CN110879267A - Method for analyzing dynamic degradation of acephate and metabolite methamidophos in leaf vegetables - Google Patents
Method for analyzing dynamic degradation of acephate and metabolite methamidophos in leaf vegetables Download PDFInfo
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Abstract
The invention provides a dynamic degradation analysis method of acephate and metabolite methamidophos in leaf vegetables, which comprises the following steps: test layout, acephate application, sample extraction, blank standard solution preparation, drawing of an acephate standard solution curve and a methamidophos standard solution curve, determination of relative standard deviation and detection of the concentration of acephate and methamidophos in leaf vegetables. The method for analyzing the dynamic degradation of acephate and metabolite methamidophos in leaf vegetables analyzes the degradation rule and main influence factors of acephate and metabolite methamidophos in leaf vegetables, thereby providing scientific basis for reasonably using acephate, avoiding residual phytotoxicity on sensitive crops of later crops and determining the planting time of leaf vegetables.
Description
Technical Field
The invention relates to the field of pesticide detection, in particular to a dynamic degradation analysis method of acephate and metabolite methamidophos in leaf vegetables.
Background
Acephate is a systemic low-toxicity insecticide, has stomach toxicity and contact killing effects, can kill eggs, has a certain fumigating effect, has a broad insecticidal spectrum, can control more than 100 pests, has high pesticide effect and moderate persistent period, and is suitable for controlling the pests of crops such as grains, leaf vegetables, fruit trees and the like. The acephate is an acetylation product of methamidophos, the toxicity of the acephate is more than 30 times lower than that of the methamidophos, and the half-life period of the acephate in plant tissues is 5-10 days.
Methamidophos is a high-toxicity organophosphorus insecticide with wide insecticidal spectrum, good insecticidal effect, low use cost and slow resistance development. Because of its high toxicity, it is easy to cause pollution to agricultural products and harm to human and animal safety, and has been banned. Currently, methamidophos has been replaced by acephate, of which 30%, 40% of acephate emulsifiable concentrate is used for field leaf vegetables. Because acephate is an acetylation product of methamidophos, a small amount of methamidophos exists in the preparation, and the acemidophos can be metabolized to form the methamidophos in the degradation process, and the methamidophos is a high-toxicity pesticide which is not allowed to be used and detected on leaf vegetables.
In recent years, in the detection and supervision of leaf vegetable pesticide residues, the overproof methamidophos residues in leaf vegetables still occur at times, the situation that both acephate and methamidophos simultaneously overproof occurs, and finally law enforcement can only process the overproof methamidophos, so that whether the phenomenon that the acemidophos is illegally used exists in the leaf vegetables to which the acemidophos is applied is difficult to identify. In the current research situation at home and abroad, under the condition that acephate and methamidophos are detected or exceed standards simultaneously, whether all the acephate is used cannot be judged, and great difficulty is brought to quality safety supervision and law enforcement of agricultural products.
Disclosure of Invention
The invention provides a dynamic degradation analysis method of acephate and metabolite methamidophos in leaf vegetables, which analyzes the degradation rule and main influence factors of acephate and metabolite methamidophos in leaf vegetables, thereby providing scientific basis for reasonably using acephate, avoiding residual phytotoxicity on sensitive crops of next crop and determining the planting time of leaf vegetables.
