Effective separation method and rapid detection method for amide herbicide in mixed beans

A herbicide and miscellaneous bean technology, applied in the field of detection, can solve the problem of no regulation of the maximum residue limit and so on

Active Publication Date: 2019-07-30
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 for amide herbicide in mixed beans
  • Effective separation method and rapid detection method for amide herbicide in mixed beans
  • Effective separation method and rapid detection method for amide herbicide in mixed 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 an amide herbicide in mixed beans. The separation method comprises the following steps of: grinding the mixed beans into powder and sieving the powder with a 80-mesh sieve; mixing the mixed bean powder and water, regulating pH into 7, and carrying out oscillation; continuously adding an extracting agent (whichis formed by carrying out isovolumetric mixing on ethyl acetate and normal hexane) and NaCl, carrying out ultrasonic extraction for 2min, and then carrying out centrifugation at a temperature of 0 DEGC under revolutions per minute of 15,000 rpm; transferring supernatant into a centrifuge tube containing an adsorbent MIL-101 (Zn), carrying out stirring and mixing, and then carrying out centrifugation under revolutions per minute of 10,000 rpm; and removing the supernatant, adding methanol into a centrifuge tube and carrying out ultrasonic elution on an analyte. The effective separation methodhas the beneficial effects that (1) the ethyl acetate and normal hexane isovolumetric mixed reagent is used as the extracting agent and is non-polar, so that the amide herbicide can be extracted fromthe mixed beans; (2) the MIL-101 (Zn) is used for carrying out absorption of the amide herbicide so as to implement separation of the amide herbicide, fat, proteins and the like; and (3) ultrasonic elution implements purification of the amide herbicide.

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 Applications(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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