Method for detecting content of trifluorobenzene pyrimidine by GC-MS

A trifluorophenylpyrimidine and GC-MS technology, applied in the field of chemical analysis and detection, can solve the problems of high usage fee and maintenance cost, high liquid chromatography analysis cost, high daily maintenance cost, etc. Simple processing and short detection time

Active Publication Date: 2021-08-31
HUNAN AGRICULTURAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The cost of liquid chromatography analysis is high, the daily maintenance cost is expensive, and the analysis time is generally longer than that of gas phase
Although the ultra-high performance liquid chromatography-tandem mass spectrometer has a shorter analysis time, it is more expensive, and the usual use and maintenance costs are higher

Method used

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  • Method for detecting content of trifluorobenzene pyrimidine by GC-MS
  • Method for detecting content of trifluorobenzene pyrimidine by GC-MS
  • Method for detecting content of trifluorobenzene pyrimidine by GC-MS

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Experimental program
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Effect test

Embodiment 1

[0032] The gas chromatography-mass spectrometer detection of trifluoropyrimidine in the pesticide preparation suspension concentrate of embodiment 1

[0033] 1. Preparation of standard working solution

[0034] Accurately weigh 0.0100 g (accurate to 0.0001 g) of trifluoropyrim standard substance (purity is 99.4%), place it in a 100 mL brown volumetric flask, dissolve it with acetone and prepare trifluoropyrimidine with a concentration of 1000.0 mg / L Standard mother liquor. Then the standard mother liquor of trifluoropyrim was prepared into standard working solutions by gradient dilution method, so that the concentrations of trifluoropyrim were all 0.01, 0.05, 0.10, 0.50, 1.00 mg / L.

[0035] 2. Sample solution preparation

[0036] Measure 1.000g of 20% trifluoropyrimidine suspension in a 10mL volumetric flask, dissolve it in acetone, dilute to volume and shake well, filter through a 0.45μm filter membrane, and take the filtrate as the sample solution.

[0037] 3. Use gas chr...

Embodiment 2

[0060] Example 2 Gas Chromatography-Mass Spectrometer Detection of Trifluoropyrim in Paddy Field Environment

[0061] 1. Paddy field environmental sample processing

[0062] Paddy field environmental samples are: brown rice, rice husk, rice straw and paddy field soil.

[0063] Accurately weigh the above-mentioned paddy field environmental samples (the weighing amount of the paddy field soil is 20.0g, and the weighing amount of the remaining samples is 10.0g), and add dichloromethane to each sample (100mL of dichloromethane is added to the straw sample, and the rest Add 40mL dichloromethane to the sample respectively), then vortex on the vortex mixer for 3-5min, vacuum filter through the Buchner funnel, wash the filter residue, Buchner funnel and suction filter bottle twice with 20mL, 20mL dichloromethane , and the combined suction filtrate was transferred to a rotary evaporator to concentrate (55° C.) to nearly dryness, and 5 mL of acetone was added to constant volume.

[00...

Embodiment 3

[0079] The mensuration of embodiment 3 actual samples

[0080]In 2019, a field test was conducted at the experimental base of Hunan Agricultural University in Furong District, Changsha City, Hunan Province. The test plot was designed according to the requirements of the pesticide residue test guidelines, 20% trifluoropyrim water dispersible granules, and the application dose was 27 g / ha (The dosage of the preparation is 9.0 g / mu). When the rice planthopper reaches the control standard (rice tillering stage), the pesticide is applied twice, and the interval between each application is 20 days. The test area was set up ((paddy field soil, rice plants (including rice straw and rice) and blank control test area, a total of 3 treatments, each with an area of ​​100m 2 . Paddy soil, rice straw and paddy grain samples were collected 14 days, 21 days and 28 days after the last spraying, respectively.

[0081] 3.1 Determination of trifluoropyrimidine in rice field soil

[0082] Soil ...

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Abstract

The invention relates to a method for detecting the content of trifluorobenzene pyrimidine by GC-MS (Gas Chromatography-Mass Spectrometer). The trifluorobenzene pyrimidine in a sample solution to be detected is detected and analyzed by GC-MS. The trifluorobenzene pyrimidine has a good linear relationship in a range of 0.01-1 mg/L, the correlation coefficient is 0.9906, the detection limit of the trifluorobenzene pyrimidine is 0.01 mg/L, and the quantitation limit of the trifluorobenzene pyrimidine is 0.01 mg/kg. The method has the advantages of being short in detection time, low in detection limit, high in precision, good in accuracy and the like, and the content of the triflumezopyrim in the triflumezopyrim suspending agent and rice field environments (soil, brown rice, rice husks and rice straws) can be rapidly and accurately determined.

Description

technical field [0001] The invention belongs to the field of chemical analysis and detection, and relates to the detection and analysis of trifluoropyrimidine content, in particular to a method for detecting trifluoropyrimidine content by gas chromatography-mass spectrometry (GC-MS). Background technique [0002] Trifluoropyrimidine, English common name: triflumezopyrim, chemical name: 3,4-dihydro-2,4-dioxo-1-(pyrimidin-5-ylmethyl)-3-(α,α,α- Trifluorom-tolyl)-2H-pyrido[1,2-α]pyrimidin-1-ium-3-salt, relative molecular mass: 398.34, chemical formula: C 2 0H 13 f 3 N 4 o 2 . Trifluoropyrimidine is a mesoionic insecticide developed by DuPont of the United States and released in 2013. It is a new type of pyrimidine compound and is mainly used in crops such as cotton, rice, corn and soybeans to control brown planthoppers and leafhoppers. Its mechanism of action is to act on the nicotinic acetylcholine receptor (nAChR) of insects, but the mechanism of action is different from...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 杨丽华王文鑫魏维科龚道新罗海峰
Owner HUNAN AGRICULTURAL UNIV
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