CN103630643A - Determination method for fipronil residue content in soil environment - Google Patents
Determination method for fipronil residue content in soil environment Download PDFInfo
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- CN103630643A CN103630643A CN201210310130.6A CN201210310130A CN103630643A CN 103630643 A CN103630643 A CN 103630643A CN 201210310130 A CN201210310130 A CN 201210310130A CN 103630643 A CN103630643 A CN 103630643A
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Abstract
The invention relates to a determination method for fipronil residue content in a soil environment. According to the present invention, the determination method adopts a gas chromatograph to perform detection, and the method for detecting fipronil residue content in the soil environment by using the gas chromatograph has characteristics of accuracy, rapidness and high sensitivity, wherein the relative standard deviation is less than 10%, the standard addition recovery rate of the sample is 92.0-100.0%, and requirements of detection works and researches of people can be met.
Description
Technical field
The present invention relates to the detection method of ethiprole in a kind of soil environment, particularly relate to a kind of by gas chromatograph to ethiprole residual content detection method in soil environment.
Background technology
[0002] sterling is white solid, 200 ~ 201 ℃ of fusing points, density 1.477 ~ 1.626(20 ℃); Partition factor (25 ℃) logP=4.0.Solubleness in water (20 ℃, mg/L) 1.9(distilled water), 1.9(PH=5), 2.4(PH=9); Solubleness in other solvent (20 ℃, g/L): acetone 545.9, methylene chloride 22.3, toluene 3.0, hexane <0.028.Stable in PH=5,7 water, when PH=9, be slowly hydrolyzed, slow degradation under solar irradiation, but rapid decomposable through illumination in aqueous solution; Ethiprole is that a kind of Phenylpyrazole insecticides, insecticidal spectrum are wide, and insect be take to stomach poison function as main, have concurrently to tag and certain systemic action, to crop without poisoning.This medicament can impose on soil, also can foliar spray.By numerous agricultural chemicals experts, be recommended as one of first-selected kind replacing high malicious organophosphorus pesticide; Ethiprole is being brought into play extremely important effect in agricultural production as pesticide, but along with the increase of actual use amount, the research of people's adsorptive power in soil to it is pay attention to day by day also.Carried out at present the research of ethiprole aspect residual in soil.The present invention detects the ethiprole residual content in environment with gas chromatograph, and method is simple to operate, has higher accuracy and precision, and actual application value is larger.
Summary of the invention
The object of the invention is to utilize gas chromatograph to detect the residual content of ethiprole in soil environment.For achieving the above object, the present invention takes following design proposal:
Main Analysis step:
1, the optimization of instrument condition: by test, chromatographic apparatus condition is as follows:
Chromatographic column: DB – 1,30.0 μ m * 3, m * 320 μ m
Injector temperature: 250 ℃
Sample introduction pattern: shunting, split ratio 10:1
Sampling volume: 1 μ L
Column temperature: 80 ℃ keep 1.0 min, rise to 200 ℃ with 40 ℃/min speed, keep 12 min, then rise to 240 ℃ with 10 ℃/min speed, keep 12 min
Carrier gas: carrier gas (N2 >=99.999%) 3 mL/min
Make-up gas (N2 >=99.999%) 30 mL/min
ECD detector temperature: 300 ℃
2, the making of typical curve
Configure the standard operation liquid of a series of ethiproles, concentration is followed successively by 0.0,0.2, and 0.4,0.8,1.6mg/L, is adjusted to above-mentioned chromatographic condition by gas chromatograph, and standard series working fluid is carried out to gas chromatograph analysis, measure its peak area, then with concentration of standard solution to peak area production standard curve, obtain regression equation and related coefficient, ethiprole standard spectrogram is shown in appendix;
3, sample determination
The pre-treatment of 3.1 samples
Pedotheque: claim air-dry pedotheque (to cross 60 mesh sieves, fully mix) 50g, put into iodine flask, add respectively 100mL acetonitrile, add again 20 g anhydrous sodium sulfates, be placed in ultrasonic extraction instrument and extract after 10 min standingly, get centrifugal 5 min of supernatant (3000 r/min); Get the centrifugal rear clarified solution of 50 mL and put into the separating funnel that fills 100 mL 6% aqueous sodium persulfate solutions, extract 3 times respectively with 30 mL, 15 mL and 15 mL ethyl acetate, get ethyl acetate and cross mutually after anhydrous sodium sulfate, the concentrated 2mL that is closely settled to, measures for GC;
The mensuration of 3.2 samples
Under the instrument condition of optimizing, the sample preparing is analyzed;
4 results are calculated
The content of ethiprole in calculation sample as follows:
C sample=C0*V0 * V extract/V clarified solution/M sample
C sample: the concentration of ethiprole in pedotheque, mg/kg, C0: the concentration of ethiprole in constant volume solution (looking into typical curve according to the peak area of measuring obtains) mg/L, V0: the sample volume after concentrated constant volume, mL, V extract: extract volume, mL, V clarified solution: clarified solution volume, mL, M sample: sampling amount, g;
accompanying drawing explanation
Fig. 1 is the ethiprole chromatogram that the embodiment of the present invention detects, and the ordinate in this chromatogram represents peak intensity, and horizontal ordinate represents retention time, and unit is minute.
