CN110470768A - Pyrazosulfuron in a kind of measurement water quality, Hostathion, butachlor residue amount method - Google Patents
Pyrazosulfuron in a kind of measurement water quality, Hostathion, butachlor residue amount method Download PDFInfo
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- CN110470768A CN110470768A CN201910794199.2A CN201910794199A CN110470768A CN 110470768 A CN110470768 A CN 110470768A CN 201910794199 A CN201910794199 A CN 201910794199A CN 110470768 A CN110470768 A CN 110470768A
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- G—PHYSICS
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- 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
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Abstract
The present invention provide it is a kind of measurement water quality in pyrazosulfuron, Hostathion, butachlor residue amount method, belong to water quality detection method technical field.This method comprises: first preparing sample, then standard working solution is prepared, is tested using standard working solution of the ultra performance liquid chromatography-tandem mass spectrum to step 2, using the peak area of various objects as ordinate, standard curve, quantified by external standard method are drawn by abscissa of corresponding concentration；The sample to be tested of step 1 ultra performance liquid chromatography-tandem mass spectrum is carried out at identical conditions to measure, measure the chromatographic peak area of pyrazosulfuron in sample to be tested, Hostathion, butachlor, it brings into standard curve, obtains the content of pyrazosulfuron in sample to be tested, Hostathion, butachlor.Method detection limit of the invention is 0.1 μ g/L, and quantitative limit is 0.3 μ g/L, and testing cost is low, method is accurate.
Description
Technical field
The invention belongs to water quality detection method technical fields, and in particular to pyrazosulfuron in a kind of measurement water quality, Hostathion,
The method of butachlor residue amount.
Background technique
Pyrazosulfuron (No. CAS: 98389-04-9) belongs to sulfonylurea herbicide, applicable crops: rice seedling bed, live streaming
Field, transplant field are mainly absorbed by root system, are turned rapidly in weeds plant body to absorb translocated herbicide in selectivity
It moves, inhibits growth, weeds are gradually dead.Rice can decompose the medicament, have little effect to the growth of rice, validity period 25-
35 days.Stability: 50 DEG C can stablize half a year, stablize to light.Pyrazosulfuron structural formula is as follows:
Hostathion (No. CAS: 24017-47-8) is broad-spectrum organophosphorous pesticide, acaricide, nematicide, is mainly used for preventing
Control fruit tree, cotton, lepidoptera pest, harmful mite, fly larvae and subterranean pest-insect on grain class crop etc..Sterling is light yellow liquid
Body dissolves in most of organic solvents, stablizes to light, hydrolyzes in acid, alkaline media, 140 DEG C of substances are harmful to environment, answer
Pay special attention to the pollution to water body.The structural formula of Hostathion is as follows:
Butachlor (No. CAS: 23184-66-9), Chinese nickname, weed eradication spy, Machete, selective preemergence herbicide.Indissoluble
Yu Shui is soluble in a variety of organic solvents.Chemical property is stablized under room temperature and neutrality, weak basic condition.It can add under strong acid condition
Its decomposition of speed, can be degraded in the soil.Be mainly used for live streaming or the annual gramineous weed prevented and kill off of transplanting rice field and certain
A little broadleaf weeds.It is also selective to wheat, barley, beet, cotton, peanut and Chinese cabbage crop.Effective dose is per hectare
(1.0-4.5kg effective component).Soil surface is handled before usually making bud, can also be applied after the seedling of paddy field, is herbicide for paddy field
Important species.The structural formula of butachlor is as follows:
In the prior art there are no in water quality detect pyrazosulfuron, Hostathion, butachlor residue amount method.
Summary of the invention
The object of the present invention is to provide it is a kind of measurement water quality in pyrazosulfuron, Hostathion, butachlor residue amount method, should
It is method simplicity, high sensitivity, reproducible.
