1987-1988 is developed jointly with E.I.Du Pont Company
Class herbicide kind, it are sold in the U.S. with trade name Accent1991, are registered for corn within 1996.Nicosulfuron enters
Enter China's existing more than ten years, as its consumption is low, effect is good, is popular.
The medicament is inner sucting conduction type sulfonylurea herbicide, can pass through plant stem-leaf and root absorption and rapidly wooden
Portion and bast conduction, by suppressing the activity of acetolactate synthestase, hinder the synthesis of branched-chain amino acid, so as to affect plant
Cell division, makes weeds stop growing, final dead.Weeds can be stopped growing after absorbing medicament quickly, typically after administration 4～
There is within 5 days poisoning symptom, damage symptoms turn yellow for lobus cardiacus, chlorosis, blade tip, leaf sheath aubergine.Annual grassy weeds 20 days or so is dead
Die, the above perennial broadleaf weed of 6 leaves is suppressed, stops growing, high dose can be lethal.
But the extensive application with herbicide nicosulfuron, nicosulfuron is to when stubble chemical injury of crops and residual medicine in recent years
Evil is than more prominent.After nicosulfuron is applied in certain areas, some corn general planting kinds generate more serious poisoning.Corn
3～5 phase foliar sprays apply 5～10d corn lobus cardiacus chlorisis, flavescence after nicosulfuron, or irregular chlorisis spot occurs in blade.Some leaves
Piece crispaturas into tubular, leaf margin shrinkage, lobus cardiacus oxtail shape, it is impossible to normal extraction.Corn growth is suppressed, and plant is downgraded, and
Possible generation part is grown thickly, secondary shoot.Poisoning is light to restore normal growth, serious impact yield.
Residual herbicide is an outstanding problem in lasting rudimental herbicide use to the harm of late stubble sensitive crop.Soil
The herbicides such as middle residual herbicides imazethapyr, Pendimethalin, Flumetsulam, nicosulfuron are caused to late stubble sensitive crop
Harm.The safety evaluatio for remaining herbicide damage in soil is significant to the plantation of succession crop.
Evaluate herbicide and biologicall test and chemical method can be used to crop safety.The biologicall test cycle is long, takes.
Chemical method has the advantages that rapid sensitive.However, as soil physico-chemical property (pH, content of organic matter etc.) is different, difference is native
In earth, herbicide has different biological effectivenesses, traditional phytotoxicity index for determining and calculating acquisition based on total concentration
(EC50 or IC50) is generally different because soil types is different, does not have comparativity each other.Therefore, exploitation one kind directly can be surveyed
The fixed chemical method to plant valid density, sets up and can obtain the residual herbicide phytotoxicity to different soils with comparativity
Evaluation method, has important practical significance to the harm of succession crop to residual herbicide in accurate fast prediction soil.
Content of the invention
The invention provides a kind of method of inspection of corn Pesticide Residues, nicosulfuron in energy fast prediction soil
Phytotoxicity.
A kind of method of inspection of corn Pesticide Residues, including：
(1) by the nicosulfuron spray solution of one group of concentration in gradient distribution in battery of tests soil, in test soil after sprinkling
Seeding corn on earth；
(2) pore water in situ of all soil is collected within 1 day after spraying, and determines the nicosulfuron concentration in pore water in situ；Culture
Behind some days, corn plant height is determined；Finally fitting obtains the agent of nicosulfuron concentration in corn plant height and the pore water in situ
Nicosulfuron concentration IC50 in pore water in situ when graded effect curvilinear equation and corn plant height inhibiting rate are 50%；
(3) the nicosulfuron concentration in soil in-situ pore water to be measured is determined, according to described dose-effect curve prediction equation
The plant height inhibiting rate of this kind of soil maize planting.
Corn plant height inhibiting rate is 50% to refer to that a height of blank of corn plants that plants in the soil after sprinkling nicosulfuron is right
According to a group half for corn plant height.
After the sprinkling nicosulfuron of test soil described in step (1), water content is the 70～75% of maximum water holding capacity.
The water yield kept when being full of water also known as the whole holes of soil saturation water-holding capacity, i.e. soil by maximum water holding capacity,
In step (1), the water content of test soil is controlled by the amount of control sprinkling nicosulfuron solution, while arranging blank
Group, the water content of blank control group soil are controlled with nicosulfuron solution usage identical water by sprinkling.
The concentration of nicosulfuron in the test soil of nicosulfuron is sprayed with described in step (1) in 0.25～16mg/kg
Between increase in gradient, meet on the premise of test requirements document by adjusting the phonetic sulphur of cigarette in the water content of the soil of control maize planting
The concentration of nicosulfuron in grand solution, makes the concentration of nicosulfuron in test soil increase between 0.25～16mg/kg in gradient
Long, typically increase in twice gradient, i.e., in described test soil, the concentration of nicosulfuron is set to 0.25,0.5,1,2,4,8 and
16mg/kg.
