CN101832979A - Determination method of residual quantity of diuron and metabolin thereof in cottonseeds - Google Patents
Determination method of residual quantity of diuron and metabolin thereof in cottonseeds Download PDFInfo
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- CN101832979A CN101832979A CN200910228931A CN200910228931A CN101832979A CN 101832979 A CN101832979 A CN 101832979A CN 200910228931 A CN200910228931 A CN 200910228931A CN 200910228931 A CN200910228931 A CN 200910228931A CN 101832979 A CN101832979 A CN 101832979A
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Abstract
The invention relates to a determination method of the residual quantity of diuron and metabolin thereof in cottonseeds. The method comprises the following steps: weighing 20.0g of samples to be placed in 200mL of HCl solution of 10 percent, adding few glass beads for preventing sudden boiling, adding 250mL of cooled NaOH solution of 40 percent, then adding antifoamer, and mixing well; then adding 2g of Zn and 5mL of TiCl3, and carrying out heating reflux reaction for 2-4 hours; distilling, stratifying collected liquid, collecting a water layer and getting rid of an upper layer; dripping 2 drops of phenolphthalein indicator to the water layer, dripping the NaOH solution of 40 percent under stirring until the solution turns pink and does not return to the achromatic color within 1min, then dripping two drops of the NaOH solution, and cooling for 15-20min; extracting with 50mL of normal hexane for twice, shaking for 2min in each extraction, standing for 10min, collecting an organic phase of the upper layer, utilizing anhydrous sodium sulfate to carrying out dehydration on the organic phase, filtering, decompressing and concentrating to be almost dry in water bath at 30DEG C, blowing dry by utilizing nitrogen, fixing volume, and detecting by adopting GC-NPD. The diuron and the metabolin thereof are determined by gas chromatography after being fully converted into 3, 4-DCA, and the method can accurately determine the residual quantity of the diuron and the metabolin thereof and can meet the requirements of pesticide residue detection.
Description
Technical field:
The invention belongs to the determination techniques field of persticide residue in the plant, relate to diuron and metabolic product determination of residual amount method thereof in the cottonseed.
Background technology:
Herbicide (herbicide) is meant and can makes weeds that withered medicament takes place up hill and dale or selectively.Sodium chlorate, borax, arsenate, trichloroacetic acid all have withered effect for the plant of any kind of, but because these all have residual influence, so can not be applied in the field.Diuron is the phenyl substituted urea compounds, and chemical name is: N-(3, the 4-dichlorophenyl)-N ', N '-dimethyl urea.Belong to the internal-suction type herbicide, can suppress the crop photosynthesis effect, be used to prevent and kill off the general weeds in noncrop area.Be mainly used in cotton, corn, jowar, sugarcane, paddy rice, tea place, orchard, vineyard and bare place.Its assay method has liquid phase process, gas phase process etc.Application number: 200710022396 disclose a kind of method of removing herbicide Dailon in the water, and it is to adopt medium blocking-discharge method that the water that contains herbicide Dailon is handled, and the diuron in the water body is degraded; With contaminant degradation is carbon dioxide, water and simple organic, the reaction conditions gentleness, and controllability is stronger, reactor apparatus and operate fairly simple.Other relevant diuron and metabolin residue detection analyses in cottonseed thereof, the present domestic open report of not seeing.
Summary of the invention:
In order to estimate the security after diuron and metabolin thereof use in cotton, the invention discloses use gas chromatography-nitrogen phosphorous detector (GC-NPD) method and measure the method for diuron in the cottonseed and metabolic product residual quantity thereof, diuron and the whole hydrolysis of metabolin thereof are converted into 3, and 4-DCA measures.Use gas chromatography-nitrogen phosphorous detector (GC-NPD) method to measure at last.For achieving the above object, the invention provides following technical scheme:
The assay method of diuron and metabolic product residual quantity thereof in the cottonseed is characterized in that being undertaken by following step:
(1) hydrolysis reaction:
1) takes by weighing the 20.0g sample and place 30mL33%HCl solution;
2) add the anti-bumping of a small amount of beaded glass, add the NaOH solution of 250mL40% cooling, add the 20mL antifoam, mix; Add 2-5g Zn and 5-7mL TiCl again
3, heating reflux reaction 2 hours; Liquid is collected in distillation, and reactant liquor is put in the refrigerator and cooled Tibetan;
(2) extractive reaction:
1) liquid of collecting is changed in the separating funnel, survey its pH value, survey its pH value.With 20-40mL normal hexane washing receiving bottle, change over to after washing in the above-mentioned separating funnel, jolting 2-5min collects lower aqueous layer.Discard the upper strata.
