CN101576479A - Method for detecting organophosphorus and carbamate pesticide residue - Google Patents
Method for detecting organophosphorus and carbamate pesticide residue Download PDFInfo
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- CN101576479A CN101576479A CNA2008101062565A CN200810106256A CN101576479A CN 101576479 A CN101576479 A CN 101576479A CN A2008101062565 A CNA2008101062565 A CN A2008101062565A CN 200810106256 A CN200810106256 A CN 200810106256A CN 101576479 A CN101576479 A CN 101576479A
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Abstract
The invention discloses a method for detecting organophosphorus and carbamate pesticide residue, which is to determine whether a sample to be tested contains organophosphorus or/and carbamate pesticides according to the suppression ratio of an extracting solution of the sample to be tested on cholinesterase, wherein the suppression ratio of the extracting solution of the sample to be tested on the cholinesterase is determined through the chromatic value of the extracting solution of the sample to be tested. The chromatic value is acquired through digital image processing technology. The method greatly improves detection efficiency, is particularly suitable for the mass detection of vegetable samples, and has the advantages of high automation degree, high measurement accuracy, quick, simple and convenient operation, few needed instruments and equipment, low cost, low requirement on environmental conditions of the determination, and no pollution.
Description
Technical field
The present invention relates to detect the method for organophosphorus and carbamate pesticide residue.
Background technology
At present, detection method at organophosphorus and carbamate chemicals for agriculture mainly contains thin-layered chromatography, vapor-phase chromatography, spectrophotometric method etc., preceding two kinds of accuracy of detection height, can realize the detection by quantitative of every kind of agricultural chemicals, but because trivial operations, the instrument costliness, and need the special messenger to operate, be difficult to satisfy the market demand quick, easy, easy row.The enzyme inhibition rate method is adopted in the detection of organophosphorus and carbamate chemicals for agriculture in standard GB/T 5009.199-2003 regulation food.This method is according to the testing sample extract inhibiting rate of cholinesterase to be determined whether contain organophosphorus or carbamate chemicals for agriculture in the testing sample.The principle of this method is: under the normal condition, cholinesterase catalysis nerve conduction metabolic product (acetylcholine) hydrolysis, its hydrolysate and developer reaction, produce yellow substance, utilize its color to be worth over time, calculate inhibiting rate, can judge the existence whether high dose organophosphorus or carbamate chemicals for agriculture are arranged in the sample by inhibiting rate.This method is highly sensitive, and detection limit can reach 0.05mg/kg.
Though the enzyme inhibition rate method of using in the national standard has very high sensitivity and lower detection limit, and can judge fast whether organophosphorus and carbamate pesticide residue exceed standard in the agricultural product such as vegetables, fruit, but the method for regulation needs before the assaying reaction and the absorbance of reaction after three minutes, this has higher requirement to spectrophotometric operation, otherwise the developing time that will make blank sample and detect sample deviation occurs because of the delay of time, thereby introduces error.This makes this method that certain limitation be arranged in actual applications, can't accurately judge residues of pesticides.
Summary of the invention
The purpose of this invention is to provide the method that detects organophosphorus and carbamate pesticide residue.
Detection organophosphorus provided by the invention and carbamate pesticide residue method, be the inhibiting rate of cholinesterase to be determined whether contain organophosphorus or carbamate chemicals for agriculture in the testing sample according to the testing sample extract, wherein, described testing sample extract is determined by the chromatic value of testing sample extract the inhibiting rate of cholinesterase.
Detection method of the present invention is except that inhibiting rate is determined by the chromatic value of testing sample extract, and other step is all identical with standard GB/T 5009.199-2003.Can judge the existence whether high dose organophosphorus or carbamate chemicals for agriculture are arranged in the sample by inhibiting rate.
Chromatic value can obtain by digital image processing techniques described in the detection method of the present invention, uses common office machine and scanner can carry out Flame Image Process.
Detection method of the present invention replaces absorbance with chromatic value and determines the inhibiting rate of testing sample extract to cholinesterase, utilize common office machine and scanner to replace the exact instrument-spectrophotometer of laboratory special use, can write down the chromatic value of 24 samples simultaneously, the colour developing data (chromatic value) that guaranteed to obtain blank sample simultaneously and detected sample, guaranteed the consistance of testing conditions, avoid in the spectrophotometric method delay because of the time occur the developing the color deviation of data, improved detection efficiency greatly.The method of invention especially is fit to the large batch of detection of vegetable sample, the automaticity height, and the measuring accuracy height operate fast and conveniently, and the instrument and equipment that needs is few, and cost is low, and is low, pollution-free to the environmental baseline requirement of measuring.Be applicable to the existence whether high dose organophosphorus and carbamate chemicals for agriculture are arranged in the quick judgement sample.
