CN106596539A - Supermolecular kit and method for quick detection of diquat - Google Patents

Supermolecular kit and method for quick detection of diquat Download PDF

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Publication number
CN106596539A
CN106596539A CN201611181781.4A CN201611181781A CN106596539A CN 106596539 A CN106596539 A CN 106596539A CN 201611181781 A CN201611181781 A CN 201611181781A CN 106596539 A CN106596539 A CN 106596539A
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China
Prior art keywords
reagent
solution
diquat dibromide
supermolecule
test kit
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CN201611181781.4A
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Chinese (zh)
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CN106596539B (en
Inventor
刘东晖
刘畅
毕嘉玮
王鹏
周志强
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China Agricultural University
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China Agricultural University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems 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
    • G01N21/78Systems 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

Abstract

Disclosed are a supermolecular kit and a method for quick detection of diquat. The supermolecular kit comprises a reagent 1 and a reagent 2, wherein the reagent 1 is a solution prepared from safranine T and carboxymethyl-beta-cyclodextrin, and the reagent 2 is a solution prepared from methylene blue and carboxymethyl-beta-cyclodextrin. The supermolecular kit is capable of detecting the diquat qualitatively through color matching by naked eyes and solves the problems about time and cost.

Description

The supermolecule test kit of quick detection diquat dibromide and method
Technical field
This patent disclosure relates generally to field of pesticide detection, and in particular to the supermolecule test kit and method of detection diquat dibromide.
Background technology
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 Rise, revocation N,N'-dimethyl-.gamma..gamma.'-dipyridylium water preparation is registered and production permit, stopping production;On July 1st, 2016 stops water preparation and sells at home and make With.And diquat dibromide is the third-largest steriland herbicide that the whole world is only second to glyphosate and N,N'-dimethyl-.gamma..gamma.'-dipyridylium.Therefore, diquat dibromide is used as BAICAO Withered replacement pesticide can be presented elevated trend in the usage amount of China.But being because the price of diquat dibromide can be far above BAICAO It is withered, therefore some producers' meeting profit-pushes, N,N'-dimethyl-.gamma..gamma.'-dipyridylium is mixed in the medicament of diquat dibromide, so to the diquat dibromide product on market It is necessary that quality carries out inspecting by random samples.And a large amount of uses with diquat dibromide and its be highly soluble in the characteristic of water, water ring Also certainly will can there is diquat dibromide in border, environmentally safe may produce threat.Therefore the method for developing quick detection diquat dibromide The quality of Pesticidal products itself is not only can guarantee that, but also people's life safety, Environmental security and agricultural product quality can be ensured Safety.
At present, for the analysis method of this diquat dibromide is mainly Instrumental Analysis, such as liquid chromatograph, capillary electrophoresis, mass spectrum Deng.However, instrumental method needs sample collecting to be returned after laboratory, identification and analysis are carried out using expensive instrument, cost Time and cost costly, especially for ruck for, the instrument not having ready conditions using complex precise.
The content of the invention
The invention aims to overcome above-mentioned some or certain defect of the prior art, there is provided a kind of supermolecule examination Agent box, and it is applied to quick detection diquat dibromide.
According to the first aspect of the invention, there is provided a kind of supermolecule test kit of quick detection diquat dibromide, the test kit Including reagent 1 and 2, reagent 1 be by safranine T (Safranine T, ST) and carboxymethyl-beta-cyclodextrin (Carboxymethyl- β- Cyclodextrin, CM- β-CD) configuration solution;Reagent 2 is by methylene blue (Methylene blue, MB) and CM- The solution of β-CD configurations.
In a preferred embodiment of the invention, the molar ratio range of ST and CM- β-CD is 1 wherein in reagent 1:1.5 To 1:2, the molar ratio range of MB and CM- β-CD is 1 in reagent 2:1.5 to 1:2.
According to the second aspect of the invention, there is provided a kind of method of quick detection diquat dibromide, comprise the following steps:
(1) the supermolecule test kit described in first aspect present invention is provided;
(2) a series of concentration diquat dibromide standard aqueous solution from low to high is respectively configured, each standard aqueous solution is divided into two Part, reagent 1 and 2 is separately added into, the reference colours band of each reagent is formed according to chromogenic reaction;
(3) detected sample 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 colours band of each reagent, draws qualification result.
Under preferable case, before reagent 1 and 2 is added, first by preparing solution into alkalescence condition.Further preferred situation Under, the pH value of alkaline solution is 11-12.In the basic conditions, object is more complete with supermolecule reagent reacting, chromogenic reaction It is clearer and more definite.
The method comprises the steps of firstly, preparing having the supermolecule test kit of specificity to diquat dibromide, can be compared with regard to energy by color It is detected, reduce analysis time and cost, suitable general public is used.
Description of the drawings
Fig. 1 is the photo that a series of diquat dibromide water sample of concentration is separately added into reagent 1.
Fig. 2 is the photo that a series of diquat dibromide water sample of concentration is separately added into reagent 2.
Specific embodiment
The invention provides a kind of supermolecule test kit and method that diquat dibromide is detected for Rapid identification, with reference to tool The present invention will be further described for body embodiment.
First, reagent
Safranine T (ST), methylene blue (MB) and hematoxylin (HT), buy in Aladdin;Carboxymethyl-beta-cyclodextrin is bought In Shandong Binzhou Zhi Yuan bio tech ltd;Diquat dibromide standard specimen, was bought in Inst. of Environment Protection & Scientific Research Monitor, Ministry of Agric, used time The working solution of desired concn is diluted to ultra-pure water.
2nd, the preparation of supermolecule test kit
Take 0.0088g ST and be placed in the ST solution that 25mL volumetric flasks obtain 0.001mol/L, 0.0093g MB are placed in 25mL appearances Measuring bottle obtains the MB solution of 0.001mol/L, 0.0850g CM- β-CD be placed in 50mL volumetric flasks obtain 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 tubes, and mix homogeneously is reagent 1;Take CM- β-CD the solution of the MB solution of 125 μ L and 250 μ L is placed in 1mL centrifuge tubes, and mix homogeneously is reagent 2.
3rd, using the method for supermolecule test kit quick detection diquat dibromide
Eight 10mL centrifuge tubes are taken, the ultra-pure water and diquat dibromide standard solution (1 of 2125 μ L alkalescence (pH=12) is 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) is then all added.Eight 10mL centrifuge tubes are taken, 2125 μ L alkalescence (pH=are separately added into 12) ultra-pure 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) is then all added.
Add in water sample after reagent, stand after 20min after mix homogeneously, observe its color change.As a result such as Fig. 1-2, Blank water sample is in first bottle in figure, the sample containing diquat dibromide is in 7 bottles thereafter.As a result show:Reagent 1 adds Enter be shown as in diquat dibromide from low concentration to high concentration for light red to orange to peony;Reagent 2 is added in diquat dibromide It is shown as from low concentration to high concentration as 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 result of Fig. 1-2 can with it is concluded that:For the pesticide sample of variable concentrations, Reagent 1 and reagent 2 can be detected well to diquat dibromide.Being combined use using reagent 1 and reagent 2 can be mutual Checking qualification result.
The reference colours band of reagent 1,2 is formed respectively by above step.When a certain sample liquid is detected, sample liquid is divided into Two parts, reagent 1,2 is added separately in a sample liquid with reference to above step, according to the color of sample liquid respectively with reagent 1, 2 reference colours band is compared, and draws qualification result.
It should be appreciated by those skilled in the art that specific embodiment mentioned 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 defined by the restriction of claims.

