Method for determining perfluorocarboxylic acid compound in crops

A technology for perfluorocarboxylic acids and compounds, which is applied in the field of pollutant determination, can solve the problems of low recovery rate of perfluorocarboxylic acid compounds, and achieve the effects of wide application range, improved recovery rate and high recovery rate

Active Publication Date: 2017-05-24
JINAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At the same time, the existing analysis methods for perfluorocarboxylic acids in crops are mainly established for one or two types of crops, and are aimed at the resistance to matrix effects and wide applicability of multiple types of crops, including cereals, root vegetables, leafy vegetables, and fruit vegetables. The method has not been reported yet
Moreover, the recovery rate of low-carbon chain (C10) perfluorocarboxylic acid compounds determined by existing analytical methods is relatively low (48% to 69%)

Method used

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  • Method for determining perfluorocarboxylic acid compound in crops
  • Method for determining perfluorocarboxylic acid compound in crops
  • Method for determining perfluorocarboxylic acid compound in crops

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Experimental program
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Embodiment 1

[0037] The optimization of perfluorocarboxylic acid compound pretreatment method in the crop of embodiment 1

[0038] Taking the leaf vegetable lettuce as the test crop, the impact of the type of extractant, the type of purification column and the amount of active graphite carbon black on the recovery of perfluorocarboxylic acid compounds in the crop was investigated by the standard recovery experiment (10ng / g), so that Obtain an optimized pretreatment method. The investigated extraction solvents include three commonly used solvents for the extraction of perfluorinated compounds in environmental samples: methyl tert-butyl ether (MTBE), acetonitrile / water mixed solution (90:10, v / v) and tetrahydrofuran (THF) / water Mixed solution (75:25, v / v); the purification column investigated includes WAX column, HLB column and Florisil column (Florisil), and the amount of graphite carbon black investigated includes 0, 10, 25, 50mg .

[0039] 1. The specific implementation process of the r...

Embodiment 2

[0048] The applicability verification of embodiment 2 optimization pretreatment method to different kinds of crops

[0049] With cereal crops (rice), root vegetables (carrots), leafy vegetables (lettuce), fruit vegetables (pumpkins) as test crops, by different concentration standard addition recovery experiments (10,25,50ng / g) investigate "embodiment 1 "Establish the applicability of optimized pre-processing methods.

[0050] 1. Specific implementation process

[0051] (1) Sample preparation: samples of different blank crops (rice, carrot, lettuce, pumpkin) were frozen, dried, ground and mixed, and then stored in a 4°C refrigerator for later use.

[0052] (2) Configuration of the standard curve of the target perfluorocarboxylic acid compound of each crop: Take different kinds of blank crop samples respectively, and obtain the extraction matrix of each crop through the process of "extraction and purification of samples in Example 1". Dilute the standard stock solution of perf...

Embodiment 3

[0067] Embodiment 3 establishes the method to the mensuration of actual sample

[0068] In order to verify the feasibility of the inventive method of the present invention, the method was used to measure the content of perfluorocarboxylic acid compounds collected from crops in the farmland around a fluorine chemical factory in a large city in southern my country. The collected samples included Chinese cabbage (2 species), lettuce (7 species), mustard greens (9 species), pakchoi (3 species) and celery (3 species). Sample analysis and determination were carried out according to the specific implementation process of "Example 1" and "Example 2", and the measured samples included actual samples and their spiked quality control samples (10, 25, 50 ng / g). The measurement results are shown in Table 3-1 and 3-2. The recovery rate of the actual samples was 75.2-105.8%, and the relative standard deviation was lower than 14.2%. Perfluorocarboxylic acid compounds were detected in differen...

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Abstract

The invention belongs to the technical field of determination of pollutants and discloses a method for determining a perfluorocarboxylic acid compound in crops. The method comprises the following main steps: freezing, drying and crushing crops to be detected, so as to obtain a sample; adding internal standard substances 13C4-PFOA (Perfluorooctanoic Acid) and 13C2-PFDA (Perfluorononanoic Acid) into the sample; after uniformly mixing, adding an extracting agent; carrying out ultrasonic extraction to obtain an extracted substance; after purifying the extracted substance through solid phase extraction of a WAX small column filled with graphite carbon black; determining by adopting a high performance liquid chromatography tandem quadrupole linear ion trap mass spectrometer; comparing with perfluorocarboxylic acid standard products which are operated in parallel, so as to carry out quantitative treatment by retention time and optimized ion characteristics; characteristic ions with less base material background interference, good peak shape and high noise to signal ratio are used as quantitative ions and are quantified through an internal standard method. The method disclosed by the invention has the advantages of high recovery rate, good precision and high sensitivity, is used for resisting complicated base material interference and is applicable to determination of the perfluorocarboxylic acid compounds in cereals, root vegetables, leaf vegetables and fruit vegetables.

Description

technical field [0001] The invention relates to the technical field of pollutant determination, in particular to a method for determining perfluorocarboxylic acid compounds in crops. Background technique [0002] Perfluoroalkyl carboxylic acids (PFCAs) refer to a class of compounds in which all hydrogen atoms connected to carbon atoms in the compound molecule are replaced by fluorine atoms, and the end of the carbon chain is connected to a carboxyl group. This type of compound is a typical perfluorinated compound, which has unique properties such as inertness, stability and high surface activity, so it is widely used as surfactants, adhesives, and additives for cosmetics and clothes. [0003] Long-term (more than 60 years) large-scale use has led to a large amount of perfluorocarboxylic acids entering the environment. At present, they have been generally detected in various environmental media and the human body. Because perfluorocarboxylic acid is rich in carbon-fluorine b...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06G01N30/14
CPCG01N30/06G01N30/14G01N30/88G01N2030/062G01N2030/146G01N2030/884
Inventor 向垒莫测辉孙腾飞陈雷余忠雄李彦文蔡全英李慧赵海明黄献培
Owner JINAN UNIVERSITY
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