The technical scheme of the invention is realized in such a way that the method for analyzing the dynamic degradation of acephate and metabolite methamidophos in leaf vegetables comprises the following steps:
(1) test layout:
arranging two areas, namely an open area and a greenhouse, wherein each area is at least provided with a blank control area and three test areas, and an isolation area is arranged at the junction of each cell and used for planting leaf vegetables respectively;
(2) and (3) acephate application treatment:
selecting the acephate solution with the concentration of 99 percent to dilute by a multiple C1、C2、C3Three concentrations of 500, 1000 and 1500 times of dilution, respectively, and spray application is carried out on different test areas, respectively1、C2、C3The application times are 2 times, the application interval time is 7 days, the application is finished at 10 am, and samples are collected at 1, 3, 5, 7, 10, 14, 17, 21, 30 and 45d after the application; the blank control zone was not dosed with drug and was sampled only at 0, 7, 21 d; the first sampling time is 2-3 hours after the medicine is applied, the second sampling time is 10 am of the next day, and the rest sampling time is selected in the am, and each area samples 25.0 g;
(2) extraction:
accurately weighing 25.0g of a test area sample and a blank control area sample respectively, placing the test area sample and the blank control area sample into a homogenizer, adding 50.0mL of extracting solution respectively, homogenizing at high speed in the homogenizer, filtering by using filter paper, collecting filtrate, adding 5-7g of sodium chloride, standing at room temperature after violent shaking to layer the extracting solution and a water phase, sucking 10.00mL of extracting solution, placing the extracting solution into a centrifuge tube, slowly introducing nitrogen or air flow into the tube, evaporating to be nearly dry, fixing the volume to 5.0mL by using a purifying solution, mixing uniformly to obtain a sample solution and a matrix standard solution respectively, and then respectively moving the sample solution and the matrix standard solution into two 2mL automatic sample feeding bottles for chromatographic determination;
(3) preparing a blank standard solution:
fully dissolving 5-7g of sodium chloride in 50.0mL of extracting solution, sucking 10.00mL of sodium chloride, placing the sodium chloride in a centrifuge tube, slowly introducing nitrogen or air flow into the centrifuge tube, evaporating to be nearly dry, fixing the volume to 5.0mL by using a purified solution, and uniformly mixing to obtain a blank standard solution;
(4) and (3) determination:
accurately preparing standard solutions of acephate and methamidophos with mass concentration of 0.05, 0.25, 0.1, 0.5, 1.0mg/L, respectively injecting 1 mu L of sample to obtain a response value of gas chromatography, and drawing an acephate standard solution curve and a methamidophos standard solution curve by using a concentration-peak area;
(5) addition recovery and relative standard deviation: setting and adding three concentrations of mixed standard solutions of acephate and methamidophos, namely 0.08, 0.12 and 0.16mg/kg, and performing an addition recovery test to obtain the addition recovery rate and the Relative Standard Deviation (RSDs) of the acephate and the methamidophos respectively;
(6) detecting the minimum detection amount of acephate and methamidophos by adopting a gas chromatography;
(7) according to the corresponding relation between the peak height and the concentration of the acephate and the methamidophos in the gas chromatography, the acephate and the methamidophos in the leaf vegetables are added according to the minimum adding concentration, the corresponding value of the added sample on an instrument is 3 times larger than that of the signal noise of the instrument, and the minimum detection concentration of the acephate and the methamidophos in the leaf vegetables is obtained.
The method for analyzing the dynamic degradation of acephate and metabolite methamidophos in leaf vegetables realizes the dynamic degradation analysis of acephate and metabolite methamidophos in leaf vegetables by combining the degradation characteristic research of acephate and metabolite methamidophos and the adjustment of the method process and parameters, and analyzes the degradation rules and main influence factors with small concentration, thereby providing scientific basis for reasonably using acephate, avoiding residual phytotoxicity on sensitive crops of later crops and determining the planting time of leaf vegetables.
Preferably, the leaf vegetables are Chinese cabbage, spinach, celery, rape, caraway, lettuce, shepherd's purse, amaranth, crowndaisy chrysanthemum, wuta-tsai, fennel, leek, garlic sprout and chicory sprout, buckwheat sprout, radish sprout and finger citron tender tip.
Preferably, the blank control area and the test area are equal in area and not less than 15m2So as to ensure the accuracy of the death result.
Preferably, the extract is an acetonitrile homogenate.
Preferably, the purification solution is an acetone solution.
Preferably, the method is also provided with analytical determination quality control and guarantee measures; each batch of analysis samples required 1 blank sample to confirm the cleanliness of reagents and containers; each batch of analysis samples was taken in 2-3 replicates to confirm reproducibility of the test results.
Preferably, in the determination process in the step (4), the sample injection sequence is blank standard solution → matrix standard solution → 3 parallel sample solutions → matrix standard solution → blank standard solution.
