CN101532987B - Method for measuring chlorotoluron content - Google Patents
Method for measuring chlorotoluron content Download PDFInfo
- Publication number
- CN101532987B CN101532987B CN2009101139792A CN200910113979A CN101532987B CN 101532987 B CN101532987 B CN 101532987B CN 2009101139792 A CN2009101139792 A CN 2009101139792A CN 200910113979 A CN200910113979 A CN 200910113979A CN 101532987 B CN101532987 B CN 101532987B
- Authority
- CN
- China
- Prior art keywords
- solution
- mol
- chlorotoluron
- chlortoluron
- platinum electrode
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Investigating Or Analysing Biological Materials (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
Abstract
The invention discloses a method for measuring chlorotoluron content. Obvious electrochemical signals are present on a platinum electrode surface in potassium ferricyanide solution. When molecule chlorotoluron to be measured reacts with chlorotoluron molecular engram, the electrochemical signals on the K3 [Fe(CN)6] platinum electrode change, thus an electrochemical analysis method for measuring chlorotoluron content is established. The solution to be measured is scanned using cyclic voltammetry and the scanning voltage is -0.2V to 0.6V and the linear relationship between chlorotoluron contentin concentration range of 3*10<-7>mol/L-1.5*10<-6>mol/L and peak current value I is good. The method conquers the defects of the prior technique such as very complex and has high sensitivity and good detection effect for chlorotoluron of 10<-7> mol/L.
Description
Technical field
The present invention relates to a kind of method of measuring chlorotoluron content, particularly a kind of electrochemical sensor of molecular imprinting fast measuring trace chlortoluron that utilizes is used for food chlortoluron Determination on content.
Background technology
Chlortoluron be a kind of on agricultural widely used substituted urea class selectivity inner sucting conduction type herbicide, mainly absorb, and the blade face action of contace poison arranged through plant roots; It is the photosynthesis electron transfer inhibitor; Because its degradation speed is slow, the residence time is long, so often be present in surface water, underground water and the crops; And their residual very low in environment, therefore research is significant to the detection method that chlortoluron has high selectivity.Molecular engram is that a kind of that development in recent years is got up has optionally synthetic method of polymers to microsphere.Along with relevant engram technology deepens continuously what study aspect the Pesticides Testing, related pesticide species is tending towards variation.The trace sensor of having reported is useful on the detection of tens kinds of agricultural chemicals such as atrazine, desmetryn, glyphosate, parathion, chloromycetin, but the research of chlortoluron molecular engram sensitive membrane sensor does not appear in the newspapers.
Summary of the invention
The object of the present invention is to provide a kind of sensor highly sensitive, that selectivity is good that utilizes, to 10
-7The chlortoluron of mol/L carries out method for measuring.
Conceive as follows: discover K
3[Fe (CN)
6] can be used as ion probe, when the chlortoluron molecular engram film forms and the chlortoluron molecular action time in platinum electrode surface, its electrochemical signals generation marked change on platinum electrode can be used for detecting the content of chlortoluron within the specific limits.
The present invention relates to molecular imprinting.When testing molecule chlortoluron and chlortoluron molecular engram film are had an effect, K
3[Fe (CN)
6] electrochemical signals on platinum electrode changes, the concentration of peak current and chlortoluron is linear within the specific limits.
Concrete steps are following:
(1) processing of platinum electrode:
Platinum electrode successively with the alumina powder polishing of 1.0~0.05 μ m, is washed at salpeter solution, absolute ethyl alcohol, the pure bubbly water of volumetric concentration 50% successively, taken out back supersound washing 5min.
(2) preparation of molecular engram film:
Take by weighing 0.028~0.112g N, the N-methylene-bisacrylamide, the chlortoluron solution of adding 20~80mL 0.03mol/L, the adding concentration expressed in percentage by volume is 98% methacrylic acid 5~20 μ L, ultrasonic 10min.Hold over night makes its fully effect each other.Add 30~120 μ L ammonium persulfates (0.5mol/L), initiated polymerization immerses platinum electrode in the polymerization liquid, takes out behind the 10min and dries.
