CN106596539B - The quickly supermolecule kit and method of detection diquat dibromide - Google Patents
The quickly supermolecule kit and method of detection diquat dibromide Download PDFInfo
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- CN106596539B CN106596539B CN201611181781.4A CN201611181781A CN106596539B CN 106596539 B CN106596539 B CN 106596539B CN 201611181781 A CN201611181781 A CN 201611181781A CN 106596539 B CN106596539 B CN 106596539B
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- diquat dibromide
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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Abstract
A kind of the supermolecule kit and method of quick detection diquat dibromide, the supermolecule kit include reagent 1 and 2, and reagent 1 is the solution as made of safranine T and carboxymethyl-beta-cyclodextrin configuration；Reagent 2 is the solution as made of methylene blue and carboxymethyl-beta-cyclodextrin configuration.Using supermolecule kit of the invention, can directly be compared by naked eye color qualitatively to be detected the pesticide, overcome the problems, such as time and cost.
Description
Technical field
This patent disclosure relates generally to field of pesticide detection, and in particular to detects the supermolecule kit and method of diquat dibromide.
Background technique
According to the Ministry of Agriculture, the Ministry of Industry and Information Technology, State Administration for Quality Supervision and Inspection and Quarantine's bulletin, from July 1st, 2014
It rises, the registration of revocation paraquat aqua and production permit stop production；Stopping on July 1st, 2016 aqua is sold and is made at home
With.And diquat dibromide is the third-largest steriland herbicide that the whole world is only second to glyphosate and paraquat.Therefore, diquat dibromide is as hundred grass
Raised trend can be presented in usage amount of the withered substitution pesticide in China.But because the price of diquat dibromide can be much higher than hundred grass
It is withered, therefore the meeting profit-push of some producers, paraquat is mixed in the medicament of diquat dibromide, so to diquat dibromide product in the market
It is necessary that quality, which carries out sampling observation,.And with a large amount of uses of diquat dibromide and its characteristic for being highly soluble in water, water ring
Can certainly will also there be diquat dibromide in border, it may environmentally safe generation threat.Therefore the method for quickly detection diquat dibromide is developed
It not only can guarantee the quality of Pesticidal products itself, but also can ensure people's life safety, Environmental security and agricultural product quality
Safety.
Currently, being mainly instrument analysis for the analysis method of this diquat dibromide, such as liquid chromatogram, Capillary Electrophoresis, mass spectrum
Deng.However, identification and analysis is carried out using expensive instrument after instrumental method needs sample acquiring go back to laboratory, cost
Time and cost costly, for ruck, the instrument do not had ready conditions using complex precise.
Summary of the invention
The purpose of the invention is to overcome above-mentioned in the prior art certain or some defect, a kind of supermolecule examination is provided
Agent box, and it is applied to quickly detection diquat dibromide.
According to the first aspect of the invention, a kind of supermolecule kit of quickly detection diquat dibromide, the kit are provided
Including reagent 1 and 2, reagent 1 is by safranine T (Safranine T, ST) and carboxymethyl-beta-cyclodextrin (Carboxymethyl- β-
Cyclodextrin, CM- β-CD) configuration made of solution；Reagent 2 is by methylene blue (Methylene blue, MB) and CM-
Solution made of β-CD configuration.
In a preferred embodiment of the invention, wherein the molar ratio range of ST and CM- β-CD is 1:1.5 in reagent 1
To 1:2, the molar ratio range of MB and CM- β-CD is 1:1.5 to 1:2 in reagent 2.
According to the second aspect of the invention, a kind of method of quickly detection diquat dibromide is provided, comprising the following steps:
(1) supermolecule kit described in first aspect present invention is provided；
(2) a series of diquat dibromide standard aqueous solution of concentration from low to high is respectively configured, each standard aqueous solution is divided into two
Part, it is separately added into reagent 1 and 2, forms the reference colour band of each reagent according to chromogenic reaction；
(3) sample to be tested liquid is provided, is divided into two parts, reagent 1,2 is added separately in a sample liquid, according to sample
The color of liquid is compared with the reference colour band of each reagent, obtains qualification result.
