CN104596968A - Method for rapidly and quantitatively detecting omethoate residue - Google Patents
Method for rapidly and quantitatively detecting omethoate residue Download PDFInfo
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Abstract
The invention relates to a method for rapidly and quantitatively detecting omethoate residue. According to the present invention, the characteristic that the omethoate aqueous solution presents the stable absorption peak at the specific ultraviolet wavelength is utilized to establish the method, wherein the omethoate content is proportional to the absorbance value and the proportional change trend is presented in the coordinate system so as to establish the standard curve, and the detected absorbance mean value of the detected sample is substituted into the regression equation so as to calculate the omethoate content in the sample, such that the purpose of the rapid and quantitative omethoate residue detection is achieved.
Description
Technical field
The invention belongs to drug measurement techniques field, be specifically related to a kind of method that Quantitative detection flolimat is residual.
Background technology
In recent years, organophosphorus pesticide (organophosphorus pesticides, Ops), owing to having the features such as efficient and use cost is low, plays an important role in world agriculture, is one of main pesticide.Organophosphorus pesticide belongs to middle and high toxicity agricultural chemicals, has interior drug resistance, and residual quantity is large in the environment, most of difficult degradation, while protection crops, also causes the severe contamination of environment, and directly or indirectly jeopardizes health.Flolimat belongs to one most widely used, maximum in organophosphorus pesticide, its advantage the same as other organophosphorus pesticides and depositing the while of harm: flolimat adopts high concentration to fill with root dispenser namely to cause soil pollution, contaminated soil flows in river through rain drop erosion again, causes water pollutions; When preventing and treating surface crops insect, the method dispenser of usual employing stem brush or sprinkling, medicine is by the stem of plant, leaf inspiration plant body, while kill pests, cause flolimat to remain in a large number in plant, produce toxic action by food chain, Timeliness coverage and detection flolimat remain has very important practical significance.In recent years, get more and more to the research that organophosphorus pesticide detects, handy root canal preparation is also constantly updated, and common method mainly contains spectral method, chromatography and inhibiting AChE.Spectral method sensitivity is not high, general is only used for roughly selecting as discrimination method qualitatively; Chromatography detects the main detection method of organophosphorus pesticide at present, be divided into again vapor-phase chromatography, thin-layered chromatography and high performance liquid chromatography three class, vapor-phase chromatography is after entering the 50's of 20th century, a kind of novel instrument analytical method that the basis of column chromatography grows up is analytical approach most widely used at present; The sensitivity that thin-layered chromatography is analyzed, the restriction of difficult quantitation, apply less; Liquid phase chromatography, compared with vapor-phase chromatography, not by the volatile grade of sample and the restriction of thermal stability, is suitable for the analysis of large molecule, unstable compound, but its speed, sensitivity and convenient in not as vapor-phase chromatography, and expend to exceed a lot.Vapor-phase chromatography is when analyzing organophosphorus pesticide, utilize different organophosphorus pesticides to be separated in Stationary liquid, detect scanning through different detecting devices and draw gas chromatogram, come qualitative by retention time, come quantitatively by peak height or peak area and standard curve control, the service condition of gas chromatograph requires high, require strict to environment for use and operating conditions, user of service will through special training, complex operation, front left and right reason is cumbersome, and length consuming time, does not have specific equipment and condition cannot realize detecting fast, quantitatively.Inhibiting AChE utilizes organophosphorus pesticide to have the effect suppressing cholinesterase activity, thus affect the reaction that acetylcholine or BuCh produce choline, acetic acid or butyric acid under cholinesterase effect, decomposition product acetic acid or butyric acid are reduced, thus according to the change of indicator color or reactant liquor pH value, reach the object detecting organophosphorus pesticide.AOAC disclosed the method the earliest and detects organophosphorus pesticide in 1964; The midwest research institute (MidwestResearch Institute) of the U.S., in the Pesticides Testing enzyme sheet (Enzyme Ticket) of report in 1985, can measure 0. 1 ~ 10 ng/L organophosphorus (OPS) or carbamates chemicals for agriculture in water; The auspicious grade of Inst. of Environment Protection & Scientific Research Monitor, Ministry of Agric of China Li Zhi have also been made similar report in 1989.National Standard of the People's Republic of China GB/the T18630-2002 newly promulgated for 2002 is using the simple and easy method of inspection of inhibiting AChE as organophosphorus in vegetables and carbamate chemicals residual amount.Current inhibiting AChE mainly contains film-electrode method and paper disk method, specifically acetylcholine (AchE) is adsorbed on carrier (electrode or the scraps of paper), when running into organophosphorus pesticide, acetylcholine (AchE) activity inhibited, the reading instruction change of electrode or the color change of the scraps of paper can qualitative detection organophosphorus pesticides.The advantage of inhibiting AChE is easy and simple to handle, speed is fast, do not need expensive instrument, be applicable to the selective mechanisms of Site Detection and gross sample, the left and right of deficiency is that degree of accuracy is low, repeatability, the recovery need to improve, and this method is only limitted to the qualitative detection of veterinary antibiotics and foodstuff organophosphorus pesticide, and quick, quantitative detection yet there are no application.