2) drip 2 phenolphthalein indicators to the lower floor aqueous phase, stir and drip 40%NaOH solution down, become pink and in 1min, do not become again colourlessly to solution, add 2 NaOH solution again, cooling 15-20min;
3) with normal hexane 50mL * 2 extractions, extract jolting 2-5min at every turn, leave standstill 10-15min, collect upper organic phase through anhydrous sodium sulfate dehydration, filter, concentrating under reduced pressure is closely dried under 30 ℃ of water-baths, nitrogen dries up, and constant volume adopts gas chromatography-nitrogen phosphorous detector to detect.
Assay method of the present invention, antifoam wherein are dimethyl silicon oil.
Assay method of the present invention, wherein said sample comprises: the mensuration of residual quantities such as cotton, cottonseed, corn, jowar, sugarcane, paddy rice or grape.
Diuron of the present invention (Diuron) 3-(3,4-dichlorophenyl)-1,1-dimethylurea and can be converted into 3, the metabolin of 4-dichloroaniline.Chemical name N-3,4-dichlorophenyl-N ', N '-dimethyl urea are inner sucting conduction type spectrum herbicide.It is as follows that the present invention measures the concrete grammar of diuron in the cottonseed and metabolic product residual quantity thereof:
1 test material
1.1 instrument and reagent
Instrument: PE AutoSystem XL gas chromatograph (band nitrogen phosphorous detector)
Chromatographic column: DB-1 (30m * 0.25mm * 0.25 μ m)
Reagent: HCl (analyzing pure), NaOH (analyzing pure), normal hexane (chromatographically pure), anhydrous sodium sulfate (analyzing pure), phenolphthalein indicator (1g phenolphthalein is dissolved in the 100mL ethanol), dimethyl silicon oil, Zn, TiCl3,
Standard model: diuron (99.6%), 3,4-DCA (99.0%), diuron metabolin DCPU (99.5%), DCPMU (99.0%) reaction unit Fig. 1.
1.2 chromatographic condition
Injector temperature: 250 ℃;
Detector temperature: 250 ℃;
Column temperature: 80 ℃ keep 1min, 20 ℃/min to 250 ℃ maintenance 3min;
Carrier gas: N2 (〉=99.999%);
Flow velocity: 2.0mL/min;
Hydrogen flow rate: 2.0mL/min;
Air velocity: 100mL/min;
Replenish gas: 30mL/min;
Sample size: 2 μ L.
1.3 standard solution preparation
Accurately take by weighing diuron, DCPU, DCPMU, 3, each 10.0mg of 4-DCA, acetone is settled to quarter in the 50mL volumetric flask.
2 specimen preparations
2.1 hydrolysis reaction
1) preparation 30mL HCL solution: 10mL concentrated hydrochloric acid+20mL distilled water is positioned in the 300mL receiving flask (triangular flask).Take by weighing the 20.0g sample and place 1L reaction bulb (ground round-bottomed flask).
2) add the anti-bumping of a small amount of beaded glass, add the NaOH solution of 250mL40% cooling, mix.Add 20mL dimethyl silicon oil (antifoam), mix.Adding 2g Zn and 5mL TiCL3 will reflux rapidly after adding and distilling apparatus connects, and the distillation valve cuts out, and connects the receiving flask in 1.Condenser pipe leads to tap water.(annotate: if having oily or indissoluble thing can add the 75mL normal hexane.)
3) heating, controlling liquid condensation from reflux condensing tube spherical pipe bottom, back flow reaction 2 hours, timing is from beginning backflow.
4) backflow was opened the distillation valve after 2 hours, improved heating-up temperature slightly and distilled, and collected 120mL liquid.
5) receiving flask is positioned in the cold storage refrigerator.
2.2 extractive reaction
1) distillation fraction with cooling changes in the separating funnel, surveys its pH value.With 25mL normal hexane washing receiving bottle, change over to after washing in the above-mentioned separating funnel, jolting 2min collects lower aqueous layer.Discard the upper strata.
2) drip 2 phenolphthalein indicators to the lower floor aqueous phase, stir and drip 40%NaOH solution down, become pink and in 1min, do not become again colourlessly to solution, add 2 NaOH solution again.Cooling 15min.