(3) detection method:
Get the small beaker of a 15mL, add and contain 3 * 10 of 0.5mol/L KCl
-4Mol/L K
3[Fe (CN)
6] solution 10mL, drip 3 * 10
-4Mol/L chlortoluron solution 30 μ L.Select for use the cyclic voltammetry in the CHI660 type electrochemical workstation solution to be measured to be scanned scanning voltage-0.2~0.6V.
(4) mensuration of chlorotoluron content
Get a 15mL small beaker, add and contain 3 * 10 of 0.5mol/L KCl
-4Mol/L K
3[Fe (CN)
6] solution 10mL, drip the solution to be measured 50 μ L that contain chlortoluron.Select for use the cyclic voltammetry in the CHI660 type electrochemical workstation that solution to be measured is scanned, scanning voltage-0.2~0.6V reads peak point current i, according to i=0.37798C-0.78127, calculates the amount of contained chlortoluron in the solution to be measured.
The present invention has overcome prior art and had too many shortcomings such as complicacy, and is highly sensitive, for 10
-7The detection of mol/L chlortoluron is easy to robotization.
Description of drawings
Fig. 1 is the cyclic voltammogram of chlortoluron molecular engram film on the embodiment of the invention platinum electrode.
Fig. 2 is the graph of a relation of embodiment of the invention chlorotoluron content and cyclic voltammetry peak current.
Embodiment
Embodiment:
(1) processing of platinum electrode:
Platinum electrode successively with the alumina powder polishing of 1.0 μ m, 0.3 μ m and 0.05 μ m, is washed at salpeter solution, absolute ethyl alcohol, the pure bubbly water of volumetric concentration 50% successively, taken out back supersound washing 5min.
(2) preparation of molecular engram film:
Take by weighing 0.028g N, the N-methylene-bisacrylamide adds the chlortoluron solution of 20mL 0.03mol/L, adds the methacrylic acid (concentration expressed in percentage by volume is 98%) of 5 μ L, ultrasonic 10min.Hold over night makes its fully effect each other.Add 30 μ L ammonium persulfates (0.5mol/L), initiated polymerization immerses platinum electrode in the polymerization liquid, takes out behind the 10min and dries.
(3) detection method:
Get the small beaker of a 15mL, add and contain 3 * 10 of 0.5mol/L KCl
-4Mol/L K
3[Fe (CN)
6] solution 10mL, drip 3 * 10
-4Mol/L chlortoluron solution 30 μ L.Select for use the cyclic voltammetry in the CHI660 type electrochemical workstation that solution to be measured is scanned, scanning voltage-0.2~0.6V (like Fig. 1).
(4) drafting of standard working curve:
Get the 15mL small beaker, add and contain 3 * 10 of 0.5mol/L KCl
-4Mol/L K
3[Fe (CN)
6] solution 10mL, add 5 μ L3 * 10 one by one
-4Mol/L chlortoluron solution, cyclic voltammetry scan.Chlortoluron is 3 * 10
-7~1.5 * 10
-6Be good linear relationship with peak point current i in the mol/L concentration range: i=0.37798C-0.78127, coefficient R=0.9998, chlorotoluron content and peak current relation are as shown in Figure 2.
(5) actual detected is used:
Get the farmland water sample and measure, but do not detect chlortoluron, reclaim experiment so adopt calibration curve method to carry out mark-on.Get a 15mL small beaker, add and contain 3 * 10 of 0.5mol/L KCl
-4Mol/L K
3[Fe (CN)
6] solution 10mL, drip the farmland WS 50 μ L that added chlortoluron.Select for use the cyclic voltammetry of CHI660 type electrochemical workstation solution to be measured to be carried out sweep measuring, scanning voltage-0.2~0.6V.Read peak point current I, and with its substitution i=0.37798C-0.78127.Calculate C.Replicate determination three times, calculate recovery rate, the result is as shown in table 1.
