CN102109470A - Method applicable to fast detection of concentration of fenvalerate pesticide - Google Patents

Method applicable to fast detection of concentration of fenvalerate pesticide Download PDF

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Publication number
CN102109470A
CN102109470A CN 201110081171 CN201110081171A CN102109470A CN 102109470 A CN102109470 A CN 102109470A CN 201110081171 CN201110081171 CN 201110081171 CN 201110081171 A CN201110081171 A CN 201110081171A CN 102109470 A CN102109470 A CN 102109470A
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China
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fenvalerate
naoh solution
reaction
enzyme
concentration
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CN 201110081171
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Chinese (zh)
Inventor
赵洁
徐斐
李思超
高武
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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Priority to CN 201110081171 priority Critical patent/CN102109470A/en
Publication of CN102109470A publication Critical patent/CN102109470A/en
Pending legal-status Critical Current

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Abstract

The invention relates to a method applicable to fast detection of the concentration of a fenvalerate pesticide, comprising: a relation curve between initial velocity at which the pesticide is catalyzed to hydrolyze by enzyme, and pesticide content is established as follows: y is equal to 0.0723x plus 0.1393; distilled water is put in an enzyme reactor, the fenvalerate pesticide is added and is magnetically stirred for 5 minutes, and the reaction temperature is controlled at 55 DEG C; then a NaOH solution is added, the pH value is adjusted to be 8.0, and the scale value of a NaOH solution dropper at the moment is recorded as V0 which is used as an initial scale; then 0.1ml enzyme liquid is added, and reaction is started and simultaneously timing is carried out; the pH value in reaction is maintained to be 8.0 all the time; and the reaction is ended after 120 seconds, the final scale V1 of the NaOH solution dropper is recorded, and the dropping amount V is calculated based on the expression that V is equal to V1 minus V0, wherein the dropping speed v of NaOH solution is equal to V/t which is equal to (V1 minus V0)/t; and if y is equal to 1/v, a corresponding value x is found on a y coordinate of the relation curve, and the concentration N of the fenvalerate pesticide is 1/x. In the method disclosed by the invention, convenience and fastness be achieved, the operation is simple and convenient, and the cost is low, the detection time is greatly detected, and the purpose of accurate and fast detection is achieved.

