CN105606729B - A kind of detection method of simulation herbicide cross direction profiles in soil layer - Google Patents
A kind of detection method of simulation herbicide cross direction profiles in soil layer Download PDFInfo
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- CN105606729B CN105606729B CN201510990258.5A CN201510990258A CN105606729B CN 105606729 B CN105606729 B CN 105606729B CN 201510990258 A CN201510990258 A CN 201510990258A CN 105606729 B CN105606729 B CN 105606729B
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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 detection methods of simulation herbicide cross direction profiles in soil layer.The present invention is by taking fomesafen as an example; its distribution in soil layer is tested and analyzed by simulating natural precipitation; the present invention provides a practicable method for detection herbicide residue drug injury problem; to reduce crop loss while effective protection environment; reduce the production cost of equivalent efficacy herbicide; it reduces farmer's burdens, increases farmers' income, there is significant social benefit.Moreover, remains of pesticide has extremely important meaning to pollution-free food production in detection soil.
Description
Technical field
The present invention relates to a kind of detection methods that simulation herbicide is distributed in soil layer, and in particular to simulation herbicide is in soil
The detection method of cross direction profiles in layer.
Background technology
It is planted with the large area of crops, herbicide is also continuously increased using area, some are not long residual, degradable
It is increasingly apparent to the drug injury problem of succession crop with the herbicide of metabolism, prevent to conciliate herbicide environmentally friendly by no means always
It is paid close attention to by various countries scientific worker.How the environment row by the simpler clear herbicide of easy method in the soil
For problem, be scientist need to face, important topic urgently to be resolved hurrily.
Fomesafen (fomesafen) also known as prowers are removed by a kind of diphenyl ether of the prompt sharp Kanggong department exploitation of Britain
Careless agent, due to its herbicide spectrum width, herbicidal effect is good, safe to soybean the advantages that be widely used in Soybean Field and prevent and kill off broad-leaved
Weeds.As frequency of use and dosage increasingly increase fomesafen in Soybean Field, and major soybean production areas winter climate is cold
It is dry, it is unfavorable for the degradation and metabolism of fomesafen, to make the accumulation of fomesafen in the soil increase, limits
Its extensive use.
Invention content
The object of the present invention is to provide a kind of detection method of simulation herbicide cross direction profiles in soil layer, inspections of the invention
Survey method is simple and practicable, can detect the cross direction profiles feelings of herbicide such as fomesafen in soil layer by simulating natural precipitation
Condition.
The detection method of simulation herbicide cross direction profiles in soil layer provided by the present invention, includes the following steps：
1) herbicide is added into soil, obtains soil sample；
2) soil sample and the soil are loaded in the soil sample container of rainfall simulator, and the soil sample position
In the upper layer of the soil, the rainfall simulator includes water container and the soil sample container, and the water is held
Container is connected with the soil sample container, and the pipeline being connected is equipped with control valve, and the soil sample puts the bottom of container
Portion is equipped with several holes A, and a window is opened up on the side wall of the soil sample container；
3) water is added dropwise in the soil sample by the water container into the soil sample container, utilizes sampling handle
The sample that different location in same level at least three kinds of soil sample containers is taken out by the window, through liquid
Phase chromatography detects to obtain the peak area of the sample；
The sampling handle includes a quadrangular, and a bottom surface of the quadrangular is that opening is arranged, another sealing bottom surface
It is arranged, one handle is connected on the bottom surface of sealed set, the side of the quadrangular is equipped with several holes B, utilizes institute
It states handle and the quadrangular is stretched into realization sampling in the soil sample container by the window；
4) standard solution of at least three kinds of herbicides is prepared, under conditions of the liquid chromatographic detection described in step 3)
The standard solution for detecting the herbicide obtains the peak area of the standard solution of the herbicide, with the standard of the herbicide
A concentration of abscissa of solution obtains the mark of the herbicide using the peak area of the standard solution of the herbicide as ordinate
Standard curve between the concentration and peak area of quasi- solution；
5) standard curve that the peak area and step 4) obtained according to step 3) obtains is contained to get to the soil sample
The soil sample of different location or the herbicide concentration in the soil in same level are put in container, is so far realized
Simulate the detection of cross direction profiles of the herbicide in soil layer.