Table 1 mark-on recovery test data
Claims (1)
1. method of measuring chlorotoluron content is characterized in that concrete steps are following:
(1) processing of platinum electrode:
Platinum electrode successively with the alumina powder polishing of 1.0~0.05 μ m, is washed at salpeter solution, absolute ethyl alcohol, the pure bubbly water of volumetric concentration 50% successively, taken out back supersound washing 5min;
(2) preparation of molecular engram film:
Take by weighing 0.028~0.112g N, the N-methylene-bisacrylamide, the chlortoluron solution of adding 20~80mL 0.03mol/L, the adding concentration expressed in percentage by volume is 98% methacrylic acid 5~20 μ L, ultrasonic 10min; Hold over night makes its fully effect each other; Add the ammonium persulfate of 30~120 μ L0.5mol/L, initiated polymerization immerses platinum electrode in the polymerization liquid, takes out behind the 10min and dries;
(3) detection method:
Get the small beaker of a 15mL, add and contain 3 * 10 of 0.5mol/L KCl
-4Mol/L K
3[Fe (CN)
6] solution 10mL, drip 3 * 10
-4Mol/L chlortoluron solution 30 μ L; Select for use the cyclic voltammetry in the CHI660 type electrochemical workstation solution to be measured to be scanned scanning voltage-0.2~0.6V;
(4) drafting of standard working curve:
Get the 15mL small beaker, add and contain 3 * 10 of 0.5mol/L KCl
-4Mol/L K
3[Fe (CN)
6] solution 10mL, add 5 μ L 3 * 10 one by one
-4Mol/L chlortoluron solution, cyclic voltammetry scan; Chlortoluron is 3 * 10
-7~1.5 * 10
-6Be good linear relationship with peak point current i in the mol/L concentration range: i=0.37798C-0.78127, coefficient R=0.9998.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN2009101139792A CN101532987B (en) | 2009-04-11 | 2009-04-11 | Method for measuring chlorotoluron content |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN2009101139792A CN101532987B (en) | 2009-04-11 | 2009-04-11 | Method for measuring chlorotoluron content |
Publications (2)
Publication Number | Publication Date |
---|---|
CN101532987A CN101532987A (en) | 2009-09-16 |
CN101532987B true CN101532987B (en) | 2012-02-15 |
Family
ID=41103717
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN2009101139792A Expired - Fee Related CN101532987B (en) | 2009-04-11 | 2009-04-11 | Method for measuring chlorotoluron content |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN101532987B (en) |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104655614A (en) * | 2013-11-20 | 2015-05-27 | 南京亿特生物科技有限公司 | Chemical-luminescent ELISA method for detecting chlortoluron |
CN103901007A (en) * | 2014-04-16 | 2014-07-02 | 桂林理工大学 | Method for detecting content of chlortoluron in farmland water by using fluorescence carbon point and cadmium telluride quantum dot energy transferring technology |
CN104931689A (en) * | 2015-05-14 | 2015-09-23 | 桂林理工大学 | Molecularly imprinted test paper strip and preparation method as well as application thereof |
CN106525922A (en) * | 2016-09-30 | 2017-03-22 | 江苏大学 | Molecular imprinting modified nickel foam electrode, preparation method and applications thereof |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2005003716A2 (en) * | 2002-09-12 | 2005-01-13 | Polytechnic University | Surface imprinting: integration of molecular recognition and transduction |
TWI252917B (en) * | 2003-01-02 | 2006-04-11 | Tse-Chuan Chou | Recognition of dopamine from neurotransmitters by molecular imprinting sensor |
CN101294926A (en) * | 2008-06-06 | 2008-10-29 | 济南大学 | Production method of molecular engram membrane electrode for detecting endocrine interference in trace amount surroundings and detecting method thereof |
CN101324541A (en) * | 2008-07-18 | 2008-12-17 | 大连理工大学 | Abricycline molecular imprinting polymer membrane electrode and preparation and application thereof |
CN201184874Y (en) * | 2008-05-07 | 2009-01-21 | 济南大学 | Molecular engram membrane electrode for detecting mycotoxins |
CN201188095Y (en) * | 2008-05-07 | 2009-01-28 | 济南大学 | Molecular engram membrane electrode for detecting circumstance incretion interference object |
-
2009
- 2009-04-11 CN CN2009101139792A patent/CN101532987B/en not_active Expired - Fee Related
