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Method for quantitatively detecting perfluorooctane sulfonate isomeride in water sample

A technology of perfluorooctane sulfonate and isomers, which is applied in the field of detection of perfluorooctane sulfonate isomers in water samples, can solve the problems of PFOS quantitative error and other problems, and achieve quantitative error , Simplify the derivatization process and improve the effect of reproducibility

Active Publication Date: 2015-04-01
NANJING UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0006] The purpose of the present invention is to overcome the deficiencies in the prior art, to provide a method for quantitative detection of perfluorooctane sulfonic acid isomers in water samples, which can solve the problem of quantitative error in the detection of PFOS in the prior art

Method used

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  • Method for quantitatively detecting perfluorooctane sulfonate isomeride in water sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Detection of PFOS isomers in surface water

[0028] 1. Instruments and reagents

[0029] Thermo Trace Ultra gas chromatograph equipped with Thermo Trace DSQ II single quadrupole mass spectrometer (Thermo Scientific, USA); DB-5ms gas chromatography column, 0.25 mm × 30 m, 0.25 μm (J&K Scientific, USA); solid phase extraction device ( Waters, Milford, MA, USA); Oasis WAX SPE cartridge, 6 cc, 150 mg, 30 μm (Waters, Milford, MA, USA); surface water sample (Taihu Lake).

[0030] Methanol: HPLC grade, purchased from Tedia (Fairfield, OH, USA); Ammonium acetate: HPLC grade, purchased from CNW (Duesseldorf, Germany); Acetic acid: >99.8%, HPLC grade, purchased from CNW (Duesseldorf, Germany ); ammonia water: ~10%, HPLC grade, purchased from CNW (Duesseldorf, Germany); tetrabutylammonium hydroxide aqueous solution: 10%, AR, purchased from Sinopharm Chemical Reagents (Shanghai, China); Octanesulfonic acid (L-PFOS); 1-trifluoromethyl-perfluoroheptanesulfonic acid (1m-PFOS); 2-tri...

Embodiment 2

[0042] Example 2 Content detection of PFOS isomers in drinking water

[0043] 1. Instruments and reagents

[0044] With the instrument and reagent in example 1.

[0045] 2. Instrument conditions

[0046] With the instrument condition in example 1

[0047] 3. Drinking water samples

[0048] Collect 12 drinking water samples from different regions in Jiangsu, and collect 1L water samples at each sampling point.

[0049] 4. Steps for the analysis of PFOS isomers

[0050] With the analysis step in example 1, the water sample measures 1L and carries out solid phase extraction

[0051] 5. Test results.

[0052] The results showed that all 7 PFOS isomers were detected in Taihu Lake water samples. The test results are as follows:

[0053] compound L-PFOS 1m-PFOS 2m-PFOS 3m-PFOS 4m-PFOS 5m-PFOS 6m-PFOS scope 0.94-9.5 0.10-0.53 0.05-0.32 0.06-0.77 0.05-0.54 0.11-0.86 0.26-3.3 average value 3.56 0.18 0.08 0.33 0.23 0.35 1.0 ...

Embodiment 3

[0054] Example 3 Construction and detection limit of standard curve for isomers of perfluorooctane sulfonic acid

[0055] The chromatographic conditions and mass spectrometry conditions of the perfluorooctane sulfonic acid isomer detection instrument are the same as those in Example 1.

[0056] Dilute the standard substance of perfluorooctane sulfonate isomers with methanol to 1mg / L as a stock solution; use methanol to dilute to 0.2, 0.5, 1, 2, 5, 10, 20, 50, 100μg / L series of standard solutions. Take 100 μL of standard solution, blow dry with nitrogen, add 100 μL of derivatization reagent and 1 mL of methyl tert-butyl ether, mix well, and blow dry again, add 100 μL of methyl tert-butyl ether and mix evenly, use gas chromatography- Mass spectrometry was used to determine the isomers of PFOS in the standard solution. A standard curve was drawn according to the obtained peak area and the corresponding concentration of each isomer of PFOS. The linear range obtained through the...

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Abstract

The invention provides a method for quantitatively detecting perfluorooctane sulfonate isomeride in a water sample, which belongs to the field of perfluorooctane sulfonate monitoring. The method for quantitatively detecting the perfluorooctane sulfonate isomeride in the water sample comprises the steps of (1) solid phase extraction: quantitatively taking the water sample, carrying out extraction with a solid phase extraction column, carrying out centrifugation to eliminate moisture in the extraction column after extraction, then purifying the dried extraction column by a buffer solution and methanol, eluting the purified extraction column with alkaline methanol, and collecting an eluant; (2) chemical processing of an extract: drying nitrogen of the eluant with wind, adding derivatization reagents, tetrabutylammonium hydroxide and methyl tertiary butyl ether, to be mixed, drying the solution nitrogen with wind, and adding the methyl tertiary butyl ether to be uniformly mixed so as to keep the volume constant; and (3) gas chromatography-mass spectrometric detection. The method successfully realizes the effective separation of the PFOS (perfluorooctane sulfonate) isomeride so as to realize the accurate and quantitative detection of the PFOS isomeride. Compared with the existing test technology, the method realizes the quantitative analysis and detection of the PFOS isomeride, and solves the problem of quantitative errors of PFOS.

Description

technical field [0001] The invention relates to a gas chromatography-mass spectrometry detection method for perfluorooctane sulfonic acid, in particular to a detection method for perfluorooctane sulfonic acid isomers in water samples. Background technique [0002] Perfluorooctane sulfonic acid (PFOS), because of its excellent hydrophobic and oleophobic properties and surface activity, is widely used in textiles, electroplating, fire extinguishers, paper and other industries. At the same time, due to its strong environmental persistence and high bioaccumulation, PFOS has been found to have global migration characteristics and toxicity to multiple organs throughout the body, and has attracted widespread attention. PFOS was also included in Schedule B of the POPs Convention in May 2009, which means that the production and use of PFOS are restricted globally. At the same time, in order to maintain human health and reduce ecological risks, the United States and Germany have formu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 韦斯于南洋于红霞史薇苏冠勇
Owner NANJING UNIV
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