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Method for detecting fenhexamid in fruits, vegetables or soil

A technology of fenhexamid and vegetables, which is applied in the field of analysis and detection, can solve the problems of unsatisfactory purification effect and instrument pollution, and achieve the effect of simple pretreatment process, high recovery rate and good repeatability

Active Publication Date: 2018-10-16
ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these methods are convenient, the purification effect is not ideal, and it is easy to cause pollution to the instrument.

Method used

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  • Method for detecting fenhexamid in fruits, vegetables or soil
  • Method for detecting fenhexamid in fruits, vegetables or soil
  • Method for detecting fenhexamid in fruits, vegetables or soil

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Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0026] 1 Materials and methods

[0027] 1.1 Main equipment and chemical reagents

[0028] Ultra-high performance liquid chromatography tandem mass spectrometer (LCMS8050, Shimadzu Corporation),

[0029] Vortex instrument (MX-S, Dalong Xingchuang Experimental Instrument (Beijing) Co., Ltd.),

[0030] R-201 rotary evaporator (Shanghai Shensheng Biotechnology Co., Ltd.),

[0031] Acetonitrile (chromatographically pure Honeywell 4L, Burdick & Jackson company),

[0032] Methanol (chromatographically pure Honeywell 4L, Burdick & Jackson company),

[0033] Formic acid (99%, HPLC 1 L, Anaqua company),

[0034] MAX small column (3cc / 60mg, Waters company)

[0035] Filter membrane (0.22μm, model TQP-61322, Pall company)

[0036] 1.2 Method

[0037] 1.2.1 Instrument conditions

[0038] Ultra-high performance liquid chromatography conditions:

[0039] Chromatographic column: ACQUITY UPLC BEH (1.7 μm, 2.1×100 mm, Waters Company). Mobile phase: acetonitrile / 0.1% aqueous formic acid...

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Abstract

The invention relates to a method for detecting fenhexamid in fruits, vegetables or soil. The method comprises the following steps: 1) weighing 5 g of a sample, adding the sample into a 50 mL centrifuging tube, adding 5 mL of acetonitrile, carrying out vortex treatment for 1 min, centrifuging the obtained solution at 4000 r / min for 5 min, collecting the obtained supernatant, carrying out extraction one time by using 5 mL of acetonitrile, collecting and mixing obtained extracts, carrying out rotary evaporation to remove the acetonitrile, and adding distilled water to a constant volume of 10 mLin order to form a solution to be purified; and 2) purifying: providing an MAX small column of 3 cc / 60 mg, respectively sequentially adding 3 mL of methanol and 3 mL of water to activate the MAX smallcolumn, completely introducing 10 mL of the above obtained sample, respectively sequentially leaching the sample with 1 mL of 2% ammonia water and 2 mL of methanol, blow-drying a liquid in the MAX small column by a rubber pipette bulb, eluting the MAX small column with 2 mL of a 1% formic acid methanol solution, concentrating the obtained eluate at 40 DEG C until the eluate is dry, adding methanol to a constant volume of 2.0 mL, allowing the obtained solution to go through a 0.22 [mu]m filter membrane, and detecting the filtered solution. The method improves the lowest detection threshold andimproves the detection sensitivity.

Description

technical field [0001] The invention belongs to the field of analysis and detection, in particular, it belongs to the analysis and detection method of fenhexamid in vegetables, fruits and soil Background technique [0002] Fenhexamid is an amide protective fungicide that can inhibit the germination of fungal spores and mycelium growth. It is mainly used to control various gray mold and related sclerotinia and black spots on horticultural crops and vegetables illness etc. Fenhexamid degrades quickly in the environment and is not volatile. It has good compatibility with the ecology and is used in large quantities. [0003] The chemical name of fenhexamid is N-(2,3-dichloro-4-hydroxyphenyl)-1-methyl-cyclohexylcarboxamide; the chemical structural formula is [0004] [0005] Molecular formula C 14 h 17 Cl 2 NO 2 , molecular weight 302.20. The melting point of fenhexamid is 153.8°C, and the boiling point is 230°C to soften. Hardly soluble in water, easily soluble in ac...

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 许振岚吴珉张昌朋赵华何红梅汤涛俞建忠李岗蒋金花王彦华陈列忠
Owner ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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