More existing technical research report shows, containing P=O or P=S double bond structure in organophosphorus pesticide molecule, this architectural feature shows the characteristic showing stable absorption peak value under ultraviolet specific wavelength, this characteristic is only for the qualitative detection of different organophosphorus pesticide, utilize this characteristic, it is feasible for carrying out quantitatively detecting to organophosphorus pesticide, but this type of technology is so far there are no report.
Summary of the invention
The object of this invention is to provide a kind of method that Quantitative detection flolimat is residual.
The characteristic that method of the present invention utilizes contained P=O double bond structure in flolimat molecule to show stable absorption peak value under ultraviolet specific wavelength is set up, with ultraviolet spectrophotometer, flolimat aqueous solution is measured, it shows maximum stable absorption peak value at ultraviolet wavelength 210nm place, peak value figure is shown in accompanying drawing, the flolimat aqueous solution of variable concentrations is directly proportional to the size of its absorbance, the two presents direct proportion variation tendency in a coordinate system, take concentration as horizontal ordinate, with the absorbance of its correspondence for ordinate drawing standard curve, namely regression equation is tried to achieve, measure and calculation goes out the flolimat content of measuring samples according to this, concrete steps are as follows:
Step one, prepares the standard aqueous solution of different flolimat final concentration: get flolimat standard solution, is 0 as benchmark with flolimat final concentration, and the concentration gradient according to 0.5 or 1.0 prepares the standard aqueous solution of one group of different flolimat final concentration;
Step 2, the making of typical curve: the standard aqueous solution getting the different flolimat final concentrations that step one is prepared take flolimat final concentration as the standard aqueous solution of 0 is blank, respective absorbance is recorded respectively with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeats to do three times, asks its mean value, with different final concentration for horizontal ordinate, with the absorbance values of its correspondence for ordinate, drawing standard curve, tries to achieve regression equation Y=aX+b(b=0), a, b are constant;
Step 3, the mensuration of contaminated samples: the aqueous solution of getting contaminated samples take flolimat final concentration as the standard aqueous solution of 0 is blank, measure the absorbance of contaminated samples with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeats to do three times, tries to achieve mean value;
Step 4, result calculates: the mean value of step 3 being tried to achieve substitutes into regression equation Y=aX+b(b=0), calculate the content of contaminated samples flolimat.
This method is determined as follows flolimat content in flolimat contaminated soil, water, leaf vegetables:
The mensuration of flolimat content in flolimat contaminated soil
Pedotheque is treated to: the soil sample soil sample of oxygen-freeization Rogor and flolimat polluted via air-dry, grinding, the process of crossing 100 mesh sieves, obtains blank soil sample and pollutes soil sample respectively.
