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Effective separation method and rapid detection method of amide herbicides in miscellaneous beans

A technology of amide herbicides and herbicides, which is applied in the field of detection and can solve problems such as no regulations on maximum residue limits

Active Publication Date: 2022-03-08
HEILONGJIANG BAYI AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] At present, my country has only stipulated the maximum residue limits of a few herbicides, and there is no regulation on the maximum residue limits of amide herbicides in most grains, especially

Method used

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  • Effective separation method and rapid detection method of amide herbicides in miscellaneous beans
  • Effective separation method and rapid detection method of amide herbicides in miscellaneous beans
  • Effective separation method and rapid detection method of amide herbicides in miscellaneous beans

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Embodiment Construction

[0049] The present invention will be specifically introduced below in conjunction with the accompanying drawings and specific embodiments.

[0050] 1. Main equipment

[0051] Agligent1260 high performance liquid chromatograph: American Agilent Company.

[0052] Eclipse XDB-C18 column (150mm×4.6mm, 3.5μm): American Agilent Company.

[0053] Allegra 64R high-speed refrigerated centrifuge: American Beckman Company.

[0054] RE-52AA vacuum rotary evaporator: Shanghai Yarong Biochemical Instrument Factory.

[0055] Millipore-q water purification system: American Millipore Company.

[0056] Rigaku D / max-2550 X-ray powder diffractometer: Japan Rigaku Company, using Cu target (Kα, ).

[0057] Tecnai G2F20S-Twin transmission electron microscope: Philips, Netherlands.

[0058] Others: Philips HR-2870 grinding machine, diode array detector, automatic sampler, quaternary gradient pump, stainless steel reaction kettle (with PTFE liner).

[0059] The ultrapure water used in the expe...

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Abstract

The invention discloses an effective separation method and a rapid detection method for amide herbicides in miscellaneous beans, wherein the separation method comprises the following steps: grinding the miscellaneous beans into powder and passing through an 80-mesh sieve, mixing the miscellaneous bean powder and water to adjust the pH to 7 , shake, continue to add extractant (equal volume of ethyl acetate and n-hexane mixed) and NaCl, ultrasonically extract for 2min, then centrifuge at 15000rpm at 0°C, transfer the supernatant to a centrifuge containing adsorbent MIL‑101 (Zn) Stir to mix, then centrifuge at 10,000 rpm, remove the supernatant, add methanol to the centrifuge tube, and ultrasonically elute the analyte. The present invention is beneficial in that: (1) use ethyl acetate and n-hexane equivolume mixed reagent as extractant, non-polar, can extract amide herbicides from miscellaneous beans; (2) use MIL- 101(Zn) carried out the adsorption of amide herbicides, and realized the separation of amide herbicides, fat, protein, etc.; (3) ultrasonic elution realized the purification of amide herbicides.

Description

technical field [0001] The invention relates to a compound separation method and a detection method, in particular to an effective separation method and a rapid detection method of amide herbicides in miscellaneous beans, and belongs to the technical field of detection. Background technique [0002] Amide herbicides are one of the most widely used herbicides in the world. At present, there are some studies on the detection methods and residue dynamics of amide herbicides in vegetables, peanuts, soybeans and other crops, but there are few reports on the detection of residues in miscellaneous grains. [0003] At present, the varieties of amide herbicides with large sales volume include: propanil, metazachlor, pretilachlor, and butachlor. These herbicides have a good weeding effect, but a little carelessness is prone to phytotoxicity. For example, pretilachlor is highly toxic to arthropods such as bees, shrimps, and crabs. Butachlor can cause red blood cells in catfish to muta...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/065
Inventor 张丽媛于润众张晨曦王长远张东杰
Owner HEILONGJIANG BAYI AGRICULTURAL UNIVERSITY
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