In above-mentioned detection method, in step 2), the filling height of soil sample described in the soil sample container is 5cm.
In above-mentioned detection method, soil sample described in the soil sample container and the soil it is total filling height be
5cm~25cm；
Control of the soil realization to inventory height is loaded in the lower part of the soil sample, as successively in the soil sample
The soil of 5cm is loaded in lower part, obtains the sample of 10cm, 15cm, 20cm and 25cm height, is finally covered in the soil sample
One layer of filter paper on filter paper plus one layer of quartz sand, generates impact, and then influence water in the soil when preventing from being added dropwise water to the soil sample
Flow velocity in sample is uneven；
In step 3), the soil sample of same level or the soil are divided into four etc. using the component in right-angled intersection
Part, the sample per equal portions is then taken out by the sampling handle.
In above-mentioned detection method, the herbicide can be fomesafen；
The concentration of herbicide described in the soil sample can be soil described in 100mg/kg；
The quality moisture content of the soil sample can be 10%.
In above-mentioned detection method, in step 3), the rate of addition of the water can be 23~25 drops/minute, often drip
Volume is 0.08mL.
In above-mentioned detection method, in step 3), before carrying out the liquid chromatographic detection to the sample, the method
Include the steps that the sample is handled as follows：
By the sample wetness, acetonitrile is then added and is impregnated, supernatant is obtained after oscillation and standing；To the supernatant
Sodium chloride is added in liquid, the acetonitrile phase positioned at upper layer is obtained after oscillation and centrifugation, the acetonitrile mutually carries out the liquid chromatogram
Detection；
The time of the immersion can be 1 hour；
The dosage of the acetonitrile can be sample described in 1mL/g；
The mass ratio of the sodium chloride and the sample can be 1：4.
In above-mentioned detection method, in step 3) and step 4), the condition of the liquid chromatographic detection is as follows：
Mobile phase is the mixture of acetonitrile and water, and the volume ratio of the acetonitrile and the water is 60：40；
Flow velocity is 1.0mLmin-1；
Column temperature is 30 DEG C；
Sample size is 20 μ L；
Detection wavelength is 295nm.
It is described to remove using the standard solution of 8 kinds of herbicides of acetontrile in step 4) in above-mentioned detection method
The concentration of the standard solution of careless agent is followed successively by 1mg/kg, 2mg/kg, 5mg/kg, 10mg/kg, 20mg/kg, 50mg/kg, 100mg/
Kg and 200mg/kg.
The present invention realizes simulation herbicide using the rainfall simulator and the sampling handle and laterally divides in soil layer
The detection of cloth.
The present invention tests and analyzes its distribution in soil layer, this hair by taking fomesafen as an example, by simulating natural precipitation
It is bright to provide a practicable method for detection herbicide residue drug injury problem, reduce agriculture while being effective protection environment
Crop damage reduces the production cost of equivalent efficacy herbicide, reduces farmer's burdens, increase farmers' income, and has significant society
It can benefit.Moreover, remains of pesticide has extremely important meaning to pollution-free food production in detection soil.
The present invention has the advantages that：
(1) present invention is applied to the test method that herbicide clay distribution detects by natural precipitation device is simulated, in agricultural
Still belong in field pioneering.
(2) same layer soil is divided by quarter by the component in right-angled intersection, is sampled per equal portions using sampling handle
To detect the distribution of herbicide in the soil, this method herbicide cross direction profiles first Application in detecting soil layer.
Description of the drawings
Fig. 1 is the structural schematic diagram for detecting herbicide rainfall simulator used in the distribution of soil depth.
Fig. 2 is the structural schematic diagram of rainfall simulator of the present invention.
Fig. 3 is the structural schematic diagram of present invention sampling handle.