Under preferable case, before reagent 1 and 2 is added, first by preparing solution at alkaline condition.Further preferred situation
Under, the pH value of alkaline solution is 11-12.Under alkaline condition, object reacts more complete with supermolecule reagent, chromogenic reaction
It is more clear.
The method comprises the steps of firstly, preparing the supermolecule kits to diquat dibromide with specificity, can compare energy by color
It is detected, analysis time and cost are reduced, is suitable for that general public uses.
Detailed description of the invention
Fig. 1 is that a series of diquat dibromide water sample of concentration is separately added into the photo of reagent 1.
Fig. 2 is that a series of diquat dibromide water sample of concentration is separately added into the photo of reagent 2.
Specific embodiment
The present invention provides a kind of supermolecule kits and method for Rapid identification detection diquat dibromide, below with reference to tool
The present invention will be further described for body embodiment.
One, reagent
Safranine T (ST), methylene blue (MB) and hematoxylin (HT), purchase is in Aladdin；Carboxymethyl-beta-cyclodextrin purchase
In Shandong Binzhou Zhi Yuan Biotechnology Co., Ltd；Diquat dibromide standard specimen was bought in Inst. of Environment Protection & Scientific Research Monitor, Ministry of Agric, used time
The working solution of required concentration is diluted to ultrapure water.
Two, the preparation of supermolecule kit
It takes 0.0088g ST to be placed in 25mL volumetric flask and obtains the ST solution of 0.001mol/L, 0.0093g MB is placed in 25mL appearance
Measuring bottle obtains the MB solution of 0.001mol/L, and 0.0850g CM- β-CD is placed in 50mL volumetric flask and obtains the CM- β-of 0.001mol/L
CD solution.CM- β-CD the solution of the ST solution and 250 μ L that take 125 μ L is placed in 1mL centrifuge tube, and being uniformly mixed is reagent 1；It takes
CM- β-CD the solution of the MB solution of 125 μ L and 250 μ L are placed in 1mL centrifuge tube, and being uniformly mixed is reagent 2.
Three, the method for quickly detecting diquat dibromide using supermolecule kit
Eight 10mL centrifuge tubes are taken, the ultrapure water and diquat dibromide standard solution (1 of 2125 μ L alkaline (pH=12) are separately added into
×10-5mol/L、5×10-5mol/L、1×10-4mol/L、2.5×10-4mol/L、5×10-4mol/L、8×10-4mol/L、1
×10-3Mol/L), reagent 1 (375 μ L) all then is added.Eight 10mL centrifuge tubes are taken, 2125 μ L alkalinity (pH=are separately added into
12) ultrapure water and diquat dibromide standard solution (1 × 10-5mol/L、5×10-5mol/L、1×10-4mol/L、2.5×10-4mol/
L、5×10-4mol/L、8×10-4mol/L、1×10-3Mol/L), reagent 2 (375 μ L) all then is added.
After reagent is added into water sample, after standing 20min after mixing, its color change is observed.As a result such as Fig. 1-2,
In first bottle it is blank water sample in figure, is thereafter the sample containing diquat dibromide in 7 bottles.The result shows that: reagent 1 adds
Enter to be shown as into diquat dibromide from low concentration to high concentration to be light red to orange to peony；Reagent 2 is added in diquat dibromide
It is shown as from low concentration to high concentration to be light blue to green to blackish green.Reagent 1 and reagent 2 are added to solution after diquat dibromide
Color changes, especially reagent 2.From the available conclusion of the result of Fig. 1-2: for the pesticide sample of various concentration,
Reagent 1 and reagent 2 can well detect diquat dibromide.Being combined use using reagent 1 and reagent 2 can be mutual
Verify qualification result.
The reference colour band of reagent 1,2 is respectively formed by above step.When detecting a certain sample liquid, sample liquid is divided into
Two parts, reagent 1,2 is added separately in a sample liquid referring to above step, according to the color of sample liquid respectively with reagent 1,
2 reference colour band is compared, and obtains qualification result.
It should be appreciated by those skilled in the art that specific embodiment described above is only for more fully understanding the present invention, and
It is not used in and limits the invention, protection scope of the present invention should be subject to the restriction of claims.