The pore water in situ is collected using centrifugal filtration.Specially：Fetch earth earth 8000 × g of centrifugal force at 21～25 DEG C
Centrifugation 80min.Directly take the soil to be put in the filter inside ultra-filtration centrifuge tube, filter under these conditions, obtain
The pore water in situ, method are simple, convenient and swift.
In the pore water in situ, the measure of nicosulfuron adopts high performance liquid chromatography, convenient and swift, only need to set height
The testing conditions and standard specimen of effect liquid phase chromatogram, just quickly can detect the concentration of nicosulfuron in pore water in situ one by one, high
The testing conditions of effect liquid phase chromatogram are：Chromatographic column：4.6mm (id) × 250mm, Eclipse XDB-C18,5 μm of particle diameter；Flowing
Phase：Acetonitrile：Water (0.1% formic acid)=35:65；Flow velocity：1mL/min；Detection wavelength：240nm；Sample size：20μL；Column temperature：30
℃.With nicosulfuron as standard specimen.
Described in step (1), the planting conditions of corn are：25 ± 1 DEG C of temperature, 14～16h/d of photoperiod, intensity of illumination 350
～400 μ E/m2/s, humidity are 75～85%.Test group and control group are cultivated in same planting conditions, and its incubation time can
Can be adjusted according to detection needs, typically cultivate 14～16 days.
Beneficial effects of the present invention：
The present invention is directly separated soil in-situ pore water using centrifugal filter device and adopts with nicosulfuron as target herbicide
HPLC determines nicosulfuron concentration therein, is set up suitable for dissimilar on the basis of nicosulfuron concentration in pore water in situ
The residual nicosulfuron of soil is to corn toxicity assessment method.The method is simple to operate, quickly, according to nicosulfuron in a kind of soil
Dose-effect curve and unknown soil situ hole water concentration in earth, the plant of nicosulfuron in the unknown soil of energy fast prediction
Thing toxicity.
Specific embodiment
For the ease of it will be appreciated by those skilled in the art that the present invention is described further below in conjunction with embodiment.
Embodiment 1
(1) soil collecting
5 kinds of soil pick up from Xiaoshan, Zhejiang, Jinhua, Hua Jiachi school districts, Nanchang and Heilongjiang Province's Yichun, are 0～20cm
Topsoil, the fresh soil of collection, crossing 2mm sieves after air-drying, to be placed under normal temperature (20～25 DEG C) standby.
(2) soil treatment
The various soil of 200g dry weights are weighed in plastic tub, a certain amount of nicosulfuron aqueous solution, stirring are sprayed with plastics watering can
Nicosulfuron and soil is fully mixed, make soil moisture content be maximum water-holding capacity 70%, final water content is respectively：Xiaoshan
Soil 24%；Jinhua soil 22%；Jiangxi soil 24%；Hua Jiachi soil 28%；Heilungkiang soil 30%.
According to biologicall test pilot study, interpolation concentration of the nicosulfuron in different soils is：Xiaoshan soil 0,0.25,
0.5,1,2,4mg/kg；Jiangxi, Jinhua, Hua Jiachi soil 0,0.5,1,2,4,8mg/kg；Heilungkiang soil 0,1,2,4,8,
16mg/kg.After process soil is transferred to volume about 0.5L flowerpots, covered with masking foil and 24h are balanced after 25 DEG C.
(3) plant biological is determined
The corn seed of 5 grain germinations is equably planted in flowerpot, planting depth is about 1cm, then planted with soil covering is processed
Son.The flowerpot of maize planting is positioned in artificial climate incubator, condition of culture be temperature (25 ± 1) DEG C, photoperiod 16h:8h
(illumination: dark), intensity of illumination is 350 μ E/m2/s, and humidity is 80%, cultivates 14 days.
(4) soil in-situ pore water concentration mensuration
Soil sampling 20.0g is put in the filter inside ultra-filtration centrifuge tube, in centrifugal force, be centrifuged under the conditions of 21 DEG C (8000 ×
G, 80min) collect pore water in situ and be directly used in high performance liquid chromatography detection.
Further, found with logistic curve matchings, nicosulfuron is to corn plant height inhibiting rate and pore water in situ
The correlation of middle nicosulfuron concentration is significantly improved compared with nicosulfuron total concentration in soil, is indicated above cigarette in pore water in situ phonetic
The grand concentration of sulphur is represented in soil to the effective herbicide concentration of plant, can be used to detect the poisoning remained in soil.
According to a kind of suppression curve figure and unknown soil situ pore water of the nicosulfuron in soil to corn plant height
Concentration, the phytotoxicity of nicosulfuron in the unknown soil of energy fast prediction.For example according to Xiaoshan, Jinhua, Jiangxi and Hua Jiachi soil
It is Y=1.69x-0.24 that earth situ hole water concentration and corn plant height inhibiting rate calculate dosage effect equation, and Y is probable value, x
For log concentration, according to corn plant height inhibiting rate in the soil of prediction equation Heilungkiang it is：3.60%th, 8.10%, 20.47%,
43.04%th, 68.99%, measured value is：7.98%th, 13.07%, 19.75%, 37.91% and 71.62%, predictablity rate compared with
High.