Preferably, the chromatographic conditions of the gas chromatography are:
the instrument comprises the following steps: an Agilent GC 7890A gas chromatograph (Agilent, usa) equipped with a flame photometric detector (FPD phosphor filter), an autosampler, split/no-split sample inlet;
a chromatographic column: DB-17(30m × 0.32mm × 0.25 μm);
temperature programming: initial column temperature 80 deg.C, maintaining for 2min, and then maintaining at 8 deg.C/min-1Raising the speed to 250 ℃, and maintaining for 6min until all the components in the sample flow out;
temperature: the temperature of the detector is 250 ℃; the temperature of a sample inlet is 220 ℃;
and (3) sample introduction mode: no shunt sampling;
sample introduction amount: 1 mu L of the solution;
carrier gas: 99.999% high-purity nitrogen gas with the flow rate of 3.0 mL/min-1(ii) a Air: 100 mL/min-1(ii) a Hydrogen gas: 75 mL/min-1。
The invention has the beneficial effects that:
(1) the method for analyzing the dynamic degradation of acephate and metabolite methamidophos in leaf vegetables realizes the dynamic degradation analysis of acephate and metabolite methamidophos in leaf vegetables by combining the degradation characteristic research of acephate and metabolite methamidophos and the adjustment of the method process and parameters, and analyzes the degradation rules and main influence factors with small concentration, thereby providing scientific basis for reasonably using acephate, avoiding residual phytotoxicity on sensitive crops of next crops and determining the planting time of leaf vegetables;
(2) by improving the pretreatment method and optimizing the conditions of a gas chromatography instrument and adopting a blank matrix matching standard solution and a front and back standard solution average value calibration method, the chromatographic peak shape is improved and the matrix effect is eliminated, so that the detection sensitivity and accuracy are improved; by researching the degradation rule of acephate pesticide and metabolite methamidophos thereof on the leaf vegetables, the change rule of the acephate and the metabolite methamidophos thereof in the degradation process is known, the pesticide safety interval period is obtained, and a technical support is provided for guiding agricultural production and agricultural product quality safety supervision and law enforcement.
Drawings
FIG. 1 is a standard graph of acephate;
FIG. 2 is a standard graph of the metabolite methamidophos;
FIG. 3 is a gas chromatography of acephate and its metabolite acephate.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention discloses a method for detecting acephate and metabolite methamidophos thereof in leaf vegetables, which adopts main instruments and chemical reagents as follows:
reagent: acetonitrile (chromatographic purity), acetone (analytical purity, redistilled), and sodium chloride (analytical purity), wherein the purity of the 3 standard solutions is greater than 96%, and the solvents are acetone.
The instrument comprises the following steps: an Agilent GC 7890A gas chromatograph (Agilent, usa) equipped with a flame photometric detector (FPD phosphor filter), an autosampler, split/no split injection port.
Example 1
A dynamic degradation analysis method of acephate and metabolite methamidophos in leaf vegetables comprises the following steps:
(1) test layout:
two areas of open air and a greenhouse are arranged, each area is provided with a blank control area and three test areas, and the areas of the blank control area and the three test areas are 15m2The junction of each cell is provided with an isolation area, and Chinese cabbages are planted in the areas respectively;
(2) and (3) acephate application treatment:
selecting the acephate solution with the concentration of 99 percent to dilute by a multiple C1、C2、C3Three concentrations of 500, 1000 and 1500 times of dilution, respectively, and spray application is carried out on different test areas, respectively1、C2、C3The application times are 2 times, the application interval time is 7 days, the application is finished at 10 am, and samples are collected at 1, 3, 5, 7, 10, 14, 17, 21, 30 and 45d after the application; the blank control zone was not dosed with drug and was sampled only at 0, 7, 21 d; the first sampling time is 2 hours after the medicine is applied, the second sampling time is 10 am of the next day, and the rest sampling time is selected in the am, and each area samples 25.0 g;
(2) extraction:
accurately weighing 25.0g of a test area sample and a blank control area sample respectively, placing the test area sample and the blank control area sample into a homogenizer, adding 50.0mL of acetonitrile solution respectively, homogenizing the samples in the homogenizer at a high speed for 2min, filtering the homogenate by using filter paper, collecting filtrate, adding 5g of sodium chloride, standing the filtrate at room temperature for 30min after violent shaking to separate an extracting solution and a water phase, sucking 10.00mL of the extracting solution again, placing the extracting solution into a 10.0mL centrifuge tube, slowly introducing nitrogen into the tube, evaporating the solution to be nearly dry, fixing the volume to 5.0mL by using acetone, uniformly mixing to obtain a sample solution and a matrix standard solution respectively, and then respectively moving the sample solution and the matrix standard solution into two 2mL automatic sample feeding bottles;
