Method for determining perfluorooctanesulfonic acid and perfluorohexanesulfonic acid in edible parts of crops

A technology of perfluorooctane sulfonic acid and hexanesulfonic acid, which is applied in the field of pollutant determination, and achieves the effects of wide application range, good precision and high sensitivity

Active Publication Date: 2017-05-10
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 PFSAs in crops are mainly established for one or two types of crops, and for multi-type crops (including cereals, root vegetables, leafy vegetables, fruit vegetables), especially the anti-matrix effect of their edible parts And the analytical method with strong applicability has not been reported yet

Method used

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  • Method for determining perfluorooctanesulfonic acid and perfluorohexanesulfonic acid in edible parts of crops
  • Method for determining perfluorooctanesulfonic acid and perfluorohexanesulfonic acid in edible parts of crops
  • Method for determining perfluorooctanesulfonic acid and perfluorohexanesulfonic acid in edible parts of crops

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] The optimization of 2 kinds of perfluorinated sulfonic acid compounds (PFOS, PFHxS) pretreatment method in the crop of embodiment 1

[0038] Taking the edible part of leaf vegetable crops (lettuce) as the test sample, the effect of the type of extraction agent, the type of purification column and the amount of active graphite carbon black on the perfluorosulfonic acid in the edible part of the crop was investigated through the standard recovery experiment (10ng / g). Compound (PFOS, PFHxS) recovery rate, so as to obtain an optimized pretreatment method. The extraction solvents investigated include the following three kinds: TBA pair-MTBE extraction (TBA-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, 50 mg.

[0039] 1. The specific im...

Embodiment 2

[0047] The applicability verification of the edible part of different kinds of crops of the optimized pretreatment method of embodiment 2

[0048] The edible parts of cereal crops (rice), root vegetables (carrots), leaf vegetables (lettuce), and fruit vegetables (pumpkins) were used as test materials, and the recovery rate experiments of different concentrations (0.5, 10, 25, 50ng / g ) Investigate the applicability of embodiment 1 to establish the optimal pretreatment method.

[0049] 1. The specific implementation process of this embodiment

[0050] (1) Sample preparation: Edible samples of different types of blank crops (rice, carrot, lettuce, pumpkin) were frozen, dried, ground and mixed, and stored in a 4°C refrigerator for later use.

[0051] (2) The configuration of the standard curve of the target PFSAs compound in the edible part of each crop: the edible part samples of different types of blank crops were taken out, and the extraction matrix of the edible part of each ...

Embodiment 3

[0063] Embodiment 3 establishes the method to the mensuration of actual sample

[0064] In order to verify the feasibility of the method of the present invention, the actual sample measurement is carried out by this method. The actual samples were collected from the farmland around a fluorine chemical factory in a large city in southern my country. The samples included cabbage (2 types), lettuce (7 types), mustard greens (9 types), pakchoi (3 types) and celery (3 types) . According to the specific implementation process of Example 1 and Example 2, the analysis and determination of the edible part PFSAs (PFOS, PFHxS) of the above-mentioned sample is carried out, and the quality control sample (0.5, 10, 25, 50ng / g). The measurement results are shown in Table 3-1 and 3-2. The recovery rate of the edible part of the actual sample is 81-105%, and the relative standard deviation is less than 12%. The target PFSAs (PFOS, PFHxS) compounds were detected in varying degrees in cabbage...

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Abstract

The invention belongs to the technical field of contaminant determination and discloses a method for determining perfluorooctanesulfonic acid and perfluorohexanesulfonic acid in edible parts of crops. The method comprises the main steps: freezing, drying and crushing the edible parts of the crops so as to obtain a sample, adding an internal standard substance into the sample, carrying out uniform mixing, then, adding a disassociation agent into the mixture for a disassociation reaction, then, adding tetrabutylammonium bisulfate and a sodium carbonate buffer solution into the reaction solution, carrying out uniform mixing thoroughly, then, adding methyl tert-butyl ether into the mixture for ultrasonic extraction, so as to obtain an extract; subjecting the extract to solid-phase extraction purification by graphite carbon black loaded WAX columellae so as to obtain sample detection liquid, and determining the sample detection liquid by adopting an HPLC-MS-MS method. According to the method disclosed by the invention, the recovery rate is high, the accuracy is good, the sensitivity is high, and the method is resistant to interference of complicated matrixes; meanwhile, the method is applicable to the determination on perfluorooctanesulfonic acid and perfluorohexanesulfonic acid 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 perfluorooctylsulfonic acid and perfluorohexanesulfonic acid in edible parts of crops. Background technique [0002] Perfluorinated compounds (PFCs), as new organic pollutants, have aroused great concern from the international community due to their extremely high persistence, bioaccumulation and toxicity. Perfluoroalkyl sulfonic acids (PFSAs) are a typical class of perfluorinated compounds, in which all hydrogen atoms connected to carbon atoms in the molecule are replaced by fluorine atoms, and a sulfonic acid group is attached to the end of the carbon chain. PFSAs have high inertness, stability and high surface activity, so in the past 60 years, they have been widely used as surfactants, fire extinguishing foams, food container materials, and additives for clothing, cosmetics, etc.; resulting in a large number of PFSAs entering the envir...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
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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