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Method for rapidly detecting phenoxyacetic acid herbicide in soil
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A phenoxyacetic acid and herbicide technology, which is applied in the field of determination of dicamba and phenoxyacetic acid herbicide residues in tobacco-growing soil, can solve the problem that the detection of herbicides is not suitable, the selectivity is not strong, and the gasification is not easy. and other problems, to achieve the effect of improving selectivity and sensitivity, shortening analysis time, and improving resolution
Inactive Publication Date: 2015-03-18
SICHUAN BRANCH OF CHINA TOBACCO
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The selectivity of thin-layer scanning method and capillary electrophoresis method is not strong, and the detection limit is relatively high, which is not suitable for the detection of phenoxycarboxylic acid herbicides with extremely low content in soil
The GC-MS method is superior to the first two methods in terms of selectivity and sensitivity, but dicamba, 2,4-D and 2,4,5-T are not easily vaporized, and derivatization is required in GC-MS detection, and their Easily residues on the column stationary phase, thereby interfering with detection
Liquid chromatography-tandem mass spectrometry (LC-MS / MS) is a detection technique developed in the past 30 years, and its residues of dicamba, 2,4-D and 2,4,5-T in fruits, textiles and grains It has been applied in the detection, but the detection of dicamba, 2,4-D and 2,4,5-T residues in soil has not been reported
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[0048] The following will be described in conjunction with the accompanying drawings and specific embodiments. see Figure 1 to Figure 15 .
[0051] Formic acid is HPLC grade (concentration is 49-51%, German Sigma company); Acetonitrile, methanol are chromatographically pure (U.S. Thermo-Fisher company); Dicamba, 2,4-D and 2,4,5-T standard substance From Labor Dr. Ehrenstorfer-Schafers (chemical purity: 98.5%, Augsburg, Germany), internal standard dicamba-d 3 ,2,4-D-d 3 From Labor Dr. Ehrenstorfer-Schafers (chemical purity: 99%, isotopic purity: 98.5%, Augsburg, Germany) 2,4,5-T-d 2 Purchased from CDN Isotopes Inc. (chemical purity: 99%, isotopic purity: 99%, Quebec Canada). N-propyl ethylenediami...
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Abstract
The invention discloses a method for rapidly detecting a phenoxyacetic acid herbicide in soil. The method comprises the following four steps of: extracting a target object in the soil, purifying N-propyl ethanediamine, preparing a standard storage solution and a standard working solution, and carrying out liquid chromatogram-tandem mass spectrum determination. The method disclosed by the invention overcomes the disadvantages of a sample processing method in the prior art; and aiming at a tobacco-planting soil sample, an enzymolysis condition, a solid-phase extraction condition and relative detection conditions of LC-MS / MS are optimized, and mainly an ion source condition, a chromatographic column and a mobile phase system are optimized. Compared with a traditional gas chromatography, a base material dispersed solid-phase extraction method is used for detecting dicamba, 2,4-D and 2,4,5-T. The pre-treatment process is simplified and the analysis sensitivity is improved.
Description
technical field [0001] The invention belongs to the technical field of pesticide residue inspection, in particular to a method for determining the residual amount of phenoxyacetic acid herbicides in soil, in particular to the residual amount of dicamba, 2,4-D and 2,4,5-T in tobacco planting soil detection method. Background technique [0002] Phenoxycarboxylic acid herbicide pesticides, such as dicamba, 2,4-D, 2,4,5-T, etc., are the first type of selective herbicides put into commercial production, and are widely used in cereal crop fields, Coniferous forests and pastures, etc. Dicamba, 2,4-D and 2,4,5-T are all low-toxic herbicides, which are absorbed and conducted through plant leaves, stems and roots, hindering the normal conduction of plant hormones and causing them to die. However, in the process of use, the results show that such substances can cause human soft tissue malignant tumors and exhibit placental toxicity to animals. Among them, 2,4-D and 2,4,5-T are consid...
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