CN106525992A - Method for dynamically analyzing degradation of quinclorac residues in different soil samples and water samples - Google Patents
Method for dynamically analyzing degradation of quinclorac residues in different soil samples and water samples Download PDFInfo
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- CN106525992A CN106525992A CN201610824541.5A CN201610824541A CN106525992A CN 106525992 A CN106525992 A CN 106525992A CN 201610824541 A CN201610824541 A CN 201610824541A CN 106525992 A CN106525992 A CN 106525992A
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- quinclorac
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- quinolinic acid
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
- G01N2030/146—Preparation by elimination of some components using membranes
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
- Soil Conditioners And Soil-Stabilizing Materials (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention provides a method for dynamically analyzing the degradation of quinclorac residues in different soil samples and water samples. The method comprises the following steps: (1) adding quinclorac: evenly spraying a quinclorac standard substance (99.5%) on soils in flowerpots with a same size according to a recommended field application amount (0.65 mg/kg), fully and evenly stirring, placing the flowerpots in a greenhouse, making the soils be in a wet state; colleting 50 grams of soil samples from each flowerpot in 1, 2, and 6 hours and 1, 2, 4, 8, 16, 40, 80, 120, and 160 d before and after the quinclorac application, evenly mixing the soil samples, taking 50 grams of mixed soil samples, pre-processing the mixed soil sample before detection; and preparing a water sample: adding a quinclorac standard solution into 50 mL of water sample according to 0.65 mg/L; and (2) soaking the soil/water sample in 50 mL of borax buffer solution (0.05 mol/L) for one hour under vibration, carrying out high speed centrifugation for 20 minutes, filtering the supernate by a 0.45 [mu]m filter membrane, and carrying out HPLC assay. The provided method can dynamically analyze the degradation of quinclorac in different soil samples and water samples and analyze the degradation rules and main influence factors of quinclorac under different soil conditions.
Description
Technical field
The present invention relates to field of chemical detection, particularly relates to residue degrading of the dichloro quinolinic acid in different soil samples and water sample
Dynamic analysing method.
Background technology
Also there are some research reports with regard to residue dynamics of the dichloro quinolinic acid in paddy rice and its ambient soil, water in field, but
In being the result that early stage is studied, the half-life of dichloro quinolinic acid is different, and has larger difference.With dichloro in produce reality
Quinolinic acid can be planted sensitive crop (eggplant, tobacco, tomato, carrot etc.) after needing 1～2 year after applying and not corresponded.Residues of pesticides
One of the factor for affecting agricultural product production and quality safety safety, due to the dichloro quinolinic acid longevity of residure it is long, it is easily sensitive to rear stubble
Crop tobacco, tomato, carrot, celery etc. cause serious harm, especially in paddy rice and tobacco crop rotation area, can cause tobacco
Growth deformity.There is not been reported for the research that different soil is affected on dichloro quinolinic acid residue degrading at present.
The content of the invention
The present invention proposes a kind of residue degrading dynamic analysing method of dichloro quinolinic acid in different soil samples and water sample, analysis
Its degradation rule and major influence factors under different soil, so as to for reasonable employment dichloro quinolinic acid, it is to avoid to rear
Stubble sensitive crop causes herbicide carryover and determines that implantation time provides scientific basis.
The technical scheme is that what is be achieved in that：Residue degrading of the dichloro quinolinic acid in different soil samples and water sample is moved
State analysis method, comprises the following steps：
(1) dichloro quinolinic acid addition is processed：By 99.5% dichloro quinolinic acid standard items according to recommendation field amount of application
0.65mg/kg uniformly sprays the soil in flowerpot of the same size, and stirs, and is put in greenhouse and keeps soil
Moistening；If three repetitions；Before dispenser, 1 after dispenser, 2,6h and 1,2,4,8,16,40,80,120,160d collection soil sample,
Per basin soil sampling 50g, taking wherein 50g soil samples after mixing carries out residue detection pre-treatment；It is prepared by water sample：By dichloro quinolinic acid standard
Solution is added in 50mL water samples according to 0.65mg/L, and each process sets three repetitions.
(2) 0.05mol/L borate buffer solutions 50mL immersions vibration 1h, high speed centrifugation 20min, take supernatant and cross 0.45 μm of filter
Film, HPLC are determined.