Claims (5)
1. a kind of supermolecule kit of quickly detection diquat dibromide, it is characterised in that: the supermolecule kit includes 1 He of reagent
2, reagent 1 is the solution as made of safranine T and carboxymethyl-beta-cyclodextrin configuration；Reagent 2 is by methylene blue and carboxymethyl-β-
Solution made of cyclodextrin configuration.
2. supermolecule kit as claimed in claim 1, it is characterised in that: wherein safranine T and carboxymethyl-beta-cyclodextrin in reagent 1
Molar ratio range be 1:1.5 to 1:2, the molar ratio range of 2 Methylene Blue of reagent and carboxymethyl-beta-cyclodextrin is 1:1.5
To 1:2.
3. a kind of method of quickly detection diquat dibromide, it is characterised in that: the following steps are included:
(1) supermolecule kit as claimed in claim 1 or 2 is provided；
(2) a series of diquat dibromide standard aqueous solution of concentration from low to high is respectively configured, each standard aqueous solution is divided into two parts, point
Not Jia Ru reagent 1 and 2, the reference colour band of each reagent is formed according to chromogenic reaction；
(3) sample to be tested liquid is provided, is divided into two parts, reagent 1,2 is added separately in a sample liquid, according to sample liquid
Color is compared with the reference colour band of each reagent, obtains qualification result.
4. method as claimed in claim 3, it is characterised in that: before reagent 1 and 2 is added, first by preparing solution at alkalinity
Condition.
5. method as claimed in claim 4, it is characterised in that: the pH value of alkaline solution is 11-12.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611181781.4A CN106596539B (en) | 2016-12-20 | 2016-12-20 | The quickly supermolecule kit and method of detection diquat dibromide |
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| CN201611181781.4A CN106596539B (en) | 2016-12-20 | 2016-12-20 | The quickly supermolecule kit and method of detection diquat dibromide |
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| CN106596539A CN106596539A (en) | 2017-04-26 |
| CN106596539B true CN106596539B (en) | 2018-12-18 |
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| CN110220892A (en) * | 2019-05-31 | 2019-09-10 | 山东大学齐鲁医院 | A kind of diquat dibromide half-quantitative detection map is formulated and urine detection method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1325333A1 (en) * | 1985-09-17 | 1987-07-23 | Всесоюзный Научно-Исследовательский Институт Гигиены И Токсикологии Пестицидов,Полимеров И Пластических Масс | Method of determining diquat |
| JPH07291803A (en) * | 1994-04-26 | 1995-11-07 | Takeda Chem Ind Ltd | Water-soluble granular agrochemical |
| CN106198507A (en) * | 2016-04-21 | 2016-12-07 | 中国科学院大连化学物理研究所 | Sulfur-bearing organophosphorus insecticide sensor and preparation thereof and application |
-
2016
- 2016-12-20 CN CN201611181781.4A patent/CN106596539B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1325333A1 (en) * | 1985-09-17 | 1987-07-23 | Всесоюзный Научно-Исследовательский Институт Гигиены И Токсикологии Пестицидов,Полимеров И Пластических Масс | Method of determining diquat |
| JPH07291803A (en) * | 1994-04-26 | 1995-11-07 | Takeda Chem Ind Ltd | Water-soluble granular agrochemical |
| CN106198507A (en) * | 2016-04-21 | 2016-12-07 | 中国科学院大连化学物理研究所 | Sulfur-bearing organophosphorus insecticide sensor and preparation thereof and application |
Non-Patent Citations (4)
| Title |
|---|
| A host–guest complexation based fluorescent probe for the detection of paraquat and diquat herbicides in aqueous solutions;Gui-Xian Song et al.;《RSC Adv》;20151117;第5卷;第7941–7980页 * |
| Fluorescence detecting of paraquat using host-guest chemistry with cucurbit[8]uril;Shiguo Sun et al;《SCIENTIFIC REPORTS》;20140106;第1-5页 * |
| Fluorescent Dyes and Their Supramolecular Host/Guest Complexes with Macrocycles in Aqueous Solution;Roy N. Dsouza et al;《Chem. Rev》;20111007;第111卷;第100316–100321页 * |
| 瓜环/农药/协同（竞争）客体超分子 体系构筑及其分析检测性能研究;宋桂先等;《中国优秀硕士学位论文全文数据库》;20160315;全文 * |
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