Description of drawings
Fig. 1 detects the process flow diagram of software for EIS1.0
Embodiment
Organophosphorus of the present invention and carbamate pesticide residue detection method specifically comprise the steps:
One, the preparation of standard solution:
(1) buffer solution: get 11.9g ADKP and 3.2g potassium dihydrogen phosphate respectively, use the 1000mL dissolved in distilled water, pH8.0.
(2) developer: get 160mg two sulfo-dinitrobenzoic acids and 15.6mg sodium bicarbonate respectively, with the dissolving of 20mL buffer solution.
(3) substrate: use the 25.0mg acetylthiocholine, add the 3.0mL dissolved in distilled water, shake up rearmounted 4 ℃ of refrigerators and preserve standby.
(4) enzyme liquid: according to the active situation of acetylcholinesterase, with the damping fluid dissolving of (1), the absorbance of 3min changes
ΔA
0Value is controlled at more than 0.3, shake up preserve in rearmounted 4 ℃ of refrigerators standby.
Two, sample preparation: choose representational vegetables blade, rinse out surperficial earth, be cut into the square fragment in the 1cm left and right sides, get the fragment of 1g, put into beaker or extraction flask, add 5mL buffer solution, concussion 1min-2min, pour out extract, leave standstill 3min-5min, stand-by.
Three, detect
1, control solution test: prior to adding the buffer solution of 2.5mL above-mentioned steps one in the test tube, add 0.1mL enzyme liquid, 0.1mL developer again, shake up the back and place more than the 15min in 37 ℃; Add the 0.1mL substrate and shake up, put into colorimetric pool immediately; Then can according to following a) or b) step carries out,
A) obtain the chromogenic reaction picture with MICROTEK Phantom K8 type scanner (Shanghai MICROTEK Technology Co. Ltd), utilize photoshop software to obtain the chromatic value of differential responses time on computers, the chromatic value changing value of record reaction 3min
ΔA
0
B) obtain the chromogenic reaction picture with MICROTEK Phantom K8 type scanner (Shanghai MICROTEK Technology Co. Ltd), utilize EIS1.0 to detect software (copyright registration 2007RSBJ3028) and obtain the chromatic value of differential responses time, the chromatic value changing value of record reaction 3min
ΔA
0
Wherein, the process flow diagram that EIS1.0 detects software as shown in Figure 1, its each step is:
1. at first call in the initial chroma picture, under system prompt, carry out the parameter setting, type of detection had two classes during parameter was provided with: the firstth, and inhibiting rate detects, by the statistics chrominance information, calculate corresponding inhibition ratio, need call in this part and just to have begun the picture that reacts and to have reacted back three minutes picture, will not show concrete chromatic value after analyzing, directly return inhibiting rate; The secondth, colorimetric detection is only analyzed a width of cloth picture at every turn, and is not calculated inhibiting rate in this part, just returns and detects the chrominance information in the useful area in the picture, and chrominance information is kept in the txt text automatically;
2. as in parameter is provided with, selecting chrominance information to detect, then this initial chroma picture being carried out chrominance information detects: mouse becomes little square frame, this initial chroma picture is carried out the selection of useful area, utilize histogram and trim button that useful area is revised, add up chrominance information, and it is kept in the txt text;
If 3. selected feature chromatic value and inhibiting rate to detect, then the colourity picture after three minutes is reacted in the prompting input, behind the picture of input reaction after three minutes, mouse becomes little square frame, carry out the selection of useful area this moment, utilize histogram and trim button that useful area is revised, the statistics chrominance information; And calculating inhibiting rate.
2, sample extracting solution test: gained extract 2.5mL in the sample preparation is added in the test tube, and other operations are identical with control solution test, the chromatic value changing value of record reaction 3min
ΔA
t
Four, the result calculates:
Inhibiting rate (%)=[(
ΔA
0-
ΔA
t)/
ΔA
0] * 100
ΔA
0---the changing value of contrast solution reaction 3min chromatic value;
ΔA
t---the changing value of sample solution reaction 3min chromatic value.
Five, the result judges
The result represents with the repressed degree of enzyme (inhibiting rate).
When vegetable sample extract during, contain organophosphorus in the expression vegetables or carbamate chemicals for agriculture exists to the inhibiting rate of enzyme 〉=50%.The sample of inhibiting rate 〉=50% needs duplicate test more than 2 times.
To the sample of inhibiting rate 〉=50%, available other method is further determined concrete pesticide species and content.
Be example in the detection spinach blade whether the method for organophosphorus or carbamate pesticide residue is arranged below, illustrate detection method of the present invention.