(3) preparing a blank standard solution:
fully dissolving 5g of sodium chloride in 50.0mL of extracting solution, sucking 10.00mL of sodium chloride, placing the sodium chloride in a centrifuge tube, slowly introducing nitrogen or air flow into the centrifuge tube, evaporating to be nearly dry, fixing the volume to 5.0mL by using a purification solution, and uniformly mixing to obtain a blank standard solution;
(4) and (3) determination:
accurately preparing standard solutions of acephate and methamidophos with mass concentration of 0.05, 0.25, 0.1, 0.5 and 1.0mg/L, detecting the standard solutions by using a high performance liquid chromatograph, respectively injecting 1 mu L of sample according to the sampling sequence of blank standard solution → matrix standard solution → 3 parallel sample solutions → matrix standard solution → blank standard solution to obtain response values of gas chromatography, respectively using the ratio of the area of the acephate with the five different concentrations to the area of the acephate peak as the ordinate y of a standard curve equation, performing linear regression on the obtained five groups of x and y data to obtain a standard curve equation of y x + b and weight coefficients a and b by fitting the ratio of the acephate concentration in the standard working solution to the acephate concentration in the internal standard working solution as the abscissa x of the standard curve equation, as shown in fig. 1 and fig. 2, the standard curve equation of acephate is that y is 10819.27R2+41.68(R20.9984), the standard curve equation of the metabolite methamidophos is that y is 5511.83R2-29.05(R2＝0.9993)；
(5) Addition recovery and relative standard deviation: the method comprises the steps of setting a mixed standard solution with three concentrations of acephate and methamidophos of 0.08, 0.12 and 0.16mg/kg, and carrying out an addition recovery test to obtain the addition recovery rate and the Relative Standard Deviation (RSDs) of acephate and methamidophos respectively, wherein the addition recovery rate and the Relative Standard Deviation (RSDs) of acephate and a metabolite methamidophos thereof are shown in Table 1, when the addition concentrations of acephate in Chinese cabbage are 0.08, 0.12 and 0.16mg/kg, the average recovery rates are 93 percent, 97 percent and 101 percent respectively, and the relative standard deviations are 7.4 percent, 5.6 percent and 4.7 percent respectively; the recycling concentrations of the methamidophos added into the Chinese cabbage are respectively 0.08, 0.12 and 0.16mg/kg, the average recycling rates are respectively 91 percent, 93 percent and 98 percent, and the relative standard deviations are respectively 6.4 percent, 6.6 percent and 8.9 percent;
TABLE 1
Table of Relative Standard Deviations (RSDs) and recovery rates of addition of acephate and its metabolite methamidophos.
(6) Detecting the minimum detection amount of acephate and methamidophos by adopting a gas chromatography;
(7) according to the corresponding relation between the peak height and the concentration of the acephate and the methamidophos in the gas chromatography, the acephate and the methamidophos in the leaf vegetables are added according to the minimum adding concentration, the corresponding value of the added sample on an instrument is 3 times larger than that of the signal noise of the instrument, and the minimum detection concentration of the acephate and the methamidophos in the leaf vegetables is obtained.
The chromatographic conditions of the gas chromatograph in the present example were:
the instrument comprises the following steps: an Agilent GC 7890A gas chromatograph (Agilent, usa) equipped with a flame photometric detector (FPD phosphor filter), an autosampler, split/no-split sample inlet;
the chromatographic column is DB-17(30m × 0.32mm × 0.25 μm);
temperature programming: initial column temperature 80 deg.C, maintaining for 2min, and then maintaining at 8 deg.C/min-1Raising the speed to 250 ℃, and maintaining for 6min until all the components in the sample flow out;
the temperature of the detector is 250 ℃; the temperature of a sample inlet is 220 ℃;
and (3) sample introduction mode: no shunt sampling;
sample introduction amount: 1 mu L of the solution;
carrier gas: 99.999% high-purity nitrogen gas with the flow rate of 3.0 mL/min-1(ii) a Air: 100 mL/min-1(ii) a Hydrogen gas: 75 mL/min-1。
The lowest detection quantity of acephate and methamidophos in gas chromatography is 3 multiplied by 10-10g。
As shown in figure 3, according to the corresponding situation of acephate and methamidophos on a gas chromatograph, the response values of samples of acephate and methamidophos with the lowest addition concentration of 0.08mg/kg in leaf vegetables on an instrument are both larger than 3 times of noise of the gas chromatograph, and the calculated lowest detection concentrations of the acephate and the methamidophos are both 0.08 mg/kg.