Fig. 4 is the standard curve between the concentration and peak area of fomesafen.
Fig. 5 is the measurement result schematic diagram of the soil sample rate of recovery in the embodiment of the present invention 1.
Fig. 6 is testing result of the fomesafen of the present invention in soil depth.
Fig. 7 is the measurement result of fomesafen cross direction profiles in soil layer in the embodiment of the present invention 1.
It is respectively marked in figure as follows：
1,1 ' Organic glass column, 2,2 ', 2 " holes, 3,3 ' organic glass bottles, 4 windows, 5 quadrangulars, 6 handles.
Specific implementation mode
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Method in following embodiment, which is respectively provided with, to be repeated to test three times, is averaged.Fomesafen used is a concentration of
100mg/kg, fomesafen standard concentration 98%, a concentration of 250 grams per liter of fomesafen aqua, when use, are diluted to pre-
Phase concentration, concentration is with effective agent gauge.
The method of water sample pre-treatment is as follows in following embodiments：
Correct amount water sampling 20mL is accurate that acetonitrile 20mL, ultrasound is added with quantitative sample injector in 250mL conical flask with cover
Or mechanical shaking extraction 30min, the liquid in conical flask is transferred in the 50mL centrifuge tubes for filling 5gNaCl, after shaking 5min, with
After the speed centrifugation 5min of 5000r/min, taking upper layer acetonitrile, mutually directly upper machine is to be measured.
The method of pedotheque pre-treatment is as follows in following embodiments：
Pedotheque 20g is weighed in 250mL conical flask with cover, deionized water 20mL moist soils are added, then accurately add
Enter acetonitrile (analysis is pure) 20mL and in 250mL conical flask with cover, after impregnating 1 hour, 30min is vibrated, after standing 5min, by supernatant
Liquid is transferred in the 50mL centrifuge tubes for filling 5gNaCl, after shaking 5min, after the speed centrifugation 5min of 5000r/min, is taken
Mutually directly upper machine is to be measured for layer acetonitrile.
The condition of liquid chromatographic detection is as follows in following embodiments：
Mobile phase：Acetonitrile/water (5% phosphoric acid)=60/40 (V/V)；Flow velocity：1.0mL·min-1；Column temperature：30℃；Detect wave
It is long：295nm；Sample size：20μL.
The detection of fomesafen medicine soil depth：
(1) fomesafen standard curve making：Fomesafen standard solution is configured to dilution in acetonitrile a concentration of
1mg/kg, 2mg/kg, 5mg/kg, 10mg/kg, 20mg/kg, 50mg/kg, 100mg/kg and 200mg/kg series standard solution,
High performance liquid chromatography measurement is carried out after water sample pre-treatment, using the concentration x of fomesafen as abscissa, peak area y is vertical sits
It is denoted as figure, obtained standard curve is as shown in Figure 4.
Test result：Standard specimen linear equation is y=27602x+17923, and related coefficient is：R2=0.99909, it is testing
Concentration range in, instrument used herein has preferable linear dependence, the water sample rate of recovery to fomesafen：Standard specimen is dense
The rate of recovery can reach 90% or more when spending 20~200mg/kg, and test result illustrates the pre-treatment side of fomesafen water sample
Method, instrument testing conditions are feasible.
(2) detection of fomesafen medicine soil depth：500g air-dries soil sample and adds 100mg/kg fomesafens respectively
Aqua is realized using rainfall simulator shown in FIG. 1 to soil depth as soil treatment object, soil moisture content 10%
Detection, the rainfall simulator include the Organic glass column 1 that an internal diameter is 10cm, and bottom is equipped with multiple uniform holes 2, and one has
Machine vial 3 is hung upside down on holder, and the aperture that bottom of bottle opens diameter 0.5cm is used for water filling, and machine vial 3 is connected with medical needle tubing
With Organic glass column 1, the control valve of needle tubing is used for adjusting rainfall rate.