3) use normal hexane 50mL, the 50mL extraction extracts jolting 2min at every turn, leaves standstill 10min, collects upper organic phase through anhydrous sodium sulfate dehydration.Filter, and wash anhydrous sodium sulfate with normal hexane.Merge.Concentrating under reduced pressure is closely dried under 30 ℃ of water-baths, and nitrogen dries up.Constant volume, GC detects.
3, the detection limit of method
Diuron and metabolin DCPU, DPCMU are added in the operation of application said method respectively in cottonseed, interpolation concentration is 0.05mg/kg.3 times of signal to noise ratio (S/N ratio) S/N are set at the instrument detection limit with instrument, and then method concentration limit (mg/kg)=instrument detection limit (ng) * dilutes volume (mL)/[sampling volume (ul) * sampling amount (g).The method of calculating detects and is limited to 0.05mg/kg at last.
4, the recovery and precision experiment
In blank cottonseed, add diuron and metabolin DCPU thereof, DCPMU standard solution, extract as stated above, purify and measure.The recovery sees Table 1.Test shows that the recovery meets agricultural residual detection requirement, has proved that this method has the recovery and repeatability preferably.
Table 1 diuron and metabolic product thereof add recovery test
The good effect that the concrete grammar of diuron and metabolic product residual quantity thereof is compared with prior art had in the mensuration cottonseed disclosed by the invention is:
Diuron and metabolite residue amount thereof in the traditional technique in measuring cottonseed, it is strong disturbed by impurity, and 3, the 4-dichloroaniline (3,4-DCA) stable and easily detection.Therefore, diuron and metabolin thereof all are converted into 3, measure with the gas spectrum behind the 4-DCA, can accurately record the residual quantity of diuron and metabolin thereof.The present invention utilizes gas chromatography to analyze diuron and metabolic product thereof, favorable reproducibility, and impurity disturbs few, and accuracy is good, and the precision height can satisfy the needs of Detecting Pesticide.
Fig. 1 reaction unit figure;
Fig. 2 .3,4-DCA standard specimen figure;
Fig. 3 cottonseed adds figure;
Fig. 4 cottonseed blank sheet.
Embodiment:
In order to explain implementation method of the present invention more fully, provide the preparation embodiment of diuron in the cottonseed and metabolic product determination of residual amount method thereof.These embodiments only are to explain rather than limit the scope of the invention.Wherein used raw material all has commercially available.
1) takes by weighing the 20.0g cottonseed and place 30mL 33%HCl solution;
2) add the anti-bumping of a small amount of beaded glass, add 250mL, the NaOH solution of 40% cooling adds the antifoam dimethyl silicon oil, mixes; Add 3g Zn and 5mL TiCl again
3, heating reflux reaction 2 hours; Liquid is collected in distillation, and reactant liquor is put in the refrigerator and cooled Tibetan;
3) liquid of collecting is changed in the separating funnel, survey its pH value, survey its pH value.With 20mL normal hexane washing receiving bottle, change over to after washing in the above-mentioned separating funnel, jolting 3min collects lower aqueous layer.Discard the upper strata
4) drip 2 phenolphthalein indicators to the lower floor aqueous phase, stir and drip 40%NaOH solution down, become pink and in 1min, do not become again colourlessly to solution, add 2 NaOH solution again, cooling 15min;
5) with normal hexane 50mL * 2 extractions, extract jolting 2min at every turn, leave standstill 10min, collect upper organic phase through anhydrous sodium sulfate dehydration, filter, concentrating under reduced pressure is closely dried under 30 ℃ of water-baths, and nitrogen dries up, and constant volume adopts gas chromatography-nitrogen phosphorous detector to detect.
1) takes by weighing the 10.0g corn and place 30mL 33%HCl solution;
2) add the anti-bumping of a small amount of beaded glass, add 250mL, the NaOH solution of 40% cooling adds the antifoam dimethyl silicon oil, mixes; Add 3g Zn and 6mL TiCl again
3, heating reflux reaction 2 hours; Liquid is collected in distillation, and reactant liquor is put in the refrigerator and cooled Tibetan;
3) liquid of collecting is changed in the separating funnel, survey its pH value, survey its pH value.With 40mL normal hexane washing receiving bottle, change over to after washing in the above-mentioned separating funnel, jolting 3min collects lower aqueous layer.Discard the upper strata
4) drip 2 phenolphthalein indicators to the lower floor aqueous phase, stir and drip 40%NaOH solution down, become pink and in 1min, do not become again colourlessly to solution, add 2 NaOH solution again, cooling 15min;
5) with normal hexane 50mL * 2 extractions, extract jolting 2min at every turn, leave standstill 10min, collect upper organic phase through anhydrous sodium sulfate dehydration, filter, concentrating under reduced pressure is closely dried under 30 ℃ of water-baths, and nitrogen dries up, and constant volume adopts gas chromatography-nitrogen phosphorous detector to detect.
