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Gas chromatography-mass spectrometry method for detecting content of fluazinam in rice field water body

A gas chromatography and fluazinam technology, which is applied in the field of gas chromatography-mass spectrometry detection of fluazinam content in paddy field water, and achieves the effects of simple pretreatment, wide linear range and good linear correlation.

Pending Publication Date: 2021-01-29
HUNAN AGRICULTURAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The detection and analysis methods of fluazinam reported at home and abroad include gas chromatography, liquid chromatography, and liquid chromatography-mass spectrometry, but there is no report on the detection method of fluazinam in water by gas chromatography-mass spectrometry

Method used

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  • Gas chromatography-mass spectrometry method for detecting content of fluazinam in rice field water body
  • Gas chromatography-mass spectrometry method for detecting content of fluazinam in rice field water body
  • Gas chromatography-mass spectrometry method for detecting content of fluazinam in rice field water body

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Example 1 Gas Chromatography-Mass Spectrometer Detection of Fluazinam in Rice Field Water

[0030] (1) Sample pretreatment: collect paddy field water samples, filter with a small funnel and filter paper; accurately measure 50mL of filtered paddy field water samples and place them in a container, add 20mL of 10% sodium chloride solution, shake well and use 40mL, 20 mL and 20 mL of n-hexane extracted once, combined the n-hexane extracts, concentrated on a rotary evaporator to near-dryness, and fixed the volume to 2.0 mL with acetone to obtain the sample solution to be tested.

[0031] (2) Gas chromatography-mass spectrometry is used for qualitative analysis of fluazinam contained in the sample solution to be tested.

[0032] The analysis conditions of gas chromatography-mass spectrometry are as follows: the chromatographic column is an Agilent capillary column HP-5MS, 30m (length) × 0.25mm (inner diameter) × 0.25um (liquid film thickness), the inlet temperature is 250°C, ...

Embodiment 2

[0048] Example 2 application

[0049] In 2018, a field experiment was conducted in Changsha, Hunan Province. A paddy field without rice was selected beside the paddy field where paddy was planted (irrigated at a depth of 3 to 5 cm), and the spraying concentration of 50% fluazinam suspension was 25-35 ml / mu. , the water consumption per mu is 30-45 kg, the spray method is used for pesticide application, and the paddy field water is collected 2h, 7d, 14d, 21d, 28d and 35d after spraying, and the test is repeated twice. Filter the collected paddy field water with a small funnel and filter paper. Accurately measure 50mL of filtered paddy field water samples and place them in a container, add 20mL of 10% sodium chloride solution, shake well, extract with 40mL, 20mL, and 20mL of n-hexane for 3 times, combine the n-hexane extracts, and put them on a rotary evaporator Concentrate to nearly dryness, dilute to 2.0 mL with acetone, and inject samples under the above-mentioned selected GC...

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Abstract

The invention relates to a gas chromatography-mass spectrometry method for detecting the content of fluazinam in a rice field water body. The method comprises the following steps: filtering rice fieldwater, extracting with normal hexane, concentrating to a constant volume, detecting by using gas chromatography-mass spectrometry (GC-MS), carrying out qualitative analysis by using retention time and monitoring ions, quantifying by using an external standard method, and under optimized conditions, the fluazinam being in a good linear relation within the range of 0.05 to 5 mg / L, the correlation coefficient being 0.999, the fluazinam detection limit being 0.05 mg / L, the quantitative limit being 0.05 mg / kg, the average adding recovery rate of the fluazinam in rice field water being 88% to 98%,and the relative standard deviation being 6% to 9%. The sensitivity, accuracy and precision of the method meet the requirements of pesticide residue detection.

Description

technical field [0001] The invention belongs to the field of chemical analysis and detection, relates to the detection and analysis of fluazinam, in particular to a method for detecting the content of fluazinam in paddy field water by gas chromatography-mass spectrometry. Background technique [0002] Fluazinam, English common name: fluazinam, chemical name: 1-(2-cyano-2-methoxyiminoacetyl)-3-ethylurea, relative molecular mass: 465.09, chemical formula: C 13 h 4 C l2 f 6 N 4 o 4 , whose chemical structure is shown in figure 1 . Fluazinam is a 2,6-dinitroaniline low-toxic fungicide successfully developed by Ishihara Co., Ltd. in Japan. Its mechanism of action is unique. It kills bacteria by blocking the formation of energy (ATP) and is not easy to develop drug resistance. , has no cross-resistance with other fungicides, and has the functions of treatment, eradication and super protection. It has obvious effects on Alternaria, Botrytis, Phytophthora, Plasmodium and Scl...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/12
CPCG01N30/02G01N30/06G01N30/12G01N2030/062G01N2030/126
Inventor 杨丽华罗海峰卿朝霞龚道新
Owner HUNAN AGRICULTURAL UNIV
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