Description

A kind of method for quick that is applicable to the fenvalerate pesticide concentration
Technical field
The present invention relates to a kind of method for quick that is applicable to the fenvalerate pesticide concentration.
Background technology
1, detection agricultural chemicals method commonly used both at home and abroad has high performance liquid chromatography (HPLC), vapor-phase chromatography (GC), gas chromatography-mass spectrography (GC/MS), enzyme analytical technology, thin-layered chromatography (TLC) etc.At present, pyrethroid pesticide detects vapor-phase chromatography and the high performance liquid chromatographies of adopting more, though these two kinds method is highly sensitive, selectivity is strong, can detect pesticide concentration more exactly, but owing to the operation steps complexity, detect length consuming time, apparatus expensive and, can not satisfy the demand of field quick detection shortcomings such as the technician have relatively high expectations.
2, enzyme assay is a kind of detection method that detects the content of respective substance by the mensuration of enzyme reaction rate.Advantage such as that this method has is efficiently single-minded, convenient and swift, simple to operate, save time has broad application prospects.Present domestic report is crossed the method for analyzing enzyme of many detection organophosphoruss and carbamate chemicals for agriculture, but but less relatively to the correlation technique report that detects pyrethroid pesticide.
Summary of the invention
The invention discloses a kind of method for quick that is applicable to the fenvalerate pesticide concentration, its purpose is to overcome the existing method that detects pyrethroid pesticide, vapor-phase chromatographies and the high performance liquid chromatographies of adopting exist the operation steps complexity, detect length consuming time, drawback such as instrument and equipment cost height more; The inventive method is not only convenient and swift, easy and simple to handle, and is with low cost and can reach precisely and the purpose of fast detecting.
A kind of method for quick that is applicable to fenvalerate class pesticide concentration, foundation is with the relation curve y=0.0723x+0.1393 between enzymatic agricultural chemicals hydrolysis initial velocity and the pesticide concentration, wherein x represents the inverse of fenvalerate pesticide concentration, y represents the inverse of enzymatic agricultural chemicals hydrolysis initial velocity, it is characterized in that: by detecting and calculate the y reciprocal of enzymatic agricultural chemicals hydrolysis initial velocity, obtain the x reciprocal of fenvalerate pesticide concentration by relation curve y=0.0723x+0.1393, finally try to achieve the fenvalerate pesticide concentration; Concrete detection step and computing method are as follows:
1) distilled water is placed enzyme reactor, add fenvalerate class agricultural chemicals, magnetic agitation 5 minutes, 55 ℃ of control temperature of reaction;
2) add NaOH solution in the step 1) enzyme reactor, adjust pH to 8.0, the scale value of record NaOH solution this moment minim pipette is V 0As initial scale;
3) to step 2) add 0.1ml enzyme liquid in the enzyme reactor, described enzyme activity is 0.5U/ml, the reaction beginning picks up counting simultaneously;
4) descend 0.1 the time as pH in the step 3) enzyme reactor, reactor is carried out in beginning in it, and pH is constant in always 8.0 when making reaction;
5) stop the termination scale V of record NaOH solution minim pipette behind the reaction 120s 1, and calculate titer V=V 1-V 0
6) obtain droplet fast v=V/t=(V of NaOH solution in 120s 1-V 0)/t;
7) make y=1/v, on the y of relation curve coordinate, find respective value x;
The concentration N=1/x of the fenvalerate agricultural chemicals of 8) being asked.
The principle that this method detects agricultural chemicals is to do substrate with the fenvalerate agricultural chemicals, by the hydrolysis of the esterase catalyzed fenvalerate agricultural chemicals of narrow spectrum chicken gizzard, generates carboxylic acid and alcohols material under alkaline environment, and its principle schematic is:
The hydrolysate carboxylic acid can discharge H +The decline of pH in the system that induces reaction, keep system pH constant with alkali-titration in the course of reaction, levy the initial velocity of agricultural chemicals hydrolysis with the alkali lye scale that reaction unit interval starting stage consumes, by the agricultural chemicals hydrolysis initial velocity of prior foundation and the relation curve between the pesticide concentration, just can quantitatively record fenvalerate class pesticide concentration in the sample, whole testing process is no more than 30 minutes.The invention has the beneficial effects as follows: shortened detection time greatly,, reduced the detection cost, improved the practicality of enzyme assay keeping the result to reduce the complexity of operation accurately simultaneously.
The inventive method is not only convenient and swift, easy and simple to handle, and is with low cost and shorten detection time greatly, promptly reaches the purpose that precisely reaches fast detecting again.
Description of drawings
Fig. 1 is the experimental provision of fast detecting fenvalerate agricultural chemicals of the present invention;
Fig. 2 is the typical curve of fast detecting fenvalerate of the present invention.
1, enzyme reactor, 2, magnetic stirring apparatus, 3, NaOH solution minim pipette, 4, the pH sensor, 5, pH meter, 6, low temperature thermostat bath, 7, stopwatch.
Embodiment
The present invention is described in detail below in conjunction with drawings and Examples.
A kind of method for quick that is applicable to the fenvalerate pesticide concentration, the pick-up unit of its use as shown in Figure 1.Enzyme reactor 1 is positioned on the magnetic stirring apparatus 2, on the top cover of enzyme reactor 1, open two apertures respectively, the top of an aperture is provided with the NaOH solution minim pipette 3 of band scale, the another aperture connects pH sensor 4, one end of sensor inserts liquid, and the other end connects pH meter 5, and the differing heights position is connected with low temperature thermostat bath 6 by pipeline on enzyme reactor 1 wall, constitute constant temperature transmission loop, adopt stopwatch 7 timing.
A kind of method for quick that is applicable to the fenvalerate pesticide concentration, specifically detect step and computing method are as follows:
1) distilled water 20ml is placed 50ml enzyme reactor 1, the fenvalerate standard items that add 0.5ml solute weight and be 1mg/L are for treating sample measuring liquid, 55 ℃ of control temperature of reaction, magnetic stirring apparatus 2 stirrings 5 minutes;
2) add NaOH solution in the step 1) enzyme reactor, adjust pH to 8.0, the scale value of record NaOH solution this moment minim pipette 3 is V 0As initial scale;
3) to step 2) add the chicken gizzard esterase liquid 0.1ml of the 0.5U/ml that has diluted in the enzyme reactor, the reaction beginning, stopwatch 7 picks up counting simultaneously;
4) descend 0.1 the time as pH in the step 3) enzyme reactor, begin to drip enzyme reactor fast with the NaOH standard solution, pH is constant in always 8.0 when making reaction;
5) stop the termination scale V of record NaOH solution minim pipette 3 behind the reaction 120s 1, and calculate titer V=V 1-V 0
6) obtain droplet fast v=V/t=(V of NaOH solution in 120s 1-V 0)/t;
8) make y=1/v, contrast Fig. 2 finds respective value x on the y of relation curve coordinate;
The concentration N=1/x=0.93mg/L of the fenvalerate agricultural chemicals of 9) being asked, the omnidistance time spent is no more than 30 minutes.

