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Method for detecting pyridazinofos, pyridaben, cypermethrin and lambda-cyhalothrin in soil or sediment
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A technology of efficient cyhalothrin and pyridazinate, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of low accuracy of results, complicated pre-treatment process, and low detection efficiency, so as to improve the detection efficiency , suitable for industrial applications, and the effect of accurate measurement results
Pending Publication Date: 2021-08-06
河北百润环境检测技术有限公司
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Existing methods for the detection of pesticides in soil or sediment are still dominated by traditional gas chromatography, the pretreatment process is complex and only depends on the retention time for qualitative analysis, which can easily lead to false positive results
The Chinese patent with the authorized publication number CN103913529B involves the detection of cypermethrin and lambda-cyhalothrin, but the sample pretreatment steps are cumbersome and the accuracy of the gas chromatography measurement results is low; the Chinese patent application with the application publication number CN109254099A has passed gas chromatography - The rapid mass spectrometry method detects pyridaben and lambda-cyhalothrin, but the heating program takes a long time, the detection efficiency is low, the detection limit is 5.3-149.1mg / kg, the span is large, and the precision is low
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Embodiment 1
[0052] The detection method of pyridifenthion, pyridaben, cypermethrin and lambda-cyhalothrin in the soil or sediment of embodiment 1
[0053] This embodiment is a method for detecting pyridazinate, pyridaben, cypermethrin and lambda-cyhalothrin in soil or sediment, comprising the following steps in sequence:
[0055] Measure the dry matter content of the soil sample according to the method of HJ 613, and set aside (if the sample is sediment, measure the water content of the sediment sample according to the method of GB17378.5 to obtain the dry matter content of the sample).
[0056] Accurately weigh 20g (accurate to 0.01g) of the sample, mix it with 2g of diatomaceous earth with a particle size of 0.6mm, use a vacuum freeze dryer, freeze-dry, dehydrate and grind to the shape of quicksand, and obtain the sample to be extracted.
[0101] The detection method of pyridifenthion, pyridaben, cypermethrin and lambda-cyhalothrin in the soil or sediment of embodiment 2-6
[0102] Examples 2-6 are respectively a detection method for pyridifenthion, pyridaben, cypermethrin and lambda-cyhalothrin in soil or sediment, the specific methods are basically the same, the difference lies in the adjustment of samples and other parameters , the specific parameters and test results are shown in Table 5.
[0103] Table 5 embodiment 2-6 process parameter
[0104]
[0105] As can be seen from the results in Table 5, the detection limit of this method is 0.02mg / kg-0.04mg / kg, the method of embodiment 2-6 can be realized to different soil or sediment sample detection result shows, this method detection limit is low , with high detection accuracy, it can realize the detection of trace pesticides in soil or sediment.
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Abstract
The invention belongs to the technical field of pesticide residue detection methods, and discloses a method for detecting pyridazinofos, pyridaben, cypermethrin and lambda-cyhalothrin in soil or sediment, which comprises the following steps of performing pressurized fluid extraction by using a dichloromethane-acetone mixed solvent, performing parallel nitrogen blowing concentration on an extracting solution, detecting by using a gas chromatography-mass spectrometry method, carrying out qualitative analysis according to retention time, fragment ionmass-to-charge ratio and abundance ratio, and calculating the contents of pyridazinofos, pyridaben, cypermethrin and lambda-cyhalothrin in a sample quantitatively through an internal standard method, so that the method is short in determination time and low in detection limit, the detection efficiency and the accuracy of a determination result are greatly improved, the detection of trace pesticides in soil or sediments is realized.
Description
technical field [0001] The invention belongs to the technical field of pesticide residue detection methods, and relates to a detection method for pesticides in soil or sediments, in particular to a detection method for pyridazinphos, pyridaben, cypermethrin and lambda-cyhalothrin in soil or sediments . Background technique [0002] As an indispensable means of production in agricultural production, pesticides have made great contributions to agricultural development and human food supply. Worldwide, the losses of agricultural diseases, insects, and weeds avoided and restored by pesticides account for 1 / 3 of the grain output. However, with the long-term and large-scale application of pesticides in recent years, the problem of pesticide residues and pollution has become increasingly serious, and it has become one of the important sources of agricultural non-point sourcepollution. According to statistics, only about 30% of the pesticides applied in the farmland are attached ...
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