The present invention provide it is a kind of measurement water quality in pyrazosulfuron, Hostathion, butachlor residue amount method, this method packet
It includes:
Step 1: sample preparation
Water sample is weighed, acetic acid acetonitrile extraction is added, adds sodium chloride and saltouts, pipettes upper organic phase, repeats extraction two
It is secondary, merge extract liquor twice, with being dried with nitrogen, methanol aqueous solution constant volume is added, filter membrane obtains sample to be tested；The water sample
Volume ratio with acetic acid acetonitrile is 2:1；The quality g of the volume mL: sodium chloride of water sample is 50:15；Water sample and methanol aqueous solution
Volume ratio is 50:1；
Step 2: the preparation of standard working solution
Standard solution: first respectively compound concentration be 100mg/L pyrazosulfuron, Hostathion, butachlor standard solution；
Standard reserving solution: take above-mentioned pyrazosulfuron, Hostathion, each 1mL of butachlor standard solution in volumetric flask, methanol is molten
Scale is solved and be settled to, standard reserving solution, concentration 10mg/L are configured to；
Hybrid standard intermediate fluid: taking each 1mL of standard reserving solution in volumetric flask, and methanol dissolves and be settled to scale, configuration
At hybrid standard intermediate fluid, concentration 1000ng/mL；
The drafting of standard curve: drawing certain volume liquid from hybrid standard intermediate fluid, be configured to 5,10,20,50,
The series standard working solution of 100ng/mL；
Step 3: measurement
It is tested using standard working solution of the ultra performance liquid chromatography-tandem mass spectrum to step 2, with various objects
Peak area be ordinate, using corresponding concentration be abscissa drafting standard curve, quantified by external standard method；
The sample to be tested of step 1 is carried out ultra performance liquid chromatography-tandem mass spectrum at identical conditions to measure, is measured
The chromatographic peak area of pyrazosulfuron, Hostathion, butachlor, brings into standard curve in sample to be tested, obtains pyrrole in sample to be tested
The content of Sulfometuron Methyl, Hostathion, butachlor；
The determination condition are as follows:
Ultra performance liquid chromatography condition
Chromatographic column: Waters BEH C18, 2.1mm × 50mm, 1.7 μm or the suitable column of performance；
Flow velocity: 0.25mL/min；
Sample volume: 10 μ L；
Column temperature: 40 DEG C；
Mobile phase: acetonitrile and 0.1% formic acid water, gradient elution, such as table 1
1 gradient elution program of table
| Time | Acetonitrile | 0.1% formic acid water |
| 0 | 5 | 95 |
| 0.5 | 5 | 95 |
| 3.0 | 100 | 0 |
| 3.1 | 5 | 95 |
| 4.0 | 5 | 95 |
Mass Spectrometry Conditions
Ion source: ESI；
Scanning mode: cation scanning；
Detection mode: multiple-reaction monitoring；
Nebulizer pressure: 50psi；
Dry gas stream speed: 12L/min；
Dry temperature degree: 350 DEG C；
Capillary voltage: 4000V；
Ion pair, orifice potential and impact energy are monitored, is shown in Table 2；
Table 2 monitors ion pair, orifice potential and impact energy
Note: * is quota ion
Preferably, the water sample is surface water.
Preferably, the volume fraction of acetic acid acetonitrile is 1% in the step 1.
Preferably, the volume fraction of methanol is 20% in the step 1.
Preferably, the temperature being dried with nitrogen is 40 DEG C.
Preferably, the filter membrane is 0.22 μm of filter membrane.
Beneficial effects of the present invention
The present invention provide pyrazosulfuron in a kind of measurement water quality, Hostathion, butachlor residue amount method, this method is sensitive
Degree is high, and the method detection limit of pyrazosulfuron, Hostathion, butachlor in this method measurement surface water is 0.1 μ g/L, quantitative limit
It is 0.3 μ g/L, testing cost is low, method is accurate.
Detailed description of the invention
Fig. 1 is pyrazosulfuron, Hostathion, butachlor standard substance total ion chromatogram in the embodiment of the present invention 1；
Fig. 2 is the ion massspectrum figure in the embodiment of the present invention 1 under the MRM mode of pyrazosulfuron standard substance；
Fig. 3 is the ion massspectrum figure in the embodiment of the present invention 1 under the MRM mode of Hostathion standard substance；
Fig. 4 is the ion massspectrum figure in the embodiment of the present invention 1 under the MRM mode of butachlor standard substance.
Specific embodiment
Further detailed description is done to the present invention combined with specific embodiments below, it should be understood that implementation of the invention is simultaneously
Do not limit to and the following examples, the accommodation in any form or change made to the present invention fall within protection of the invention
Range.
Agents useful for same in embodiment is unless otherwise indicated that analysis is pure, and water should meet second level as defined in GB/T 6682
Water.
Acetonitrile: chromatographically pure；Methanol: chromatographically pure；Sodium chloride: analysis is pure；Acetic acid: excellent pure grade；
Embodiment 1
Pyrazosulfuron in a kind of measurement water quality, Hostathion, butachlor residue amount method, this method comprises:
Step 1: sample preparation
Water sample is acquired with ground glass stoppered bottle, the sample after acquisition is saved in 4 DEG C of refrigerators, and removing in sample transportational process should prevent
Shake, avoids sunlight from irradiating at cryo-conservation, should also be prevented from transport vehicle and is contaminated.All samples acquire parallel double samples, every lot sample
Product should one full procedure blank of band and a transport blank.