Claims (1)

1. method for quick that is applicable to the fenvalerate pesticide concentration, foundation is with the relation curve y=0.0723x+0.1393 between enzymatic agricultural chemicals hydrolysis initial velocity and the pesticide concentration, wherein x represents the inverse of fenvalerate pesticide concentration, y represents the inverse of enzymatic agricultural chemicals hydrolysis initial velocity, it is characterized in that: by detecting and calculate the y reciprocal of enzymatic agricultural chemicals hydrolysis initial velocity, obtain the x reciprocal of fenvalerate pesticide concentration by relation curve y=0.0723x+0.1393, finally try to achieve the fenvalerate pesticide concentration; Concrete detection step and computing method are as follows:
1) distilled water is placed enzyme reactor, add fenvalerate class agricultural chemicals, magnetic agitation 5 minutes, 55 ℃ of control temperature of reaction;
2) add NaOH solution in the step 1) enzyme reactor, adjust pH to 8.0, the scale value of record NaOH solution this moment minim pipette is V 0As initial scale;
3) to step 2) add 0.1ml enzyme liquid in the enzyme reactor, described enzyme activity is 0.5U/ml, the reaction beginning picks up counting simultaneously;
4) descend 0.1 the time as pH in the step 3) enzyme reactor, reactor is carried out in beginning in it, and pH is constant in always 8.0 when making reaction;
5) stop the termination scale V of record NaOH solution minim pipette behind the reaction 120s 1, and calculate titer V=V 1-V 0
6) obtain droplet fast v=V/t=(V of NaOH solution in 120s 1-V 0)/t;
7) make y=1/v, on the y of relation curve coordinate, find respective value x;
The concentration N=1/x of the fenvalerate agricultural chemicals of 8) being asked.
CN 201110081171 2011-03-31 2011-03-31 Method applicable to fast detection of concentration of fenvalerate pesticide Pending CN102109470A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102492617A (en) * 2011-11-22 2012-06-13 上海理工大学 Device suitable for enzyme method to rapidly detect concentration of fenvalerate pesticides in food

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1624480A (en) * 2004-10-20 2005-06-08 扬州大学 Fenvalerate direct competition enzyme joint immune absorption analysis technology and its kit
CN101650343A (en) * 2008-12-15 2010-02-17 河南工程学院 Rapid detection of pyrethroid pesticide in water

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1624480A (en) * 2004-10-20 2005-06-08 扬州大学 Fenvalerate direct competition enzyme joint immune absorption analysis technology and its kit
CN101650343A (en) * 2008-12-15 2010-02-17 河南工程学院 Rapid detection of pyrethroid pesticide in water

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
《东北农业大学学报》 20110225 李思超等 鸡肝酯酶快速检测氰戊菊酯农药的试验研究 10-15 1 第42卷, 第02期 2 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102492617A (en) * 2011-11-22 2012-06-13 上海理工大学 Device suitable for enzyme method to rapidly detect concentration of fenvalerate pesticides in food

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Inventor after: Xu Fei

Inventor after: Zhao Jie

Inventor after: Li Sichao

Inventor after: Cao Hui

Inventor after: Yu Jinsong

Inventor after: Gao Wu

Inventor before: Zhao Jie

Inventor before: Xu Fei

Inventor before: Li Sichao

Inventor before: Gao Wu

COR Change of bibliographic data

Free format text: CORRECT: INVENTOR; FROM: ZHAO JIE XU FEI LI SICHAO GAO WU TO: XU FEI ZHAO JIE LI SICHAO CAO HUI YU JINSONG GAO WU

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Application publication date: 20110629