Chromatographiccondition is：
Chromatographic column：5 μm of HP ODS Hypersil, 4.0 × 250mm；
Mobile phase：Methyl alcohol：1% acetic acid aqueous solution, volume ratio are 60/40；
Flow velocity：1mL/min；
Detection wavelength is：240nm；
Sample size：10μl.
Further, quality measurement control and safeguard measure is analyzed, the control of analysis quality measurement is additionally provided with method and is ensured
Measure：Blank sample and Duplicate Samples；1 blank sample of band is needed per batch analysis sample, with Confirmation reagent and the clean-up performance of container；Divide per batch
Analysis sample needs 2～3 Duplicate Samples of band, with the repeatability of exact p-value result.
Residue degrading dynamic analysing method of the dichloro quinolinic acid of the present invention in different soil samples and water sample, with reference to soil
The degradation characteristic research of dichloroquinoline in earth, and the adjustment of procedure and parameter, realize to dichloro quinolinic acid in different soil
Residue degrading dynamic analysis in sample and water sample, and analyze its degradation rule under different soil and mainly affect because
Element, so as to for reasonable employment dichloro quinolinic acid, it is to avoid causes herbicide carryover to late stubble sensitive crop and determines that implantation time is provided
Scientific basis.
Description of the drawings
Fig. 1：Dichloro quinolinic acid clears up curve map in the soil of Nanxiong；
Fig. 2：Dichloro quinolinic acid clears up curve map in the soil of iron Lu lake；
Fig. 3：Dichloro quinolinic acid clears up curve map in the soil of Liaoning Fuxin；
Fig. 4：Dichloro quinolinic acid clears up curve map in Dongzhou Period in Chuxiong soil；
Fig. 5：Dichloro quinolinic acid clears up curve map in Yunnan Yuxi's soil.
Specific embodiment
Below in conjunction with the accompanying drawing of embodiments of the invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than the embodiment of whole.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
1st, dichloro quinolinic acid addition is processed
99.5% dichloro quinolinic acid standard items are uniformly sprayed in a diameter of according to recommendation field amount of application 0.65mg/kg
Soil in 17cm, high 13cm flowerpots of the same size, and stir, it is put in greenhouse and keeps ground moistening.If
Three repetitions.Before dispenser, 1 after dispenser, 2,6h and 1,2,4,8,16,40,80,120,160d collection soil samples, take per basin
Soil sample 50g, taking wherein 50g soil samples after mixing carries out residue detection pre-treatment.It is prepared by water sample：Dichloro quinolinic acid standard liquid is pressed
Add in 50mL water samples according to 0.65mg/L, each process sets three repetitions.
2nd, pedotheque pre-treatment
0.05mol/L borate buffer solutions 50mL immersion vibration 1h, high speed centrifugation 20min (6000r/min), take supernatant mistake
0.45 μm of filter membrane, HPLC are determined.
3rd, chromatographiccondition
Chromatographic column：5 μm of HP ODS Hypersil, 4.0 × 250mm；
Mobile phase：Methyl alcohol：1% acetic acid aqueous solution (volume ratio is 60/40)；
Flow velocity：1mL/min；
Detection wavelength is：240nm；
Sample size：10μl.
4th, method Quality Control measure
The control of analysis quality measurement and safeguard measure：1. blank sample：1 blank sample of band is needed per batch analysis sample, to confirm examination
Agent and the clean-up performance of container；2. Duplicate Samples：2～3 Duplicate Samples (20%) of band are needed per batch analysis sample, with exact p-value result
Repeatability.
According to said method, it is analyzed in different water samples and soil sample respectively.
What the various sources of dichloro quinolinic acid were different sees Fig. 1-5 for examination soil and the degraded trend in water sample；
Dichloro quinolinic acid is substantially following first _ order kinetics equation, i.e. Ct=for examination soil and the degradation dynamic in water sample
C0e- kt, t1/2The parameter of dichloro quinolinic acid Residue Degradation equation in sample is listed in=ln2/k. table 2-4, table 2-4, in sample
Correlation coefficient r between residual quantity Ct of middle dichloro quinolinic acid and degradation time t is more than 0.87.Dichloro quinolinic acid in sample
Half-life scope be 48.6d～66.7d.