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2005003716A2 (en) * | 2002-09-12 | 2005-01-13 | Polytechnic University | Surface imprinting: integration of molecular recognition and transduction |
TWI252917B (en) * | 2003-01-02 | 2006-04-11 | Tse-Chuan Chou | Recognition of dopamine from neurotransmitters by molecular imprinting sensor |
CN201184874Y (en) * | 2008-05-07 | 2009-01-21 | 济南大学 | Molecular engram membrane electrode for detecting mycotoxins |
CN201188095Y (en) * | 2008-05-07 | 2009-01-28 | 济南大学 | Molecular engram membrane electrode for detecting circumstance incretion interference object |
CN101294926A (en) * | 2008-06-06 | 2008-10-29 | 济南大学 | Production method of molecular engram membrane electrode for detecting endocrine interference in trace amount surroundings and detecting method thereof |
CN101324541A (en) * | 2008-07-18 | 2008-12-17 | 大连理工大学 | Abricycline molecular imprinting polymer membrane electrode and preparation and application thereof |
Non-Patent Citations (1)
Title |
---|
王金成等.苯基脲类除草剂分子印迹聚合物的.《高等学校化学学报》.2006,第27卷(第7期),1227-1231. * |
Also Published As
Publication number | Publication date |
---|---|
CN101532987A (en) | 2009-09-16 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN107271522B (en) | Electrochemical sensor based on multi-stage porous Cu-BTC material and its application in the detection of pesticide glyphosate | |
CN103926294A (en) | Preparation and application of CS/IL-GR modified bovine serum albumin molecular imprinting electrode | |
Wang et al. | Alternative coulometric signal readout based on a solid-contact ion-selective electrode for detection of nitrate | |
CN102072925A (en) | Stroma moisture and conductivity in situ detector and method for determining salinity | |
CN101532987B (en) | Method for measuring chlorotoluron content | |
Yasri et al. | Chronoamperometric determination of lead ions using PEDOT: PSS modified carbon electrodes | |
CN102706927B (en) | Method for measuring gibberellin in fruits by aid of molecularly imprinted electrochemically modified electrode | |
CN105021679A (en) | Silk-screen printing electrode sensor preparation method based on ionic liquid-multi-wall carbon nano-tube modification | |
CN103940866B (en) | A kind of fast detector of quantitative detection fruits and vegetables Pesticide Residues | |
CN104634843A (en) | Preparation method and application of sensor based on screen-printed carbon electrode | |
CN106556638B (en) | One kind being based on MnO2The electrochemical sensor and the preparation method and application thereof of@Ag core-shell type nano material | |
CN104931554A (en) | Preparation method and application of sensor based on screen-printed carbon electrode | |
CN203216891U (en) | Soil nutrient sensor in solar greenhouse | |
CN103940861B (en) | A kind of method that adopts aptamer visible ray electrode detection incretion interferent | |
CN201974399U (en) | Matrix humidity and conductivity in-situ detector | |
CN102901757A (en) | Sudan I molecular imprinting electrochemical sensor and preparation method thereof | |
CN107121484B (en) | A kind of electrochemical method of Sensitive Detection glyphosate | |
CN103454327B (en) | P3MT/N-GE modified glassy carbon electrode and the application in detection pesticide phoxim | |
CN105259167A (en) | Preparation method and application of molecularly-imprinted electrochemiluminescence sensing material | |
CN104020205B (en) | The imprinted polymer membrane electrode of parachloroanilinum, its preparation method and application process | |
CN104458870A (en) | Heavy metal ion concentration automatic detection system | |
CN103940868B (en) | A kind of rapid detector for pesticide residue based on enzyme immunosensor | |
CN103852642A (en) | Method for detecting electrical conductivity of small number of solids | |
CN101710116B (en) | Method for determining trace terramycin by utilizing molecularly imprinted immunosensor | |
CN103454332B (en) | Electrochemical method used for rapidly detecting imidacloprid serving as pesticide |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
C17 | Cessation of patent right | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120215 Termination date: 20130411 |