Embodiment
The mensuration of embodiment Fluorine in Soils worm nitrile residual quantity
(1) configure the standard operation liquid of a series of ethiproles, concentration is followed successively by 0.0,0.2,0.4,0.8,1.6mg/L,, the service condition of gas chromatography instrument is as follows:
Chromatographic column: DB – 1,30.0 μ m * 3, m * 320 μ m;
Injector temperature: 250 ℃
Sample introduction pattern: shunting, split ratio 10:1
Sampling volume: 1 μ L
Column temperature: 80 ℃ keep 1.0 min, rise to 200 ℃ with 40 ℃/min speed, keep 12 min, then rise to 240 ℃ with 10 ℃/min speed, keep 12 min
Carrier gas: carrier gas (N2 >=99.999%) 3 mL/min
Make-up gas (N2 >=99.999%) 30 mL/min
ECD detector temperature: 300 ℃
Standard series is analyzed, and the equation that records ethiprole typical curve is Y=10127X+1351, linearly dependent coefficient R
2=0.999.
(2) pedotheque: claim air-dry pedotheque (to cross 60 mesh sieves, fully mix) 50g, put into iodine flask, add respectively 100mL acetonitrile, add again 20 g anhydrous sodium sulfates, be placed in ultrasonic extraction instrument and extract after 10 min standingly, get centrifugal 5 min of supernatant (3000 r/min); Get the centrifugal rear clarified solution of 50 mL and put into the separating funnel that fills 100 mL 6% aqueous sodium persulfate solutions, with 30 mL, 15 mL and 15 mL ethyl acetate, extract 3 times respectively, get ethyl acetate and cross mutually after anhydrous sodium sulfate, the concentrated 2mL that is closely settled to, sample 1 μ L, carry out gas chromatograph analysis;
(3) mensuration of method precision and accuracy
With identical processing mode, prepare six Duplicate Samples, and six parallel sample are carried out to gas chromatograph analysis calculation sample content, analysis result is in Table 1-1, and from table 1-1, the relative standard deviation of Duplicate Samples (RSD) is 7.0%;
Ethiprole concentration repeatability measurement result table in table 1-1 pedotheque
For the further accuracy of checking the method, get above-mentioned six parallel sample and carry out the test of 0.015mg/kg recovery of standard addition, according to addition and measured result, the recovery of standard addition of calculation sample, the results are shown in Table 1-2, from table 1-2, the recovery of standard addition of sample is between 92.0%-100.0%;
Ethiprole recovery of standard addition measurement result table in table 1-2 pedotheque
Obviously, those skilled in the art, can detect the residual quantity of ethiprole in environmental sample by vapor-phase chromatography of the present invention;
Above-described embodiment is used for illustrative purposes only; and be not limitation of the present invention; the those of ordinary skill in relevant technologies field; without departing from the present invention; can also make various variations and modification; therefore all technical schemes that are equal to also should belong to category of the present invention, and scope of patent protection of the present invention should be limited by each claim.