Therefore, the method completely meets the requirements of accuracy, precision and sensitivity in pesticide residue analysis.
Example 2
A dynamic degradation analysis method of acephate and metabolite methamidophos in leaf vegetables comprises the following steps:
(1) test layout:
two areas of open air and a greenhouse are arranged, each area is provided with a blank control area and three test areas, and the areas of the blank control area and the three test areas are both 20m2The junction of each cell is provided with an isolation region, and shepherd's purse is planted in the region;
(2) and (3) acephate application treatment:
selecting the acephate solution with the concentration of 99 percent to dilute by a multiple C1、C2、C3Three concentrations of 500, 1000 and 1500 times of dilution, respectively, and spray application is carried out on different test areas, respectively1、C2、C3The application times are 2 times, the application interval time is 7 days, the application is finished at 10 am, and samples are collected at 1, 3, 5, 7, 10, 14, 17, 21, 30 and 45d after the application; the blank control zone was not dosed with drug and was sampled only at 0, 7, 21 d; the first sampling time is 3 hours after the medicine is applied, the second sampling time is 10 am of the next day, and the rest sampling time is selected in the am, and each area samples 25.0 g;
(2) extraction:
accurately weighing 25.0g of a test area sample and a blank control area sample respectively, placing the test area sample and the blank control area sample into a homogenizer, adding 50.0mL of acetonitrile solution respectively, homogenizing the samples in the homogenizer at a high speed for 2min, filtering the homogenate by using filter paper, collecting filtrate, adding 8g of sodium chloride, standing the filtrate at room temperature for 30min after violent shaking to separate an extracting solution and a water phase, sucking 10.00mL of the extracting solution again, placing the extracting solution into a 10.0mL centrifuge tube, slowly introducing nitrogen into the tube, evaporating the solution to be nearly dry, fixing the volume to 5.0mL by using acetone, uniformly mixing to obtain a sample solution and a matrix standard solution respectively, and then respectively moving the sample solution and the matrix standard solution into two 2mL automatic sample feeding bottles;
(3) preparing a blank standard solution:
fully dissolving 8g of sodium chloride in 50.0mL of extracting solution, sucking 10.00mL of sodium chloride, placing the sodium chloride in a centrifuge tube, slowly introducing nitrogen or air flow into the centrifuge tube, evaporating to be nearly dry, fixing the volume to 5.0mL by using a purification solution, and uniformly mixing to obtain a blank standard solution;
(4) and (3) determination:
accurately preparing standard solutions of acephate and methamidophos with mass concentration of 0.05, 0.25, 0.1, 0.5 and 1.0mg/L, detecting the standard solutions by using a high performance liquid chromatograph, respectively injecting 1 mu L of sample according to the sampling sequence of blank standard solution → matrix standard solution → 3 parallel sample solutions → matrix standard solution → blank standard solution to obtain response values of gas chromatography, respectively using the ratio of the area of the acephate with the five different concentrations to the area of the acephate peak as the ordinate y of a standard curve equation, performing linear regression on the obtained five groups of x and y data to obtain a standard curve equation of y x + b and weight coefficients a and b by fitting the ratio of the acephate concentration in the standard working solution to the acephate concentration in the internal standard working solution as the abscissa x of the standard curve equation, wherein the standard curve equation of acephate is that y is 10819.27R2+41.68(R20.9984), the standard curve equation of the metabolite methamidophos is that y is 5511.83R2-29.05(R2＝0.9993)；
(5) Addition recovery and relative standard deviation: setting and adding three concentrations of mixed standard solutions of acephate and methamidophos, namely 0.08, 0.12 and 0.16mg/kg, and performing an addition recovery test to obtain the addition recovery rate and the Relative Standard Deviation (RSDs) of the acephate and the methamidophos respectively;
(6) detecting the minimum detection amount of acephate and methamidophos by adopting a gas chromatography;
