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Method for separating and enriching amide herbicides in naked oats

A technology for amide herbicides and naked oats, which is applied in the field of separation and enrichment of amide herbicides in naked oats, and achieves the effects of simplifying the operation process, reducing RSDs and improving extraction efficiency.

Inactive Publication Date: 2019-05-31
HEILONGJIANG BAYI AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Simultaneous Determination of Amide Herbicide Residues in Oats by Ionic Liquid (IL-based) Matrix Solid Phase Dispersion-Froth Flotation-Solid Phase Extraction (MSPD-FF-SPE) and High Performance Liquid Chromatography (HPLC) still less

Method used

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  • Method for separating and enriching amide herbicides in naked oats
  • Method for separating and enriching amide herbicides in naked oats
  • Method for separating and enriching amide herbicides in naked oats

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Example 1 illustrates the effect of dispersant type on the extraction recovery rate of amide herbicide

[0056] Before extraction, use 0.6mL acetonitrile and 0.8mL formic acid solution to activate Bond Elut PRS, accurately weigh 1.000 grams of naked oat powder samples, and add 3.000g of Florisil, diatomaceous earth, activated carbon, neutral alumina and silica gel. 100μL[C 8 MIM]BF 4 Place the mixture in an agate mortar and grind with a pestle for 3 minutes to obtain a uniform mixture. Then transfer the mixture to a flotation vessel, add 10 mL of water, shake and mix uniformly, and adjust the pH of the sample solution to 7.5 with 1 mol / L NaOH solution. Turn on the carrier gas switch, the carrier gas passes through the flotation cell at a flow rate of 120 mL / min, the flotation time is 8 min, and the carrier gas passes through the sample. The generated foam passes through the glass wool, where the solid particles do not pass, and is introduced into the Bond Elut PRS and ads...

Embodiment 2

[0059] Example 2 illustrates the effect of ionic liquid types on the extraction recovery rate of amide herbicides

[0060] Before extraction, use 0.6mL acetonitrile and 0.8mL formic acid solution to activate Bond Elut PRS, accurately weigh 1.000g naked oat powder samples and 3.000g diatomaceous earth, and add 100μL [C 4 MIM][BF 4 ](A), [C 6 MIM][BF 4 ](B), [C 8 MIM][BF 4 ](C), [C 6 MIM][PF 6 ](D), [C 8 MIM][PF 6 ](E) The mixture is placed in an agate mortar, and a pestle is used to grind for 3 minutes to obtain a uniform mixture. Then transfer the mixture to a flotation vessel, add 10 mL of water, shake and mix uniformly, and adjust the pH of the sample solution to 7.5 with 1 mol / L NaOH solution. Turn on the carrier gas switch, the carrier gas passes through the flotation cell at a flow rate of 120 mL / min, the flotation time is 8 min, and the carrier gas passes through the sample. The generated foam passes through the glass wool, where the solid particles do not pass, and is intr...

Embodiment 3

[0063] Example 3 illustrates the effect of the type of solid phase extraction column on the extraction recovery rate of amide herbicides

[0064] Before extraction, use 0.6mL acetonitrile and 0.8mL formic acid solution to activate the solid phase extraction column (SPE), and accurately weigh 1.000 grams of naked oat powder samples, 3.000g diatomaceous earth, 100μL [C 8 MIM]BF 4 Place the mixture in an agate mortar and grind with a pestle for 3 minutes to obtain a uniform mixture. Then transfer the mixture to a flotation vessel, add 10 mL of water, shake and mix uniformly, and adjust the pH of the sample solution to 7.5 with 1 mol / L NaOH solution. Turn on the carrier gas switch, the carrier gas passes through the flotation cell at a flow rate of 120 mL / min, the flotation time is 8 min, and the carrier gas passes through the sample. The generated foam passes through the glass wool, where the solid particles do not pass, and are introduced into Bond Elut NH 2 (1mL, 100mg), Bond Elut...

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Abstract

The invention relates to a method for separating and enriching amide herbicides in naked oats. With naked oats adopted as a sample, an ionic liquid adopted as an extractant, a matrix solid-phase dispersion-foam flotation-solid phase extraction method and high-efficiency liquid phase chromatography (HPLC) are simultaneously adopted to separate and enrich amide herbicides in the naked oats. According to the invention, the process conditions of the above method are optimized. With the method of the invention adopted, extraction efficiency can be improved; a purification effect can be improved; anenrichment factor can be increased; experiment costs are decreased; RSDs are decreased; an operation flow can be simplified; sample pretreatment can be completed in a few minutes; impurities such asproteins and lipids are not required to be removed by acid precipitation before an experiment, instead, can be directly removed by a foam flotation process; and a green reagent ionic liquid is adoptedto replace an organic solvent, and therefore, the consumption of organic solvents is reduced during the experiment, and the method is environmentally sustainable.

Description

Technical field [0001] The invention belongs to the field of pesticide residue analysis, and particularly relates to a method for separating and enriching amide herbicides in naked oats. Background technique [0002] Oats are one of the most nutritious grains in the world. Its nutritional value is very high. Its fat content is 4 times that of rice, and it contains 8 essential amino acids for the body. Vitamin E content is also higher than that of rice and wheat. Now nutritionists have discovered that oatmeal is an ideal food, especially for the prevention of atherosclerosis, high blood pressure and coronary heart disease. It has medical and health care functions. It is a food and medicine homologous food, which can reduce blood fat, control blood sugar, lose weight and beauty. , Moisturizing the bowel, laxative, preventing colon cancer, etc. Oatmeal is rich in linoleic acid, which accounts for 35-52% of the total unsaturated fatty acids, which is very beneficial in increasing t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/14G01N30/08G01N30/02
Inventor 张丽媛张春芝王长远张东杰阮长青
Owner HEILONGJIANG BAYI AGRICULTURAL UNIVERSITY