Gas chromatography-mass spectrometry rapid determination method for non-registered components in pesticide preparation

A pesticide preparation and gas chromatography technology, applied in the field of gas chromatography-mass spectrometry rapid determination, can solve problems such as large defects, inability to efficiently and accurately detect pesticide components, etc., achieve high sensitivity, improve detection types and detection efficiency, strong resistance Effects of Interference Ability

Active Publication Date: 2019-01-22
SILKWORM COCOON RES GROUP CHINESE INST OF TEST TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In fact, the non-registered ingredients in pesticides are unknown before confirmation, and have strong concealment, randomness, diversity and complexity. Conventional gas chromatography, liquid chromatography and other chromatographic methods can only rely on retention Qualitative and quantitative analysis can not efficiently and accurately detect all the pesticide ingredients that may be added without authorization, and there are big defects in the detection of non-registered ingredients in pesticides, while gas chromatography-mass spectrometry, liquid chromatography-tandem mass spectrometry, etc. The chromatography-mass spectrometry method takes into account the high separation efficiency of chromatography and the characteristics of accurate identification of compound structures by mass spectrometry, which is very suitable for the comprehensive, accurate and efficient detection of non-registered components in pesticides

Method used

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  • Gas chromatography-mass spectrometry rapid determination method for non-registered components in pesticide preparation
  • Gas chromatography-mass spectrometry rapid determination method for non-registered components in pesticide preparation
  • Gas chromatography-mass spectrometry rapid determination method for non-registered components in pesticide preparation

Examples

Experimental program
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Effect test

Embodiment 1

[0068] 1. Instruments and equipment

[0069]Agilent 7890B-5977B gas chromatography-mass spectrometer; Eppendorf 5810R high-speed refrigerated centrifuge; Sartorius BP 211D electronic balance; XW-80A vortex mixer.

[0070] 2. Materials and Reagents

[0071] Pesticide standard products: 131 kinds of pesticide standard products, such as acrylamide, fluorosulfuron-methyl, chrysanthemum, demeton, hexachlorobenzene, trifluralin, prometon, terbufos, and dicrotophos, were purchased from Germany Dr. Ehrenstorfer Company.

[0072] Reagents: Chromatographically pure acetonitrile, purchased from Sigma-Aldrich, USA.

[0073] Sample: commercially available pesticide sample A——eucalyptol (5% soluble agent).

[0074] 3. Preparation of standard solution: Accurately weigh an appropriate amount of pesticide standard substance, use chromatographically pure acetonitrile as solvent, prepare acrylamide, flurimsulfuron-methyl, isoeugenol, chrysanthemum, demeton, hexachlorobenzene, fluoxetine A si...

Embodiment 2

[0088] As described in Example 1, another pesticide preparation sample B was selected, and the measured content of each non-registered component in the sample is shown in Table 6.

[0089] Table 6 Test results of non-registered components in sample B

[0090]

Embodiment 3

[0092] As described in Example 1, another pesticide preparation sample E was selected, and the measured content of each non-registered component in the sample is shown in Table 7.

[0093] Table 7 Test results of 131 non-registered ingredients in sample E

[0094]

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Abstract

The invention relates to a gas chromatography-mass spectrometry rapid determination method for non-registered components in a pesticide preparation, and belongs to the technical field of pesticide quality detection. The gas chromatography-mass spectrometry rapid determination method for the non-registered components in the pesticide preparation comprises the following steps of preparing a standardsolution; preparing a sample solution; preparing a blank solution; performing GC-MS detection: injecting the standard working solution and the blank solution into a GC-MS, performing selected ion monitoring, and performing regression analysis on the corresponding concentrations of the non-registered components by the quantitative ion peak areas of the non-registered components after blank deduction, so as to obtain a standard working curve; and injecting a to-be-detected sample solution into the GC-MS under the same condition, obtaining the quantitative ion peak areas of the non-registered components in the sample after blank deduction, and substituting the quantitative ion peak areas into the standard working curve, so as to obtain the content of the non-registered components in the sample. According to the method disclosed by the invention, the capability of performing high-throughput accurate qualitative screening and accurate quantitative detection on the 131 non-registered components in the pesticide preparation is realized, so that the detection types and the detection efficiency are greatly improved.

Description

technical field [0001] The invention relates to a gas chromatography-mass spectrometry rapid determination method for non-registered components in pesticide preparations, belonging to the technical field of pesticide quality detection. Background technique [0002] Pesticides are important means of agricultural production and disaster relief materials. They play an indispensable role in preventing and controlling agricultural pests, ensuring agricultural production, increasing farmers' income and storing agricultural products. However, in recent years, in order to pursue economic benefits, reduce production costs, improve the control effect of pesticide products, and evade the supervision of pesticide registration policies, some pesticide manufacturers have added non-registered ingredients, also known as recessive ingredients or unregistered ingredients, to pesticide preparations without authorization. , has become an "open secret" and "hidden rule" in the industry, seriously...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72G01N2030/025G01N2030/062
Inventor 唐祥凯冯德建李怀平史谢飞许洋邹燕管驰
Owner SILKWORM COCOON RES GROUP CHINESE INST OF TEST TECH
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