(7) according to the corresponding relation between the peak height and the concentration of the acephate and the methamidophos in the gas chromatography, the acephate and the methamidophos in the leaf vegetables are added according to the minimum adding concentration, the corresponding value of the added sample on an instrument is 3 times larger than that of the signal noise of the instrument, and the minimum detection concentration of the acephate and the methamidophos in the leaf vegetables is obtained.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. A dynamic degradation analysis method of acephate and metabolite methamidophos in leaf vegetables is characterized by comprising the following steps:
(1) test layout:
arranging two areas, namely an open area and a greenhouse, wherein each area is at least provided with a blank control area and three test areas, and an isolation area is arranged at the junction of each cell and used for planting leaf vegetables respectively;
(2) and (3) acephate application treatment:
selecting the acephate solution with the concentration of 99 percent to dilute by a multiple C1、C2、C3Three concentrations of 500, 1000 and 1500 times of dilution, respectively, and spray application is carried out on different test areas, respectively1、C2、C3The application times are 2 times, the application interval time is 7 days, the application is finished at 10 am, and samples are collected at 1, 3, 5, 7, 10, 14, 17, 21, 30 and 45d after the application; the blank control zone was not dosed with drug and was sampled only at 0, 7, 21 d; the first sampling time is 2-3 hours after the medicine is applied, the second sampling time is 10 am of the next day, and the rest sampling time is selected in the am, and each area samples 25.0 g;
(2) extraction:
accurately weighing 25.0g of a test area sample and a blank control area sample respectively, placing the test area sample and the blank control area sample into a homogenizer, adding 50.0mL of extracting solution respectively, homogenizing at high speed in the homogenizer, filtering by using filter paper, collecting filtrate, adding 5-7g of sodium chloride, standing at room temperature after violent shaking to layer the extracting solution and a water phase, sucking 10.00mL of extracting solution, placing the extracting solution into a centrifuge tube, slowly introducing nitrogen or air flow into the tube, evaporating to be nearly dry, fixing the volume to 5.0mL by using a purifying solution, mixing uniformly to obtain a sample solution and a matrix standard solution respectively, and then respectively moving the sample solution and the matrix standard solution into two 2mL automatic sample feeding bottles for chromatographic determination;
(3) preparing a blank standard solution:
fully dissolving 5-7g of sodium chloride in 50.0mL of extracting solution, sucking 10.00mL of sodium chloride, placing the sodium chloride in a centrifuge tube, slowly introducing nitrogen or air flow into the centrifuge tube, evaporating to be nearly dry, fixing the volume to 5.0mL by using a purified solution, and uniformly mixing to obtain a blank standard solution;
(4) and (3) determination:
accurately preparing standard solutions of acephate and methamidophos with mass concentration of 0.05, 0.25, 0.1, 0.5, 1.0mg/L, respectively injecting 1 mu L of sample to obtain a response value of gas chromatography, and drawing an acephate standard solution curve and a methamidophos standard solution curve by using a concentration-peak area;
(5) addition recovery and relative standard deviation:
setting and adding three concentrations of mixed standard solutions of acephate and methamidophos, namely 0.08, 0.12 and 0.16mg/kg, and performing an addition recovery test to obtain the addition recovery rate and the Relative Standard Deviation (RSDs) of the acephate and the methamidophos respectively;
(6) detecting the minimum detection amount of acephate and methamidophos by adopting a gas chromatography;
(7) according to the corresponding relation between the peak height and the concentration of the acephate and the methamidophos in the gas chromatography, the acephate and the methamidophos in the leaf vegetables are added according to the minimum adding concentration, the corresponding value of the added sample on an instrument is 3 times larger than that of the signal noise of the instrument, and the minimum detection concentration of the acephate and the methamidophos in the leaf vegetables is obtained.
2. The method for analyzing the dynamic degradation of acephate and a metabolite methamidophos in leafy vegetables according to claim 1, wherein the method comprises the following steps: the leaf vegetables are Chinese cabbage, caulis et folium Brassicae Capitatae, herba Spinaciae, herba Apii Graveolentis, caulis et folium Brassicae campestris, herba Coriandri, herba Capsellae, herba Amaranthi Tricoloris, caulis et folium Chrysanthemi Segeti, WUJIANCAI, fructus Foeniculi, folium Allii tuberosi, Bulbus Allii seedling and herba Cichorii bud, semen Fagopyri Esculenti bud, radix Raphani bud, and tender tips of.