It is poured into 1000mL volumetric flask with the acetic acid that graduated cylinder measures 10mL, adds acetonitrile constant volume, after mixing, pour into 1% acetic acid
In acetonitrile special-purpose bottle；
Homogeneous sample 50.00mL is pipetted with big tripe pipette to be added in 250mL separatory funnel, and 25.00mL is accurately added
1% (volume fraction) acetic acid acetonitrile is vortexed and mixes, and adds 15g sodium chloride, is vortexed and mixes, saltouts, it is organic accurately to pipette upper layer
Phase, repetition are extracted twice, and are merged extract liquor twice, are dried with nitrogen at 40 DEG C, and 1.00mL 20% (volume fraction) methanol is added
Aqueous solution constant volume crosses 0.22 μm of filter membrane, obtains sample to be tested；
Step 2: the preparation of standard working solution
Standard solution: first respectively compound concentration be 100mg/L pyrazosulfuron, Hostathion, butachlor standard solution；
Standard reserving solution: take above-mentioned pyrazosulfuron, Hostathion, each 1mL of butachlor standard solution in 10mL volumetric flask, first
Alcohol dissolves and is settled to scale, is configured to standard reserving solution, and concentration 10mg/L is protected from light storage in 4 DEG C of refrigerators；
Hybrid standard intermediate fluid: taking each 1mL of standard reserving solution in 10mL volumetric flask, and methanol dissolves and be settled to scale,
It is configured to hybrid standard intermediate fluid, concentration 1000ng/mL is protected from light storage in 4 DEG C of refrigerators；
The drafting of standard curve: drawing certain volume liquid from hybrid standard intermediate fluid, be configured to 5,10,20,50,
The series standard working solution of 100ng/mL；
Step 3: measurement
It is tested using standard working solution of the ultra performance liquid chromatography-tandem mass spectrum to step 2, obtains standard work
Pyrazosulfuron, Hostathion, butachlor standard substance total ion chromatogram and pyrazosulfuron, Hostathion, butachlor standard in liquid
Ion massspectrum figure under the MRM mode of substance, as shown in Figs 1-4, using the peak area of various objects as ordinate, with corresponding
Concentration is that abscissa draws standard curve, calibration curve equation such as table 3, quantified by external standard method；
Table 3
| Title | Regression equation | Related coefficient |
| Pyrazosulfuron | Y=5623.45x-3725.46 | 0.9996 |
| Hostathion | Y=928.46x-6901.74 | 0.9997 |
| Butachlor | Y=579.63x-783.22 | 0.9997 |
Method detection limit is 0.1 μ g/L, and quantitative limit is 0.3 μ g/L；
The sample to be tested of step 1 is carried out ultra performance liquid chromatography-tandem mass spectrum at identical conditions to measure, is measured
The chromatographic peak area of pyrazosulfuron, Hostathion, butachlor, brings into linear equations in sample to be tested, obtains pyrrole in sample to be tested
The content of Sulfometuron Methyl, Hostathion, butachlor；
Quantified by external standard method calculates the content of object in sample as follows:
In formula:
X --- the content of determinand in sample, unit are micro- gram per liter (μ g/L)；
C --- testing concentration in sample solution derived from standard operating curves, unit are nanograms per milliliter (ng/
mL)；
V --- constant volume, unit are milliliter (mL)；
V0--- claim sample volume, unit is milliliter (mL)；
F --- extension rate；(f=1)
The determination condition are as follows:
Ultra performance liquid chromatography condition
Chromatographic column: Waters BEH C18, 2.1mm × 50mm, 1.7 μm or the suitable column of performance；
Flow velocity: 0.25mL/min；
Sample volume: 10 μ L；
Column temperature: 40 DEG C；
Mobile phase: acetonitrile and 0.1% formic acid water, gradient elution, such as table 2；
2 gradient elution program of table
Mass Spectrometry Conditions
Ion source: ESI；
Scanning mode: cation scanning；
Detection mode: multiple-reaction monitoring；
Nebulizer pressure: 50psi；
Dry gas stream speed: 12L/min；
Dry temperature degree: 350 DEG C；
Capillary voltage: 4000V；
Ion pair, orifice potential and impact energy are monitored, is shown in Table 3；
Table 3 monitors ion pair, orifice potential and impact energy
Note: * is quota ion
The surface water for taking 5 different places is respectively labeled as surface water No. 1, No. 2, No. 3, No. 4 and No. 5, according to above-mentioned reality
The method for applying example 1 is measured, each sample METHOD FOR CONTINUOUS DETERMINATION 5 times, takes the average value (unit μ g/L) of 5 measurements, as a result such as table 4
It is shown:
Table 4
| No. 1 | No. 2 | No. 2 | No. 4 | No. 5 | |
| Pyrazosulfuron | 20.59 | 20.6 | 20.63 | 20.61 | 20.62 |
| Hostathion | 18.45 | 18.47 | 18.44 | 18.46 | 18.45 |
| Butachlor | 19.20 | 19.22 | 19.23 | 19.21 | 19.23 |
It is above that certain exemplary embodiments of the invention are only described by way of explanation, undoubtedly, for ability
The those of ordinary skill in domain without departing from the spirit and scope of the present invention can be with a variety of different modes to institute
The embodiment of description is modified.Therefore, above-mentioned attached drawing and description are regarded as illustrative in nature, and should not be construed as to the present invention
The limitation of claims.
