Method for determining residual quantity of fosetyl-aluminium in environmental sample

A technique for determining aluminum triethylphosphonate and its determination method, which is applied in the field of aluminum triethylphosphonate residues, can solve problems such as the lack of research on aluminum triethylphosphonate residues, and achieve the promotion of detection of pesticide residues with a low detection limit , Conducive to the effect of promoting the application

Inactive Publication Date: 2013-02-27
谱尼测试集团深圳有限公司
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  • Abstract
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Problems solved by technology

[0010] However, there is no research on the residues of triethylphosphonate in soil and environmental water quality.

Method used

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  • Method for determining residual quantity of fosetyl-aluminium in environmental sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The mensuration of aluminum triethylphosphonate residue in water of embodiment 1

[0042] 1. Sample pretreatment: pre-activate C with 10mL methanol and 10mL water 18 Solid-phase extraction column, transfer 5mL water sample into the solid-phase extraction column, control the flow rate to 2 drops / second, discard the first 1mL effluent, collect the remaining effluent, pass through a 0.22μm water filter membrane, take 200μL sample solution, add 800μL After dilution with ultra-pure water, it was determined by high-performance liquid chromatography-tandem mass spectrometry.

[0043] 2. Determination by high performance liquid chromatography-tandem mass spectrometry

[0044] The sample and standard working solution were determined according to the conditions of liquid chromatography-tandem mass spectrometry, the concentration of the sample solution was corrected by the standard curve, and the external standard method was used for quantification.

[0045] 3. Linear relationsh...

Embodiment 2

[0051] The mensuration of aluminum triethylphosphonate residual amount in the soil of embodiment 2

[0052] 1. Sample extraction: Weigh 5.0g of the prepared soil sample into a 50mL centrifuge tube with a cover, add 10mL of 10% methanol solution, after ultrasonic extraction for 30min, centrifuge at 8000rpm for 5min, pipette 5mL supernatant to C 18 In the solid-phase extraction column (activated with 5-15mL methanol and 5-15mL water in advance), control the flow rate to 2 drops / second, discard the first 1mL effluent, collect the remaining effluent, pass through a 0.22μm organic filter membrane, and use an ultra- Diluted with pure water for high performance liquid chromatography-tandem mass spectrometry.

[0053] 2. Determination by high performance liquid chromatography-tandem mass spectrometry: same as in Example 1.

[0054] 3. Recovery rate and precision

[0055] Negative soil samples were used to add standards to determine its accuracy. The concentrations of the standard a...

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Abstract

The invention discloses a method for determining residual quantity of fosetyl-aluminium in an environmental sample, which comprises the following steps that (1) after a soil sample is extracted with a 10% to 50% methanol aqueous solution, purified with a C18 solid phase extraction column and diluted with ultrapure water, a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) system is adopted for separation and detection; and (2) after an environmental water sample is purified with the C18 solid phase extraction column and diluted with the ultrapure water, the HPLC-MS/MS system is adopted for separation and detection. The adopted chromatographic column is a chromatographic column which uses carbon octadecyl bonded silica gel as a filling agent, a mobile phase is acetonitrile-water, and the fosetyl-aluminium is separated and detected through gradient elution and electro spray in a negative ion scanning mode. Through systemic comparative study, the invention establishes the method for determining the residual quantity of the fosetyl-aluminium in the environmental sample, and the method has the technical characteristics of good separating effect, accurate determination, high sensitivity, strong specificity, simpleness, convenience and rapidity in analysis and the like.

Description

technical field [0001] The invention relates to a pesticide residue analysis method, in particular to a high-performance liquid chromatography-tandem mass spectrometry method for determining the residual amount of triethylphosphonate aluminum in environmental samples. Background technique [0002] Aluminum triethylphosphonate, English name Phosethyl-Al, molecular formula C 6 h 18 AlO 9 P 3 , molecular weight 354.10. Aluminum triethylphosphonate is a colorless powder with a melting point greater than 300°C; a vapor pressure of <0.013mpa (25°C); a solubility in water of 120g / L (20°C). Stable under general storage conditions, hydrolyzed by strong acid and strong alkali, can be oxidized by oxidant, decomposed at >200℃. [0003] Canada stipulates that the maximum residue limit of triethylphosphonate aluminum on turmeric root is 15mg / kg, that on onion is 10mg / kg, and on citrus is 9mg / kg; the EU stipulates that the maximum residue limit of triethylphosphonate aluminum on...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 宋薇
Owner 谱尼测试集团深圳有限公司
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