Take 7 above-mentioned rainfall simulators, the height of wherein Organic glass column 1 be respectively 5cm, 10cm, 15cm, 20cm,
25cm, 30cm and 35cm, highly just to load 500g soil samples in the Organic glass column of 5cm 1, remaining 6 Bio-Glas is
It loads in the following manner：The lower part of 500g soil samples load successively 500g soil obtain 10cm, 15cm, 20cm, 25cm,
The sample of 30cm and 35cm height covers one layer of filter paper in soil sample, adds one layer of quartz sand, simulated rainfall speed control on filter paper
23~25 drops/minute, the volume often dripped be 0.08mL, 5cm~35cm earth pillars add respectively water 300ml, 400ml, 500ml,
600ml, 700ml, 800ml and 900ml Fluid Dynamics rainfall, simulated rainfall liquid carry out efficient liquid phase after water sample pre-treatment
Chromatography detects.
Test result：As shown in fig. 6, fomesafen detects when soil layer 5cm a concentration of 96.34mg/kg, soil layer 25cm
When fomesafen detection a concentration of 6.91mg/kg, when soil layer is more than 30cm fomesafen detection a concentration of 0, i.e., not
Detect fomesafen.According to above-mentioned test result, the detection that 5~20cm of soil depth carries out cross direction profiles is chosen.
Embodiment 1, the detection for simulating fomesafen medicine cross direction profiles in soil layer
The detection of the soil sample rate of recovery：Fomesafen standard solution is added into blank soil, makes to add concentration in soil sample
Respectively 0,1,5,10,50,100,150mgkg-1, high performance liquid chromatography detection is carried out after soil pre-treatment, as a result such as
Shown in Fig. 5.
Test result：10~150mgkg of liquor strength-1When average recovery rate can reach 90% or more, test result
Illustrate that the fomesafen soil sample pre-treating method that the present invention uses is feasible.
It takes 1 part of 500g to air-dry soil sample and adds 100mg/kg fomesafens aqua as soil treatment object, soil water-containing
Amount 10%, using rainfall simulator shown in Fig. 2 and sampling handle shown in Fig. 3 realization to medicament in soil layer cross direction profiles
Detection, the rainfall simulator include that the Organic glass column 1 ' that an internal diameter is 10cm is used as soil sample container, and bottom is equipped with
Multiple uniform holes 2 ', side wall are equipped with the window 4 of 20 × 8cm, and an organic glass bottle 3 ' is hung upside down on holder, and bottom of bottle is opened
The aperture of diameter 0.5cm is used for water filling, and machine vial 3 ' and Organic glass column 1 ', the control valve of needle tubing are connected with medical needle tubing
For adjusting rainfall rate.It includes a quadrangular 5 to sample handle, and a bottom surface of the quadrangular 5 is that opening is arranged, another bottom
Face is sealed set, and the bottom surface of sealed set connects a handle 6, and 2 holes are equipped on a side of quadrangular 5
2 ", when sampling, quadrangular 5 is stretched to by window 4 using handle 6 and realizes sampling in Organic glass column 1 ', be provided in
The balance for ensureing external pressure in Organic glass column 1 ' when the effect of hole 2 " on the side of quadrangular 5 is sampling, can smoothly take
To soil sample.
Above-mentioned rainfall simulator is taken then to exist highly just to load 500g soil samples in the Organic glass column 1 ' of 5cm
The lower part filling 500g soil of 500g soil samples obtains the sample of 20cm height, one layer of filter paper of covering preferably in soil sample, on filter paper
Add one layer of quartz sand, rainfall 1000ml, 23~25 drops of simulated rainfall speed control/minute simulated rainfall process, the body often dripped
Product is 0.08mL.Sample handle sampling after simulated rainfall shown in Fig. 3 in 5cm, 10cm, 15cm and 20cm soil layer, it is sharp first
Every layer of soil sample is divided into quarter with the component in right-angled intersection, is then stretched to quadrangular 5 by window 4 using handle 6
It is taken out successively per equal portions, by carrying out high performance liquid chromatography detection 100mg/kg fluorine sulfanilamide (SN) after soil sample pre-treatment in machine glass column 1 '
Distribution situation of the careless ether aqua in soil layer.