Claims (6)
1. it is a kind of measurement water quality in pyrazosulfuron, Hostathion, butachlor residue amount method, which is characterized in that this method comprises:
Step 1: sample preparation
Water sample is weighed, acetic acid acetonitrile extraction is added, adds sodium chloride and saltouts, pipettes upper organic phase, repetition is extracted twice, and is closed
And methanol aqueous solution constant volume is added with being dried with nitrogen in extract liquor twice, filter membrane obtains sample to be tested；The water sample and acetic acid
The volume ratio of acetonitrile is 2:1；The quality g of the volume mL: sodium chloride of water sample is 50:15；The volume ratio of water sample and methanol aqueous solution
For 50:1；
Step 2: the preparation of standard working solution
Standard solution: first respectively compound concentration be 100mg/L pyrazosulfuron, Hostathion, butachlor standard solution；
Standard reserving solution: taking above-mentioned pyrazosulfuron, Hostathion, each 1mL of butachlor standard solution in volumetric flask, and methanol dissolves simultaneously
It is settled to scale, is configured to standard reserving solution, concentration 10mg/L；
Hybrid standard intermediate fluid: taking each 1mL of standard reserving solution in volumetric flask, and methanol dissolves and be settled to scale, is configured to mix
Standardization intermediate fluid, concentration 1000ng/mL；
The drafting of standard curve: certain volume liquid is drawn from hybrid standard intermediate fluid, is configured to 5,10,20,50,100ng/
The series standard working solution of mL；
Step 3: measurement
It is tested using standard working solution of the ultra performance liquid chromatography-tandem mass spectrum to step 2, with the peak of various objects
Area is ordinate, draws standard curve, quantified by external standard method by abscissa of corresponding concentration；
The sample to be tested of step 1 is carried out ultra performance liquid chromatography-tandem mass spectrum at identical conditions to measure, is measured to be measured
The chromatographic peak area of pyrazosulfuron, Hostathion, butachlor, brings into standard curve in sample, obtains the phonetic sulphur of pyrrole in sample to be tested
The content of grand, Hostathion, butachlor；
The determination condition are as follows:
Ultra performance liquid chromatography condition
Chromatographic column: Waters BEH C18, 2.1mm × 50mm, 1.7 μm or the suitable column of performance；
Flow velocity: 0.25mL/min；
Sample volume: 10 μ L；
Column temperature: 40 DEG C；
Mobile phase: acetonitrile and 0.1% formic acid water, gradient elution, such as table 1
Table 1
Mass Spectrometry Conditions:
Ion source: ESI；
Scanning mode: cation scanning；
Detection mode: multiple-reaction monitoring；
Nebulizer pressure: 50psi；
Dry gas stream speed: 12L/min；
Dry temperature degree: 350 DEG C；
Capillary voltage: 4000V；
Ion pair, orifice potential and impact energy are monitored, is shown in Table 2；
Table 2
2. it is according to claim 1 it is a kind of measurement water quality in pyrazosulfuron, Hostathion, butachlor residue amount method,
It is characterized in that, the water sample is surface water.
3. it is according to claim 1 it is a kind of measurement water quality in pyrazosulfuron, Hostathion, butachlor residue amount method,
It is characterized in that, the volume fraction of acetic acid acetonitrile is 1% in the step 1.
4. it is according to claim 1 it is a kind of measurement water quality in pyrazosulfuron, Hostathion, butachlor residue amount method,
It is characterized in that, the volume fraction of methanol is 20% in the step 1.
5. it is according to claim 1 it is a kind of measurement water quality in pyrazosulfuron, Hostathion, butachlor residue amount method,
It is characterized in that, the temperature being dried with nitrogen is 40 DEG C.
6. it is according to claim 1 it is a kind of measurement water quality in pyrazosulfuron, Hostathion, butachlor residue amount method,
It is characterized in that, the filter membrane is 0.22 μm of filter membrane.
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Cited By (2)
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| CN113960196A (en) * | 2021-10-11 | 2022-01-21 | 太湖流域水文水资源监测中心（太湖流域水环境监测中心） | Method for on-line determination of sulfonylurea herbicide in water |
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