Determination step is:
Step one, prepare the soil sample supernatant of different flolimat final concentration: the triangular flask getting 6 50mL, respectively add the blank soil sample of 0.50g, according to the concentration gradient of 1.0, add respectively flolimat standard solution make its blank soil sample be respectively 0 containing the final concentration of flolimat, 1.0,2.0,3.0,4.0,5.0g/kg soil, then 10mL deionized water is added respectively, shaking table concussion 30min, place 30min, put centrifugal 10 min of hydro-extractor 6000r/min, get supernatant, the soil sample supernatant of obtained different flolimat final concentration;
Step 2, the making of typical curve: the soil sample supernatant being 0.0g/kg soil with flolimat final concentration in step one is for blank, the absorbance of soil sample supernatant is measured respectively with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeats to do three times, tries to achieve respective absorbance values, with different final concentration for horizontal ordinate, with the absorbance values of its correspondence for ordinate, drawing standard curve, tries to achieve regression equation Y
soil=aX+b(b=0), a, b are constant;
Step 3, pollute the mensuration of soil sample supernatant: accurately take 0.50g and pollute soil sample in 50mL triangular flask, add 10mL deionized water, shaking table concussion 30min, place 30min, put the centrifugal 10min of hydro-extractor 6000r/min, get supernatant and must pollute soil sample supernatant, be that the soil sample supernatant of 0.0 g/kg soil is for blank with flolimat final concentration in step one, its absorbance is measured with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeats to do three times, tries to achieve the absorbance values polluting soil sample supernatant;
Step 4, result calculates: the absorbance values of step 3 gained is substituted into regression equation Y
soil=a
soilx+b(b=0), the content polluting soil sample flolimat is calculated.
The mensuration of flolimat content in flolimat contaminant water
Step one, prepare the standard aqueous solution of different flolimat final concentration: get 6 test tubes, respectively add 10ml deionized water, according to the concentration gradient of 0.5, add flolimat standard solution respectively, make flolimat final concentration be respectively 0.0,0.5,1.0,1.5,2.0, the standard aqueous solution of 2.5mg/L;
Step 2, the making of typical curve: the standard aqueous solution being 0.0mg/L with flolimat final concentration in step one is blank, respective absorbance is recorded respectively with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeats to do three times, asks its mean value, with different final concentration for horizontal ordinate, with the absorbance values of its correspondence for ordinate, drawing standard curve, tries to achieve regression equation Y
water=a
waterx+b(b=0);
Step 3, the mensuration of pollution water sample: pollution water sample is adjusted PH to 6.5, getting 5ml adds in vitro, the standard aqueous solution being 0.0mg/L with flolimat final concentration is blank, its absorbance is measured with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeats to do three times, tries to achieve the absorbance values of pollution water sample;
Step 4, result calculates: the absorbance values of step 3 being tried to achieve substitutes into regression equation Y
water=a
waterx+b(b=0), the content of pollution water sample flolimat is calculated.
Flolimat pollutes the mensuration of flolimat content in leaf vegetables
The process of leaf vegetables sample is: by blank leaf vegetables sample with pollute leaf vegetables sample respectively through slitting, squeezes the juice, centrifugal after dilute 10 times, gets supernatant, obtained blank leaf vegetables supernatant and pollution leaf vegetables supernatant.
Determination step is:
Step one, prepare the leaf vegetables supernatant of different flolimat final concentration: get 6 test tubes, respectively add the blank leaf vegetables supernatant of 5ml, according to the concentration gradient of 0.5, adding flolimat standard solution makes its final concentration be respectively 0.0,0.1,0.5,1.0,1.5,2.0 mg/L, oscillator concussion 5min, static 10min, obtain the leaf vegetables supernatant of 6 different flolimat final concentrations;
Step 2, the making of typical curve: the leaf vegetables supernatant being 0.0mg/L with flolimat final concentration in step one is blank, the absorbance of the leaf vegetables supernatant of different flolimat final concentration is recorded respectively with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeats to do three times, asks its mean value, take final concentration as horizontal ordinate, with the absorbance values of its correspondence for ordinate, drawing standard curve, tries to achieve regression equation Y
leaf vegetables=a
leaf vegetablesx+b(b=0), a, b are constant;
Step 3, pollute the mensuration of leaf vegetables supernatant: get pollution leaf vegetables supernatant 5ml and add people in vitro, the leaf vegetables supernatant being 0.0mg/L with flolimat final concentration in step one is blank, its absorbance is measured with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeat to do three times, try to achieve the absorbance values polluting leaf vegetables supernatant;
Step 4, result calculates: the absorbance values of the pollution leaf vegetables supernatant of step 3 being tried to achieve substitutes into regression equation Y
leaf vegetables=a
leaf vegetablesx+b(b=0), the content polluting flolimat in leaf vegetables is calculated.
