A method for the analysis and detection of four heterocyclic pesticides in environmental water samples
A detection method and a heterocyclic technology, applied in the field of pesticide detection, can solve the problems of high cost of use and maintenance of gas chromatography-mass spectrometry, low service life of extraction fibers, and easy blockage of columns, and save analysis time and cost. , easy operation, mild reaction conditions
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Embodiment 1
[0061] The analysis and detection method of four kinds of heterocyclic pesticides in the environmental water samples involved in the embodiment specifically includes the following steps:
[0062] Step 1: Preparation of magnetic metal organic framework material MOF-5:
[0063] (1) Dissolve 1.0 g of ferric chloride hexahydrate in 20 mL of ethylene glycol, then add 3 g of sodium acetate and 10 mL of ethanolamine, and stir to dissolve;
[0064] (2) The mixture prepared in step (1) was reacted for 8h at 200°C in the solvothermal reaction kettle, and the obtained mixture in the solvothermal reaction kettle was washed with ultrapure water to obtain ferric iron tetraoxide ( NH 2 -Fe 3 o 4 ), the prepared NH 2 -Fe 3 o 4 Vacuum dry at 60°C for 12 hours;
[0065] (3) Dissolve 0.5065g terephthalic acid in 40mL N,N dimethylamide (DMF), 2.302g hexahydrate and zinc nitrate (Zn(NO 3 ) 2 ·6H 2 O) be dissolved in 50mL DMF, and it is slowly added dropwise in the DMF solution that is di...
Embodiment 2
[0075] This embodiment investigates the main factors affecting the extraction recovery of four heterocyclic pesticides, calculates the optimum value of each factor when the extraction recovery is the highest, and then determines the four heterocyclic pesticides under the condition of the optimum value of each factor. The parameters related to the working curve of the pesticide and the detection limit and precision of the method, the specific process includes the following steps:
[0076] Step 1: Calculate the optimal value of each factor when the extraction recovery of the four heterocyclic pesticides is the highest:
[0077] (1) The investigation of the amount of adsorbent to the extraction recovery
[0078] In this example, the effect of the amount of adsorbent on the extraction recovery rate was investigated, and 4, 6, 7, 8, and 10 mg of magnetic metal-organic framework material MOF-5 were weighed in 20 mL of simulated water samples, and the four heterocyclic pesticides in ...
Embodiment 3
[0099] Determination of residues of four heterocyclic pesticides in Nuocheng Reservoir of Qingdao City, Qianhan Reservoir of Qingdao City, and the Yellow River. After collecting three kinds of water samples, filter them with rapid qualitative filter paper with a pore size of 80-120 μm, and then use a 0.45 μm filter membrane Filtration; the filtered water sample is measured by the method described in Example 1, and the accuracy test is carried out by the method described in Example 2, and the concentrations of four kinds of heterocyclic pesticides are respectively prepared as 5 μg / L, 50 μg / L, and 100 μg The actual water samples with low, medium and high concentrations of / L were tested for the standard recovery rate, and each concentration point was measured 3 times, and the average value, relative standard deviation and standard recovery rate of the three determinations were calculated; among them, the three None of the four heterocyclic pesticides were detected in the water sa...
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