3. Acetyl according to claim 1The dynamic degradation analysis method of methamidophos and metabolite methamidophos in leaf vegetables is characterized in that: the blank control area and the test area are equal in area and not less than 15m2。
4. The method for analyzing the dynamic degradation of acephate and a metabolite methamidophos in leafy vegetables according to claim 1, wherein the method comprises the following steps: the extract is an acetonitrile homogenate.
5. The method for analyzing the dynamic degradation of acephate and a metabolite methamidophos in leafy vegetables according to claim 1, wherein the method comprises the following steps: the purifying liquid is acetone solution.
6. The method for analyzing the dynamic degradation of acephate and a metabolite methamidophos in leafy vegetables according to claim 1, wherein the method comprises the following steps: the method is also provided with quality control and guarantee measures for analysis and determination; each sample for analysis requires 1 blank sample, and each sample for analysis requires 2-3 parallel samples.
7. The method for analyzing the dynamic degradation of acephate and a metabolite methamidophos in leafy vegetables according to claim 1, wherein the method comprises the following steps: in the determination process in the step (4), the sample introduction sequence is blank standard solution → matrix standard solution → 3 parallel samples → matrix standard solution → blank standard solution.
8. The method for analyzing the dynamic degradation of acephate and a metabolite methamidophos in leafy vegetables according to any one of claims 1 to 5, wherein the chromatographic conditions of the gas chromatography method are as follows:
the instrument comprises the following steps: an Agilent GC 7890A gas chromatograph (Agilent, usa) equipped with a flame photometric detector (FPD phosphor filter), an autosampler, split/no-split sample inlet;
a chromatographic column: DB-17(30m × 0.32mm × 0.25 μm);
temperature programming: initial column temperature 80 deg.C, maintaining for 2min, and then maintaining at 8 deg.C/min-1Raising the speed to 250 ℃, and maintaining for 6min until all the components in the sample flow out;
temperature: the temperature of the detector is 250 ℃; the temperature of a sample inlet is 220 ℃;
and (3) sample introduction mode: no shunt sampling;
sample introduction amount: 1 mu L of the solution;
carrier gas: 99.999% high-purity nitrogen gas with the flow rate of 3.0 mL/min-1(ii) a Air: 100 mL/min-1(ii) a Hydrogen gas: 75 mL/min-1。
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| CN102221589A (en) * | 2011-03-28 | 2011-10-19 | 中国水稻研究所 | Method for detecting residual quantity of pesticides in vegetable sample by utilizing liquid chromatogram-high resolution mass spectrometer |
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| CN103472155A (en) * | 2013-09-29 | 2013-12-25 | 邬金飞 | Gas chromatographic method for detecting residue amount of nine kinds of organophosphorus pesticide in rice |
| WO2014202505A1 (en) * | 2013-06-20 | 2014-12-24 | Bayer Cropscience Ag | Aryl sulfide derivatives and aryl sulfoxide derivatives as acaricides and insecticides |
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| CN102221589A (en) * | 2011-03-28 | 2011-10-19 | 中国水稻研究所 | Method for detecting residual quantity of pesticides in vegetable sample by utilizing liquid chromatogram-high resolution mass spectrometer |
| CN102914608A (en) * | 2012-11-12 | 2013-02-06 | 天津出入境检验检疫局动植物与食品检测中心 | Method for quickly detecting pesticide multiple residues in traditional Chinese medicine through membrane separation and comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometer |
| WO2014202505A1 (en) * | 2013-06-20 | 2014-12-24 | Bayer Cropscience Ag | Aryl sulfide derivatives and aryl sulfoxide derivatives as acaricides and insecticides |
| CN103472155A (en) * | 2013-09-29 | 2013-12-25 | 邬金飞 | Gas chromatographic method for detecting residue amount of nine kinds of organophosphorus pesticide in rice |
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| KUMAR VIJAY 等: "A review on sample preparation and chromatographic determination of acephate and methamidophos in different samples", 《ARABIAN JOURNAL OF CHEMISTRY》 * |
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