The organophosphorus in embodiment 1, the spinach blade and the detection of carbamate pesticide residue
Choose 10 samples, according to the spectrophotometric method and the chromatmetry of the present invention of GB/T 5009.199-2003 defined organophosphorus and carbamate chemicals for agriculture are measured respectively.The result is as shown in table 1, utilizes two kinds of detection methods to detect inhibiting rate and does not have significant difference, and its related coefficient is 0.9975, illustrate that both have higher consistance, and final judged result is in full accord.Utilize chromatmetry of the present invention when obtaining picture, to guarantee the unanimity of developing time, avoided the inconsistent error of introducing owing to sample and blank sample developing time.Operate simplyr, be more suitable for the needs of fast detecting.
Table 1 spectrophotometric method and chromatmetry testing result of the present invention are relatively
T Δ=0.9804＜t0.05 in the table 1,11=2.20 shows that there is not significant difference in the two.
Utilize spectrophotometric method and chromatmetry of the present invention to detect respectively at same sample, the result shows when utilizing spectrophotometric method to detect, there is bigger difference in each testing result, its relative standard deviation is 57.86%, if therefore adopt spectrophotometric method to detect, probably test result of samples made false judgment.Adopt chromatmetry of the present invention to detect, detect inhibiting rate at every turn and be more or less the same, standard deviation is 5.69%, has consistance preferably.
Table 3 spectrophotometric method and chromatmetry testing result relative standard deviation of the present invention are relatively
RSD represents relative standard deviation in the table 3.
Claims (2)
1, detects the method for organophosphorus and carbamate pesticide residue amount, be according to the testing sample extract inhibiting rate of cholinesterase to be determined whether contain organophosphorus in the testing sample or/and carbamate chemicals for agriculture is characterized in that: described testing sample extract is determined by the chromatic value of testing sample extract the inhibiting rate of cholinesterase.
2, detection method according to claim 1 is characterized in that: described chromatic value obtains by Digital Image Processing.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102565044A (en) * | 2011-12-19 | 2012-07-11 | 北京市农林科学院 | Method for detecting pesticide residue by adopting rapid-determination card on basis of image processing |
| CN102692388A (en) * | 2012-06-19 | 2012-09-26 | 中国农业大学 | Digital imaging system and method for rapid detection of organophosphorus pesticide residues in fruits and vegetables by using same |
| CN103421880A (en) * | 2013-08-01 | 2013-12-04 | 中国石油大学(华东) | Detection method of organophosphorus pesticide |
| CN103837529A (en) * | 2014-03-06 | 2014-06-04 | 北京工业大学 | Detection tube for detecting content of hydrogen in water and application of detection tube |
| CN109187386A (en) * | 2018-08-23 | 2019-01-11 | 成都众粒生物科技有限公司 | For detecting gel and its application of Organophosphorus and carbamate pesticides class pesticide concentration |
| CN110343604A (en) * | 2019-07-15 | 2019-10-18 | 浙江大学 | A kind of residual detection chip of micro-fluidic agriculture and application |
| CN111007061A (en) * | 2019-12-24 | 2020-04-14 | 赵莉莉 | Pesticide residue detection method and system |
-
2008
- 2008-05-09 CN CNA2008101062565A patent/CN101576479A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102565044A (en) * | 2011-12-19 | 2012-07-11 | 北京市农林科学院 | Method for detecting pesticide residue by adopting rapid-determination card on basis of image processing |
| CN102565044B (en) * | 2011-12-19 | 2013-11-06 | 北京市农林科学院 | Method for detecting pesticide residue by adopting rapid-determination card on basis of image processing |
| CN102692388A (en) * | 2012-06-19 | 2012-09-26 | 中国农业大学 | Digital imaging system and method for rapid detection of organophosphorus pesticide residues in fruits and vegetables by using same |
| CN102692388B (en) * | 2012-06-19 | 2014-07-16 | 中国农业大学 | Digital imaging system and method for rapid detection of organophosphorus pesticide residues in fruits and vegetables by using same |
| CN103421880A (en) * | 2013-08-01 | 2013-12-04 | 中国石油大学(华东) | Detection method of organophosphorus pesticide |
| CN103421880B (en) * | 2013-08-01 | 2015-08-05 | 中国石油大学(华东) | A kind of On Detection of Organophosphorus Pesticide |
| CN103837529A (en) * | 2014-03-06 | 2014-06-04 | 北京工业大学 | Detection tube for detecting content of hydrogen in water and application of detection tube |
| CN109187386A (en) * | 2018-08-23 | 2019-01-11 | 成都众粒生物科技有限公司 | For detecting gel and its application of Organophosphorus and carbamate pesticides class pesticide concentration |
| CN110343604A (en) * | 2019-07-15 | 2019-10-18 | 浙江大学 | A kind of residual detection chip of micro-fluidic agriculture and application |
| CN111007061A (en) * | 2019-12-24 | 2020-04-14 | 赵莉莉 | Pesticide residue detection method and system |
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