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Detection method for trinexapac-ethyl residual quantity in high performance liquid chromatography determination environmental sample

A technology of high performance liquid chromatography and determination method, which is applied in the field of high performance liquid chromatography to determine the residual amount of trinexapac-ethyl in environmental samples, and achieves the effects of universal instrument, environmental protection and less impurity dissolution.

Inactive Publication Date: 2013-06-05
XIAMEN PONY TEST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there are few domestic and foreign studies on the residues of trinexapac-ethyl in water quality, soil, vegetables, fruits and other substrates

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The mensuration of trinexapac-ethyl residue in surface water of embodiment 1

[0031] 1. Sample pretreatment

[0032] Activate the HLB solid-phase extraction column with 10mL methanol and 10mL water sequentially in advance, gradually transfer 50mL water sample into the solid-phase extraction column, rinse the solid-phase extraction column with 5mL ultrapure water, and control the flow rate to 2 drops / second. Elute with 10mL methanol, and collect the eluate in a centrifuge tube. The eluate was blown to near dryness at 40°C with nitrogen, dissolved in 1.00 mL of methanol, passed through a 0.22 μm organic filter membrane, and tested.

[0033] 2. Determination by high performance liquid chromatography

[0034] Determine the sample and standard working solution according to the conditions of liquid chromatography, use the standard curve to correct the concentration of the sample solution, and quantify with the external standard method. The liquid chromatography conditions...

Embodiment 2

[0047] The mensuration of trinexapac-ethyl residue in the soil of embodiment 2

[0048] 1. Sample extraction: Weigh 10.00g of the prepared soil sample into a 50mL centrifuge tube, add water to moisten it, add 20mL acetonitrile, vortex mix, shake and extract for 30min, add 5g sodium chloride, vortex mix, and centrifuge at 8000rpm After 10 minutes, use a pipette to pipette 10 mL of the organic layer solution into a heart-shaped bottle, and evaporate it in a 40°C water bath to nearly dryness, dissolve the residue with 1.00 mL of methanol, pass through a 0.22 μm organic filter membrane, and wait for the test.

[0049] 2. Determination by high performance liquid chromatography: with embodiment 1.

[0050] 3. Recovery rate and precision

[0051] Negative soil samples were used to measure the accuracy of standard addition, the concentration of standard addition was 0.04mg / kg and 0.2mg / kg respectively, each concentration was measured in parallel three times, the average recoveries we...

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Abstract

The invention discloses a detection method for the trinexapac-ethyl residual quantity in a high performance liquid chromatography determination environmental sample. The detection method for the trinexapac-ethyl residual quantity in the high performance liquid chromatography determination environmental sample comprises the following steps: (1) a water sample is enriched by a hydrophile-lipophile balance (HLB) solid phase extraction column, eluted by carbinol, and concentrated with a constant volume and then fractionation detection is carried out on the water sample with a high performance liquid chromatography system; (2) a soil sample is wet with water, extracted in a vibrating mode by acetonitrile and layered through salting out, an organic phase is concentrated with a constant volume, and then fractionation detection is carried out on the soil sample with the high performance liquid chromatography system. Octadecyl silane is adopted as a filling agent by a chromatographic column, and a detector is a ultraviolet detector with a diode array. A mobile phase is a mixed solvent of carbinol and a 0.1% phosphoric acid aqueous solution, the ratio is that, by volume, the carbinol accounts for 50%-70%, and the 0.1% phosphoric acid aqueous solution accounts for 50%-30%. The detection wavelength is 280 nm, the temperature of the column is 25 DEG C to 40 DEG C, and the injected sample volume is 10-20 mu L. Through systematic comparative study, the detection method for the trinexapac-ethyl residual quantity in the high performance liquid chromatography determination environmental sample is created. The detection method for the trinexapac-ethyl residual quantity in the high performance liquid chromatography determination environmental sample has the technical advantages of being good in fractionation effect, accurate in determination, high in sensitivity, strong in specificity, convenient and quick to analyze and the like.

Description

technical field [0001] The invention relates to an analysis method for pesticide residues, in particular to a method for measuring trinexapac-ethyl residues in environmental samples by high performance liquid chromatography. Background technique [0002] Trinexapac-ethyl English common name trinexapac-ethyl, cas number 95266-40-3, molecular formula C 13 h 16 o 5 , Molecular formula chemical name: 4-cyclopropyl (hydroxyl) methylene-3,5-diketone cyclohexane carboxylic acid ethyl ester, belongs to cyclohexane carboxylic acid plant growth regulator, and is gibberellin biosynthesis inhibitor agent to control plant growth by reducing the content of gibberellin. [0003] China and the European Union have not yet formulated the maximum residue limit (MRL) of trinexapac-ethyl, and Japan stipulates that the MRL value of trinexapac-ethyl in various fruits and vegetables is 0.02mg / kg. [0004] "Pesticide Science and Management 2010, 31, (8)" disclosed that methanol: 0.1% phosphoric ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/08G01N30/14
Inventor 宋薇
Owner XIAMEN PONY TEST
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