Claims (5)

1. a kind of supermolecule test kit of quick detection diquat dibromide, it is characterised in that:The supermolecule test kit includes the He of reagent 1 2, reagent 1 is the solution configured by safranine T (ST) and carboxymethyl-beta-cyclodextrin (CM- β-CD);Reagent 2 is by methylene Blue (MB) and the solution of CM- β-CD configurations.
2. supermolecule test kit as claimed in claim 2, it is characterised in that:The molar ratio range of ST and CM- β-CD wherein in reagent 1 For 1:1.5 to 1:2, the molar ratio range of MB and CM- β-CD is 1 in reagent 2:1.5 to 1:2.
3. a kind of method of quick detection diquat dibromide, it is characterised in that:Comprise the following steps:
(1) supermolecule test kit as claimed in claim 1 or 2 is provided;
(2) a series of concentration diquat dibromide standard aqueous solution 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 colours band of each reagent is formed according to chromogenic reaction;
(3) detected sample 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 colours band of each reagent, draws 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 into alkalescence Condition.
5. method as claimed in claim 4, it is characterised in that:The pH value of alkaline solution is 11-12.
CN201611181781.4A 2016-12-20 2016-12-20 The quickly supermolecule kit and method of detection diquat dibromide Expired - Fee Related CN106596539B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

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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

Patent Citations (3)

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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

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GUI-XIAN SONG ET AL.: "A host–guest complexation based fluorescent probe for the detection of paraquat and diquat herbicides in aqueous solutions", 《RSC ADV》 *
ROY N. DSOUZA ET AL: "Fluorescent Dyes and Their Supramolecular Host/Guest Complexes with Macrocycles in Aqueous Solution", 《CHEM. REV》 *
SHIGUO SUN ET AL: "Fluorescence detecting of paraquat using host-guest chemistry with cucurbit[8]uril", 《SCIENTIFIC REPORTS》 *
宋桂先等: "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", 《中国优秀硕士学位论文全文数据库》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

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