Said method detection is toxicity of the nicosulfuron to corn plant height in soil, can also detect to corn germination
The toxicity of rate, fresh weight etc..
Claims (8)
1. a kind of method of inspection of corn Pesticide Residues, it is characterised in that include：
(1) by the nicosulfuron spray solution of one group of concentration in gradient distribution in battery of tests soil, in test soil after sprinkling
Seeding corn on earth；
(2) pore water in situ of all soil is collected within 1 day after spraying, and determines the nicosulfuron concentration in pore water in situ；Culture
Behind some days, corn plant height is determined；Finally fitting obtains the agent of nicosulfuron concentration in corn plant height and the pore water in situ
Nicosulfuron concentration IC50 in pore water in situ when graded effect curvilinear equation and corn plant height inhibiting rate are 50%；
(3) the nicosulfuron concentration in soil in-situ pore water to be measured is determined, according to described dose-effect curve prediction equation
The plant height inhibiting rate of this kind of soil maize planting.
2. method according to claim 1, it is characterised in that after the sprinkling nicosulfuron of test soil described in step (1)
Water content for maximum water holding capacity 70～75%.
3. method according to claim 1, it is characterised in that be sprayed with the test soil of nicosulfuron described in step (1)
In earth, the concentration of nicosulfuron increases between 0.25～16mg/kg in gradient.
4. method according to claim 3, it is characterised in that the concentration of nicosulfuron is set in the test soil
0.25th, 0.5,1,2,4,8 and 16mg/kg.
5. method according to claim 1, it is characterised in that the pore water in situ is collected using centrifugal filtration.
6. method according to claim 1, it is characterised in that the measure of nicosulfuron is using high in the pore water in situ
Effect liquid phase chromatogram.
7. method according to claim 1, it is characterised in that the planting conditions of corn are described in step (1)：Temperature 25
± 1 DEG C, 14～16h/d of photoperiod, 350～400 μ E/m2/s of intensity of illumination, humidity are 75～85%.
8. method according to claim 1, it is characterised in that culture determined corn plant height after 14～16 days in step (2).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611083571.1A CN106501413A (en) | 2016-11-30 | 2016-11-30 | A kind of method of inspection of corn Pesticide Residues |
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| CN201611083571.1A CN106501413A (en) | 2016-11-30 | 2016-11-30 | A kind of method of inspection of corn Pesticide Residues |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108918709A (en) * | 2018-07-12 | 2018-11-30 | 河北医科大学 | Screening, quantitative detecting method and the application of common herbicide in a kind of blood |
| CN109239221A (en) * | 2018-10-02 | 2019-01-18 | 丁立平 | The gas chromatography-mass spectrometry of three kinds of trace imidazolinone herbicides in a kind of measurement bean powder |
| RU2711561C1 (en) * | 2018-12-25 | 2020-01-17 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Московский государственный университет имени М.В. Ломоносова" (МГУ) | Method of assessing the effectiveness of the ameliorant for reducing soil toxicity by the level of sprouting stimulation and developing seeds of cereal crops |
| CN110800412A (en) * | 2019-11-18 | 2020-02-18 | 湖南农业大学 | Method for preventing and treating phytotoxicity of residual herbicide to crops by using carbon nano tube |
| CN118191244A (en) * | 2024-05-16 | 2024-06-14 | 江西农业大学 | Evaluation method for influence of residual clomazone on crops |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108918709A (en) * | 2018-07-12 | 2018-11-30 | 河北医科大学 | Screening, quantitative detecting method and the application of common herbicide in a kind of blood |
| CN108918709B (en) * | 2018-07-12 | 2021-05-18 | 河北医科大学 | Screening and quantitative detection method for common herbicides in blood and application |
| CN109239221A (en) * | 2018-10-02 | 2019-01-18 | 丁立平 | The gas chromatography-mass spectrometry of three kinds of trace imidazolinone herbicides in a kind of measurement bean powder |
| RU2711561C1 (en) * | 2018-12-25 | 2020-01-17 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Московский государственный университет имени М.В. Ломоносова" (МГУ) | Method of assessing the effectiveness of the ameliorant for reducing soil toxicity by the level of sprouting stimulation and developing seeds of cereal crops |
| CN110800412A (en) * | 2019-11-18 | 2020-02-18 | 湖南农业大学 | Method for preventing and treating phytotoxicity of residual herbicide to crops by using carbon nano tube |
| CN118191244A (en) * | 2024-05-16 | 2024-06-14 | 江西农业大学 | Evaluation method for influence of residual clomazone on crops |
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