Test result：As shown in fig. 7,5~20cm soil layers sample A, B, C and D quarter, 5cm, 10cm, 15cm and 20cm
In soil layer, through every layer of 4 equal portions soil sample residual concentration of liquid chromatographic detection, calculate every layer of soil sample concentration variance be respectively 10.6,
3.1,1.1 and 0.03, the smaller otherness of variance is with regard to smaller, so the above results prove the increase fluorine sulfanilamide (SN) grass with soil depth
Ether concentration is lower, and the cross direction profiles of same layer soil sample fomesafen are more uniform, and otherness is smaller.
Claims (1)
1. a kind of detection method of simulation herbicide cross direction profiles in soil layer, includes the following steps：
1）Herbicide is added into soil, obtains soil sample；
The herbicide is fomesafen；
Soil described in a concentration of 100mg/kg of herbicide described in the soil sample；
The quality moisture content of the soil sample is 10%；
2）The soil sample and the soil are loaded in the soil sample container of rainfall simulator, and the soil sample is located at institute
The upper layer of soil is stated, the rainfall simulator includes water container and the soil sample container, the water container
It is connected with the soil sample container, the pipeline being connected is equipped with control valve, the bottom of the soil sample container
Equipped with several holes A, a window is opened up on the side wall of the soil sample container；
The filling height of soil sample described in the soil sample container is 5cm；
Soil sample described in the soil sample container and the total filling height of the soil are 5cm ~ 25cm；
3）Water is added dropwise in the soil sample into the soil sample container by the water container, is passed through using sampling handle
The window takes out the sample of different location in same level at least three kinds of soil sample containers, is examined through liquid chromatogram
Measure the peak area of the sample；
The sampling handle includes a quadrangular, and a bottom surface of the quadrangular is that opening is arranged, the setting of another sealing bottom surface,
One handle is connected on the bottom surface of sealed set, the side of the quadrangular is equipped with several holes B, utilizes the handle
The quadrangular is stretched to by the window and realizes sampling in the soil sample container；
The soil sample of same level or the soil are divided by quarter using the component in right-angled intersection, then pass through institute
State the sample that sampling handle takes out every equal portions；
The rate of addition of the water is 23 ~ 25 drops/minute, and the volume often dripped is 0.08mL；
Before the liquid chromatographic detection being carried out to the sample, the step that the method includes the sample is handled as follows
Suddenly：
By the sample wetness, acetonitrile is then added and is impregnated, supernatant is obtained after oscillation and standing；Into the supernatant
Sodium chloride is added, the acetonitrile phase positioned at upper layer is obtained after oscillation and centrifugation, the acetonitrile mutually carries out the liquid chromatographic detection；
The time of the immersion is 1 hour；
The dosage of the acetonitrile is sample described in 1mL/g；
The mass ratio of the sodium chloride and the sample is 1：4；
4）The standard solution for preparing the herbicide, in step 3）Described in detect the weeding under conditions of liquid chromatographic detection
The standard solution of agent obtains the peak area of the standard solution of the herbicide, with a concentration of of the standard solution of the herbicide
Abscissa obtains the concentration of the standard solution of the herbicide using the peak area of the standard solution of the herbicide as ordinate
Standard curve between peak area；
Using the standard solution of 8 kinds of herbicides of acetontrile, the concentration of the standard solution of the herbicide is followed successively by 1mg/