The repeatability of this method and Stability Determination: with the flolimat standard items aqueous solution of 5.0mg/L and 10.0mg/L for determination object, respectively by this method simultaneously METHOD FOR CONTINUOUS DETERMINATION 10 times, and survey 10 days continuously, replicate determination every day 2 times, calculate its variation within batch coefficient and interassay coefficient of variation is respectively 1.45% and 2.83%, display has good repeatability and stability.
The determination of recovery rates of this method: pollute in soil sample supernatant at flolimat and add 1.0mg/L flolimat standard items, detect by this method, in triplicate, detect the absorbance values obtained, calculate its sample TIANZHU XINGNAO Capsul and all reach more than 95%, result vapor-phase chromatography detection validation, coincidence rate is more than 90%.
This method requires that the mensuration at every turn or often criticized all will do typical curve simultaneously, to obtain respective standard equation, obtains result accurately according to this.
The inventive method has easy and simple to handle compared with the conventional method, and speed is fast, and cost is low, metrical error is little, highly sensitive, reproducible, recovery advantages of higher, this method does not need chemical reagent and expensive instrument, and be suitable for the detection of large batch of sample and several samples, variation within batch coefficient and interassay coefficient of variation are respectively 1.45% and 2.83%, there is good repeatability and stability, sample TIANZHU XINGNAO Capsul all reaches more than 95%, and result vapor-phase chromatography detection validation, coincidence rate is more than 90%.This method is easy to popularize, for agriculture quality testing department and technical research personnel provide conveniently detection means, except the flolimat contaminated soil described except this method, the detection of water and Chinese cabbage, other flolimat contaminated samples, after eliminating the factor affecting ultraviolet spectrophotometry result, also can be applied this method and carry out the residual quantitative detection of flolimat.
Accompanying drawing explanation
Fig. 1 be flolimat aqueous solution in the mensuration of ultraviolet spectrophotometer, in the peak value figure of the maximum stable absorption peak value of wavelength 210nm place display.
Embodiment
embodiment 1the detection of certain suburbs insecticide factory flolimat contaminated soil
Pedotheque process: get free of contamination pedotheque and suburbs insecticide factory flolimat contaminated soil sample respectively through air-dry, crosses 100 mesh sieves after grinding, the carclazyte sample and pollute soil sample of having leisure.
Determination step is:
Step one, prepare the soil sample supernatant of different flolimat final concentration: the triangular flask getting 6 50mL, respectively add the blank soil sample of 0.50g, according to the concentration gradient of 1.0, add respectively flolimat standard solution make its blank soil sample be respectively 0 containing the final concentration of flolimat, 1.0,2.0,3.0,4.0,5.0g/kg soil, then 10mL deionized water is added respectively, shaking table concussion 30min, place 30min, put centrifugal 10 min of hydro-extractor 6000r/min, get supernatant, the soil sample supernatant of obtained different flolimat final concentration;
Step 2, the making of typical curve: the soil sample supernatant being 0.0g/kg soil with flolimat final concentration in step one is for blank, the absorbance of the soil sample supernatant of different flolimat final concentration is recorded respectively with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeats to do three times, asks its mean value, with different final concentration for horizontal ordinate, with the absorbance values of its correspondence for ordinate, drawing standard curve, tries to achieve regression equation Y
soil=0.3053X+b(b=0);
Step 3, pollute the mensuration of soil sample supernatant: accurately take 0.50g and pollute soil sample in 50mL triangular flask, add 10mL deionized water, shaking table concussion 30min, place 30min, put the centrifugal 10min of hydro-extractor 6000r/min, get supernatant and must pollute soil sample supernatant, be that the soil sample supernatant of 0.0 g/kg soil is for blank with flolimat final concentration, its absorbance is measured with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeats to do three times, and trying to achieve the absorbance values polluting soil sample supernatant is 0.105;
Step 4, result calculates: the absorbance values 0.105 of pollution soil sample supernatant step 3 recorded substitutes into regression equation Y
soil=0.3053X+ b(b=0), calculating the content polluting soil sample flolimat is 0.3439g/kg soil.