Claims (5)
1. the assay method of ethiprole residual content in soil environment, is characterized in that, described assay method comprises the steps:
(1) drafting of typical curve: the standard operation liquid that configures a series of ethiproles, concentration is followed successively by 0.0,0.2,0.4,0.8,1.6mg/L, standard series working fluid is carried out to gas chromatograph analysis, measure its peak area, then with concentration of standard solution to peak area production standard curve, obtain regression equation and related coefficient; During detection, GC conditions is as follows:
Chromatographic column: DB – 1,30.0 μ m * 3, m * 320 μ m
Injector temperature: 250 ℃
Sample introduction pattern: shunting, split ratio 10:1
Sampling volume: 1 μ L
Column temperature: 80 ℃ keep 1.0 min, rise to 200 ℃ with 40 ℃/min speed, keep 12 min, then rise to 240 ℃ with 10 ℃/min speed, keep 12 min
Carrier gas: carrier gas (N2 >=99.999%) 3 mL/min
Make-up gas (N2 >=99.999%) 30 mL/min
ECD detector temperature: 300 ℃
(2) sample preparation: pedotheque: claim air-dry pedotheque (to cross 60 mesh sieves, fully mix) 50g, put into iodine flask, add respectively 100mL acetonitrile, add again 20 g anhydrous sodium sulfates, be placed in ultrasonic extraction instrument and extract after 10 min standingly, get centrifugal 5 min of supernatant (3000 r/min); Get the centrifugal rear clarified solution of 50 mL and put into the separating funnel that fills 100 mL 6% aqueous sodium persulfate solutions, extract 3 times respectively with 30 mL, 15 mL and 15 mL ethyl acetate, get ethyl acetate and cross mutually after anhydrous sodium sulfate, the concentrated 2mL that is closely settled to, measures for GC; Do blank test simultaneously;
(3) mensuration of sample: under the instrument condition of optimization, the sample preparing is analyzed;
(4) result is calculated: the content of ethiprole in calculation sample as follows:
C
sample=C
0* V
0* V
extract/ V
clarified solution/ M
sample
C
sample: the concentration of ethiprole in pedotheque, mg/kg, C
0: the concentration of ethiprole in constant volume solution (looking into typical curve according to the peak area of measuring obtains) mg/L, V
0: the sample volume after concentrated constant volume, mL, V
extract: extract volume, mL, V
clarified solution: clarified solution volume, mL, M
sample: sampling amount, g.
2. the assay method of ethiprole residual content in soil environment according to claim 1, is characterized in that: the solvent of employing and reagent are acetonitrile, ethyl acetate, 6% aqueous sodium persulfate solution and anhydrous sodium sulfate.
3. the assay method of ethiprole residual content in soil environment according to claim 1, is characterized in that: in ultrasonic extraction instrument, extract 10 min, centrifugal 5 min of supernatant (3000 r/min), purify, extract again the concentrated 2mL that is closely settled to.
4. the assay method of ethiprole residual content in soil environment according to claim 1, is characterized in that: utilize gas chromatograph to measure ethiprole.
5. the assay method of ethiprole residual content in soil environment according to claim 1, is characterized in that: with ECD detecting device, detect, qualitative according to retention time, external standard peak area method is quantitative.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105738512A (en) * | 2016-02-23 | 2016-07-06 | 黑龙江八一农垦大学 | Pretreatment method for detecting butachlor and fipronil in liquid milk |
| CN105823835A (en) * | 2016-03-11 | 2016-08-03 | 山东省农业科学院农业质量标准与检测技术研究所 | GC-MS-MS determination method for determining residual quantity of flufiprole in vegetables |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001036067A1 (en) * | 1999-11-12 | 2001-05-25 | Aventis Cropscience S.A. | Multiple sorbent cartridges for solid phase extraction |
| CN101156584A (en) * | 2007-11-02 | 2008-04-09 | 江苏东宝农药化工有限公司 | Synergistic pesticide composition containing fipronil and hexaflumuron and preparation method thereof |
-
2012
- 2012-08-28 CN CN201210310130.6A patent/CN103630643A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001036067A1 (en) * | 1999-11-12 | 2001-05-25 | Aventis Cropscience S.A. | Multiple sorbent cartridges for solid phase extraction |
| CN101156584A (en) * | 2007-11-02 | 2008-04-09 | 江苏东宝农药化工有限公司 | Synergistic pesticide composition containing fipronil and hexaflumuron and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 何艺兵: "氟虫腈在甘蓝和土壤中的残留分析方法", 《农药科学与管理》, vol. 21, no. 3, 31 March 2000 (2000-03-31), pages 17 - 19 * |
| 操海群 等: "氟虫腈在番茄和土壤中残留分析方法的研究", 《安徽农业大学学报》, vol. 32, no. 1, 31 January 2005 (2005-01-31), pages 31 - 35 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105738512A (en) * | 2016-02-23 | 2016-07-06 | 黑龙江八一农垦大学 | Pretreatment method for detecting butachlor and fipronil in liquid milk |
| CN105738512B (en) * | 2016-02-23 | 2018-03-06 | 黑龙江八一农垦大学 | Butachlor and the pre-treating method of ethiprole detection in liquid milk |
| CN105823835A (en) * | 2016-03-11 | 2016-08-03 | 山东省农业科学院农业质量标准与检测技术研究所 | GC-MS-MS determination method for determining residual quantity of flufiprole in vegetables |
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Application publication date: 20140312 |