Kg, 2mg/kg, 5mg/kg, 10mg/kg, 20mg/kg, 50mg/kg, 100mg/kg and 200 mg/kg；
5）According to step 3）The obtained peak area and step 4）Obtained standard curve holds appearance to get to the soil sample
The soil sample of different location or the herbicide concentration in the soil in same level in device, so far realize simulation
The detection of cross direction profiles of the herbicide in soil layer；
The condition of the liquid chromatographic detection is as follows：
Mobile phase is the mixture of acetonitrile and water, and the volume ratio of the acetonitrile and the water is 60：40；
Flow velocity is 1.0mLmin-1；
Column temperature is 30 DEG C；
Sample size is 20 μ L；
Detection wavelength is 295nm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510990258.5A CN105606729B (en) | 2014-12-26 | 2015-12-25 | A kind of detection method of simulation herbicide cross direction profiles in soil layer |
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| CN2014108243694 | 2014-12-26 | ||
| CN201410824369.4A CN104407076A (en) | 2014-12-26 | 2014-12-26 | Method for detecting soil layer distribution of herbicides |
| CN201510990258.5A CN105606729B (en) | 2014-12-26 | 2015-12-25 | A kind of detection method of simulation herbicide cross direction profiles in soil layer |
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| CN105606729B true CN105606729B (en) | 2018-07-20 |
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| CN201410824369.4A Pending CN104407076A (en) | 2014-12-26 | 2014-12-26 | Method for detecting soil layer distribution of herbicides |
| CN201510990258.5A Expired - Fee Related CN105606729B (en) | 2014-12-26 | 2015-12-25 | A kind of detection method of simulation herbicide cross direction profiles in soil layer |
| CN201510990257.0A Pending CN105606728A (en) | 2014-12-26 | 2015-12-25 | Detection method for simulating longitudinal distribution of herbicide in soil layer |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101769845A (en) * | 2010-01-19 | 2010-07-07 | 浙江大学 | Device for researching leaching migration of exogenous additional substance in soil in process of crop growth |
| CN103063712A (en) * | 2012-12-27 | 2013-04-24 | 合肥工业大学 | Layered soil moisture lysimeter sensor and installation method thereof |
| CN103308346A (en) * | 2013-07-03 | 2013-09-18 | 贵州省烟草科学研究院 | Method for researching tobacco roots and nutrient distribution of rhizosphere soil, and rhizosphere soil excavator |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7730662B2 (en) * | 2002-10-15 | 2010-06-08 | Encap, Llc. | Soil stabilizer carrier |
| JP2010100607A (en) * | 2008-09-25 | 2010-05-06 | Sumitomo Chemical Co Ltd | Method for controlling weed in place where jatropha grows |
-
2014
- 2014-12-26 CN CN201410824369.4A patent/CN104407076A/en active Pending
-
2015
- 2015-12-25 CN CN201510990258.5A patent/CN105606729B/en not_active Expired - Fee Related
- 2015-12-25 CN CN201510990257.0A patent/CN105606728A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101769845A (en) * | 2010-01-19 | 2010-07-07 | 浙江大学 | Device for researching leaching migration of exogenous additional substance in soil in process of crop growth |
| CN103063712A (en) * | 2012-12-27 | 2013-04-24 | 合肥工业大学 | Layered soil moisture lysimeter sensor and installation method thereof |
| CN103308346A (en) * | 2013-07-03 | 2013-09-18 | 贵州省烟草科学研究院 | Method for researching tobacco roots and nutrient distribution of rhizosphere soil, and rhizosphere soil excavator |
Non-Patent Citations (3)
| Title |
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| 阿特拉津在室内滴灌施药条件和农田尺度下运移的数值模拟;毛萌;《中国优秀博士学位论文全文数据库 农业科技辑》;20040915;第2004年卷(第03期);第D046-1页 * |
| 除草剂氟磺胺草醚在不同土壤中的环境行为;郭玉莲;《生态学杂志》;20140228;第33卷(第2期);第429-432页 * |
| 除草剂胺苯磺隆在土壤中的淋溶及其影响因素的研究;张瑾;《中国优秀硕士学位论文全文数据库 农业科技辑》;20040315;第2004年卷(第1期);第D046-81页 * |
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| Publication number | Publication date |
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| CN104407076A (en) | 2015-03-11 |
| CN105606728A (en) | 2016-05-25 |
| CN105606729A (en) | 2016-05-25 |
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