embodiment 2the mensuration of flolimat content in insecticide factory of Yu Dongmou county trench drain flolimat contaminant water
Step one, prepare the standard aqueous solution of different flolimat final concentration: get 6 test tubes, respectively add 10ml deionized water, according to the concentration gradient of 0.5, add flolimat standard solution respectively, make flolimat final concentration be respectively 0.0,0.5,1.0,1.5,2.0, the standard aqueous solution of 2.5mg/L;
Step 2, the making of typical curve: the standard aqueous solution being 0.0mg/L with flolimat final concentration in step one is blank, respective absorbance is recorded respectively with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeats to do three times, asks its mean value, with different final concentration for horizontal ordinate, with the absorbance values of its correspondence for ordinate, drawing standard curve, tries to achieve regression equation Y
water=0.0272X+b(b=0);
Step 3, the mensuration of pollution water sample: the pollution water sample in insecticide factory trench drain is adjusted PH to 6.5, getting 5ml adds in vitro, the standard aqueous solution being 0.0mg/L with flolimat final concentration is blank, its absorbance is measured with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeats to do three times, and the absorbance values of trying to achieve pollution water sample is 0.386;
Step 4, result calculates: the absorbance values 0.386 of the pollution water sample of step 3 being tried to achieve substitutes into regression equation Y
water=0.0272X+b(b=0), the content calculating pollution water sample flolimat in insecticide factory trench drain is 14.191mg/L.
embodiment 3the mensuration of flolimat content in the Chinese cabbage that vegetable garden, east, palpus region of rivers and lakes flolimat pollutes
Cabbage samples process: the Chinese cabbage slitting respectively getting free of contamination Chinese cabbage and the flolimat pollution of vegetable garden, east, the palpus region of rivers and lakes, squeezes the juice, centrifugal after diluting 10 times, gets supernatant and obtains blank Chinese cabbage supernatant and pollution Chinese cabbage supernatant.
Determination step is:
Step one, prepare the Chinese cabbage supernatant of different flolimat final concentration: get 6 test tubes, respectively add the blank Chinese cabbage supernatant of 5ml, according to the concentration gradient of 0.5, adding flolimat standard solution makes its final concentration be respectively 0.0,0.1,0.5,1.0,1.5,2.0 mg/L, oscillator concussion 5min, static 10min, obtain the Chinese cabbage supernatant of 6 different flolimat final concentrations;
Step 2, the making of typical curve: the Chinese cabbage supernatant being 0.0mg/L with flolimat final concentration in step one is blank, the absorbance of the Chinese cabbage supernatant of different flolimat final concentration is recorded respectively with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeats to do three times, asks its mean value, take final concentration as horizontal ordinate, with the absorbance values of its correspondence for ordinate, drawing standard curve, tries to achieve regression equation Y
leaf vegetables=0.0034X+b(b=0);
Step 3, pollute the mensuration of Chinese cabbage supernatant: get pollution Chinese cabbage supernatant 5ml and add people in vitro, be that the Chinese cabbage supernatant of 0.0 mg/L is for blank with flolimat final concentration in step one, its absorbance is measured with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeat to do three times, trying to achieve the absorbance values polluting Chinese cabbage supernatant is 0.097;
Step 4, result calculates: the absorbance values 0.097 of the pollution Chinese cabbage supernatant of step 3 being tried to achieve substitutes into regression equation Y
leaf vegetables=0.0034X+b(b=0), calculating the content polluting Chinese cabbage flolimat is 28.5294mg/L.