Residue degrading result such as following table of the dichloro quinolinic acid in pedotheque：
Presently preferred embodiments of the present invention is the foregoing is only, not to limit the present invention, all essences in the present invention
Within god and principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (3)
1. residue degrading dynamic analysing method of the dichloro quinolinic acid in different soil samples and water sample, it is characterised in that including following
Step：
(1) dichloro quinolinic acid addition is processed：By 99.5% dichloro quinolinic acid standard items according to recommendation field amount of application 0.65mg/kg
The soil in flowerpot of the same size is uniformly sprayed, and is stirred, be put in greenhouse and keep ground moistening；Respectively
Before dispenser, 1 after dispenser, 2,6h and 1,2,4,8,16,40,80,120,160d collection soil samples, per basin soil sampling 50g, after mixing
Taking wherein 50g soil samples carries out residue detection pre-treatment；It is prepared by water sample：Dichloro quinolinic acid standard liquid is added according to 0.65mg/L
In 50mL water samples.
(2) pedotheque pre-treatment：0.05mol/L borate buffer solutions 50mL immersion vibration 1h, high speed centrifugation 20min, take supernatant
Liquid crosses 0.45 μm of filter membrane, and HPLC is determined.
2. residue degrading dynamic analysing method of the dichloro quinolinic acid in different soil samples and water sample as described in the appended claim 1, its
It is characterised by：In step (2), chromatographiccondition is：
Chromatographic column：5 μm of HP ODS Hypersil, 4.0 × 250mm；
Mobile phase：Methyl alcohol：1% acetic acid aqueous solution, volume ratio are 60/40；
Flow velocity：1mL/min；
Detection wavelength is：240nm；
Sample size：10μl.
3. residue degrading dynamic analysing method of the dichloro quinolinic acid in different soil samples and water sample as described in the appended claim 1, its
It is characterised by：The control of analysis quality measurement and safeguard measure is additionally provided with method：Blank sample and Duplicate Samples；Band is needed per batch analysis sample
1 blank sample, needs 2～3 Duplicate Samples of band per batch analysis sample.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610824541.5A CN106525992A (en) | 2016-09-14 | 2016-09-14 | Method for dynamically analyzing degradation of quinclorac residues in different soil samples and water samples |
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| CN201610824541.5A CN106525992A (en) | 2016-09-14 | 2016-09-14 | Method for dynamically analyzing degradation of quinclorac residues in different soil samples and water samples |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109212108A (en) * | 2018-11-25 | 2019-01-15 | 丁立平 | Gas chromatography-mass spectrometry that is a kind of while measuring three kinds of trace quinolines herbicides in rice and soybean |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000005956A1 (en) * | 1998-07-25 | 2000-02-10 | Dongbu Hannong Chemical Co., Ltd. | Herbicidal phenoxypropionic acid n-alkyl-n-2-fluorophenyl amide compounds |
| CN102901782A (en) * | 2012-10-30 | 2013-01-30 | 湖南省烟草公司郴州市公司 | Residue detection method for quinclorac in tobacco leaf and tobacco planting soil |
-
2016
- 2016-09-14 CN CN201610824541.5A patent/CN106525992A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000005956A1 (en) * | 1998-07-25 | 2000-02-10 | Dongbu Hannong Chemical Co., Ltd. | Herbicidal phenoxypropionic acid n-alkyl-n-2-fluorophenyl amide compounds |
| CN102901782A (en) * | 2012-10-30 | 2013-01-30 | 湖南省烟草公司郴州市公司 | Residue detection method for quinclorac in tobacco leaf and tobacco planting soil |
Non-Patent Citations (4)
| Title |
|---|
| 张倩等: "二氯喹啉酸在不同土壤中的降解规律及其影响因子", 《中国烟草科学》 * |
| 王一茹等: "二氯喹啉酸及其代谢物在稻田水土作物中的气谱和液谱残留分析方法研究", 《农业环境保护》 * |
| 苑学霞等: "二氯喹啉酸在水稻、土壤和田水中消解动态及残留", 《生态环境学报》 * |
| 陈泽鹏等: "烟区土壤残留二氯喹啉酸的消解动态", 《农药》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109212108A (en) * | 2018-11-25 | 2019-01-15 | 丁立平 | Gas chromatography-mass spectrometry that is a kind of while measuring three kinds of trace quinolines herbicides in rice and soybean |
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