1) takes by weighing the 20.0g Chinese sorghum and place 30mL33%HCl solution;
2) add the anti-bumping of a small amount of beaded glass, add the NaOH solution of 250mL40% cooling, add the 20mL antifoam, mix; Add 3g Zn and 6mL TiCl again
3, heating reflux reaction 2 hours; Liquid is collected in distillation, and reactant liquor is put in the refrigerator and cooled Tibetan;
3) liquid of collecting is changed in the separating funnel, survey its pH value, survey its pH value.With 30mL normal hexane washing receiving bottle, change over to after washing in the above-mentioned separating funnel, jolting 3min collects lower aqueous layer.Discard the upper strata.
4) drip 2 phenolphthalein indicators to the lower floor aqueous phase, stir and drip 40%NaOH solution down, become pink and in 1min, do not become again colourlessly to solution, add 2 NaOH solution again, cooling 15-20min;
5) with normal hexane 50mL * 2 extractions, extract jolting 3min at every turn, leave standstill 12min, collect upper organic phase through anhydrous sodium sulfate dehydration, filter, concentrating under reduced pressure is closely dried under 30 ℃ of water-baths, and nitrogen dries up, and constant volume adopts gas chromatography-nitrogen phosphorous detector to detect.
After the preferred embodiment that describes in detail, being familiar with this technology personage can be well understood to, can carry out various variations and modification not breaking away under above-mentioned claim and the spirit, all foundations technical spirit of the present invention is done any simple modification, equivalent variations and modification to above embodiment, all belongs to the scope of technical solution of the present invention.And the present invention also is not subjected to the restriction of the embodiment that gives an actual example in the instructions.
Claims (4)
1. the assay method of diuron and metabolic product residual quantity thereof in the cottonseed is characterized in that being undertaken by following step:
(1) hydrolysis reaction:
1) takes by weighing the 20.0g sample and place 30mL33%HCl solution;
2) add the anti-bumping of a small amount of beaded glass, add the NaOH solution of 250mL40% cooling, add the 20mL antifoam, mix; Add 2-5g Zn and 5-7mL TiCl again
3, heating reflux reaction 2 hours; Liquid is collected in distillation, and reactant liquor is put in the refrigerator and cooled Tibetan;
(2) extractive reaction:
1) liquid of collecting is changed in the separating funnel, survey its pH value, survey its pH value.With 20-40mL normal hexane washing receiving bottle, change over to after washing in the above-mentioned separating funnel, jolting 2-5min collects lower aqueous layer.Discard the upper strata.
2) drip 2 phenolphthalein indicators to the lower floor aqueous phase, stir and drip 40%NaOH solution down, become pink and in 1min, do not become again colourlessly to solution, add 2 NaOH solution again, cooling 15-20min;
3) with normal hexane 50mL * 2 extractions, extract jolting 2-5min at every turn, leave standstill 10-15min, collect upper organic phase through anhydrous sodium sulfate dehydration, filter, concentrating under reduced pressure is closely dried under 30 ℃ of water-baths, nitrogen dries up, and constant volume adopts gas chromatography-nitrogen phosphorous detector to detect.
2. the described assay method of claim 1, antifoam wherein is a dimethyl silicon oil.
3. the described assay method of claim 1 is during the reactant hydrolysis, if having oily or indissoluble thing can add the 75mL normal hexane.
4. the described assay method of claim 1, wherein said sample comprises: the mensuration of residual quantities such as cotton, cottonseed, corn, jowar, sugarcane, paddy rice or grape.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108828101A (en) * | 2018-08-08 | 2018-11-16 | 广西科技师范学院 | The remaining method of diuron in measurement sugarcane based on 3,4- dichloroaniline |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108828101A (en) * | 2018-08-08 | 2018-11-16 | 广西科技师范学院 | The remaining method of diuron in measurement sugarcane based on 3,4- dichloroaniline |
| CN108828101B (en) * | 2018-08-08 | 2021-05-07 | 广西科技师范学院 | Method for determining diuron residues in sugarcane based on 3, 4-dichloroaniline |
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Application publication date: 20100915 |