Claims (7)
1. the method that Quantitative detection flolimat is residual, it is characterized in that the characteristic that this method utilizes contained P=O double bond structure in flolimat molecule to show stable absorption peak value under ultraviolet specific wavelength is set up, concrete steps are as follows:
Step one, prepares the standard aqueous solution of different flolimat final concentration: get flolimat standard solution, is 0 as benchmark with flolimat final concentration, and the concentration gradient according to 0.5 or 1.0 prepares the standard aqueous solution of one group of different flolimat final concentration;
Step 2, the making of typical curve: the standard aqueous solution getting the different flolimat final concentrations that step one is prepared take flolimat final concentration as the standard aqueous solution of 0 is blank, respective absorbance is recorded respectively with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeats to do three times, asks its mean value, with different final concentration for horizontal ordinate, with the absorbance values of its correspondence for ordinate, drawing standard curve, tries to achieve regression equation Y=aX+b(b=0), a, b are constant;
Step 3, the mensuration of contaminated samples: the aqueous solution of getting contaminated samples take flolimat final concentration as the standard aqueous solution of 0 is blank, measure the absorbance of contaminated samples with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeats to do three times, tries to achieve mean value;
Step 4, result calculates: the mean value of step 3 being tried to achieve substitutes into regression equation Y=aX+b(b=0), calculate the content of contaminated samples flolimat.
2. the method that a kind of Quantitative detection flolimat as claimed in claim 1 is residual, it is characterized in that the sample that flolimat described in step 3 pollutes is soil, the process of pedotheque is: the soil sample soil sample of oxygen-freeization Rogor and flolimat polluted via air-dry, grinding, the process of crossing 100 mesh sieves, obtains blank soil sample and pollutes soil sample respectively.
3. the method that a kind of Quantitative detection flolimat as claimed in claim 2 is residual, is characterized in that determination step is:
Step one, prepare the soil sample supernatant of different flolimat final concentration: the triangular flask getting 6 50mL, respectively add the blank soil sample of 0.50g, according to the concentration gradient of 1.0, add respectively flolimat standard solution make its blank soil sample be respectively 0 containing the final concentration of flolimat, 1.0,2.0,3.0,4.0,5.0g/kg soil, then 10mL deionized water is added respectively, shaking table concussion 30min, place 30min, put centrifugal 10 min of hydro-extractor 6000r/min, get supernatant, the soil sample supernatant of obtained 6 bottles of different flolimat final concentrations;
Step 2, the making of typical curve: the soil sample supernatant being 0.0g/kg soil with flolimat final concentration in step one is for blank, the absorbance of the soil sample supernatant that step one is prepared is measured respectively with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeats to do three times, tries to achieve respective absorbance values, with different final concentration for horizontal ordinate, with the absorbance values of its correspondence for ordinate, drawing standard curve, tries to achieve regression equation Y
soil=aX+b(b=0), a, b are constant;
Step 3, pollute the mensuration of soil sample supernatant: accurately take 0.50g and pollute soil sample in 50mL triangular flask, add 10mL deionized water, shaking table concussion 30min, place 30min, put the centrifugal 10min of hydro-extractor 6000r/min, get supernatant and must pollute soil sample supernatant, be that the soil sample supernatant of 0.0 g/kg soil is for blank with flolimat final concentration in step one, its absorbance is measured with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeats to do three times, tries to achieve the absorbance values polluting soil sample supernatant;
Step 4, result calculates: the absorbance values of the pollution soil sample supernatant of step 3 gained is substituted into regression equation Y
soil=a
soilx+b(b=0), the content polluting soil sample flolimat is calculated.
4. the method that a kind of Quantitative detection flolimat as claimed in claim 1 is residual, is characterized in that the sample that flolimat described in step 3 pollutes is the water that flolimat pollutes:
Step one, prepare the standard aqueous solution of different flolimat final concentration: get 6 test tubes, respectively add 10ml deionized water, according to the concentration gradient of 0.5, add flolimat standard solution respectively, make flolimat final concentration be respectively 0.0,0.5,1.0,1.5,2.0, the standard aqueous solution of 2.5mg/L;
Step 2, the making of typical curve: the standard aqueous solution being 0.0mg/L with flolimat final concentration in step one is blank, respective absorbance is recorded respectively with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeats to do three times, asks its mean value, with different final concentration for horizontal ordinate, with the absorbance values of its correspondence for ordinate, drawing standard curve, tries to achieve regression equation Y
water=a
waterx+b(b=0);
Step 3, the mensuration of pollution water sample: pollution water sample is adjusted PH to 6.5, getting 5ml pollution water sample enters in vitro, the standard aqueous solution being 0.0mg/L with flolimat final concentration is blank, its absorbance is measured with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeats to do three times, tries to achieve the absorbance values of pollution water sample;
Step 4, result calculates: the absorbance values of the pollution water sample of step 3 being tried to achieve substitutes into regression equation Y
water=a
waterx+b(b=0), the content of pollution water sample flolimat is calculated.
5. the method that a kind of Quantitative detection flolimat as claimed in claim 1 is residual, it is characterized in that the sample that flolimat described in step 3 pollutes is leaf vegetables, the process of leaf vegetables sample is: by blank leaf vegetables sample with pollute leaf vegetables sample respectively through slitting, squeeze the juice, centrifugal after diluting 10 times, get supernatant and obtain blank leaf vegetables supernatant and pollute leaf vegetables supernatant.
6. the method that a kind of Quantitative detection flolimat as claimed in claim 5 is residual, is characterized in that determination step is:
Step one, prepare the leaf vegetables supernatant of different flolimat final concentration: get 6 test tubes, respectively add the blank leaf vegetables supernatant of 5ml, according to the concentration gradient of 0.5, adding flolimat standard solution makes its final concentration be respectively 0.0,0.1,0.5,1.0,1.5,2.0 mg/L, oscillator concussion 5min, static 10min, obtain the leaf vegetables supernatant of 6 different flolimat final concentrations;
Step 2, the making of typical curve: the leaf vegetables supernatant being 0.0mg/L with flolimat final concentration in step one is blank, the absorbance of the leaf vegetables supernatant of different flolimat final concentration is recorded respectively with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeats to do three times, asks its mean value, take final concentration as horizontal ordinate, with the absorbance values of its correspondence for ordinate, drawing standard curve, tries to achieve regression equation Y
leaf vegetables=a
leaf vegetablesx+b(b=0), a, b are constant;
Step 3, pollute the mensuration of leaf vegetables supernatant: get pollution leaf vegetables supernatant 5ml and add people in vitro, the leaf vegetables supernatant being 0.0mg/L with flolimat final concentration in step one is blank, its absorbance is measured with ultraviolet spectrophotometer, ultraviolet wavelength 210nm, repeat to do three times, try to achieve the absorbance values polluting leaf vegetables supernatant;
Step 4, result calculates: the absorbance values of the pollution leaf vegetables supernatant of step 3 being tried to achieve substitutes into regression equation Y
leaf vegetables=a
leaf vegetablesx+b(b=0), the content polluting flolimat in leaf vegetables is calculated.
7. the method that a kind of Quantitative detection flolimat as claimed in claim 5 is residual, is characterized in that described leaf vegetables sample is Chinese cabbage.
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| CN106596442A (en) * | 2015-10-15 | 2017-04-26 | 江苏维赛科技生物发展有限公司 | Method for rapidly and quantitatively detecting phorate residue |
| CN107561069A (en) * | 2017-08-28 | 2018-01-09 | 贵州大学 | A kind of method of the distinguishable colorimetric detection Rogor of naked eyes |
| CN107607484A (en) * | 2017-10-25 | 2018-01-19 | 天津市环境保护科学研究院 | The method of thimet content in quick measure soil |
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| CN109752335A (en) * | 2017-11-02 | 2019-05-14 | 镇江亿特生物科技发展有限公司 | A kind of remaining method of rapid quantitative detection sulfaquinoxaline |
| CN110186914A (en) * | 2018-08-08 | 2019-08-30 | 珠海市慧康生物科技有限公司 | A kind of fruit press and Fast Determination of Pesticide Residue all-in-one machine and detection method |
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