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SPE Column for PFCs/PFAS Analysis

In addition to perfluorooctanesulfonic acid (PFOS) or a salt thereof already listed as Class I Specified Chemical Substances of the Chemical Substances Control Law in Japan (called Japanese TSCA), it was decided that PFOA (perfluorooctanoic acid) or a salt thereof was also listed in the same category. According to this regulation, these chemicals and mixtures are not anymore handled in the domestic market of Japan in terms of production, usage, and import.

The products introduced here are solid-phase extraction columns packed with divinyl benzene-polymethacrylate resin base. Presep® PFC-II is packed with a newly developed polymer, targeting high recovery rate in a wide range of PFCs/PFAS. They can be used as clean-up columns for PFCs, such as perfluorooctanoic acid (PFOA), perfluorooctanesulfonic acid (PFOS), and perfluorohexanesulfonic acid (PFHxS).

PFCs have heat and chemical resistance which are used as surfactant, water repellent and antifouling material. PFCs hardly decomposes and accumulates in organisms, because of highly stable. So PFCs are listed in the Stockholm Convention on POPs*.
FUJIFILM Wako provides SPE columns and solvents for PFCs analysis.

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    PFOA (PerFluoroOctanoic acid)
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    PFOS (PerFluoroOctaneSulfonic acid)
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    PFHxS (PerFluoroHexaneSulfonic acid)

*POPs(Persistent Organic Pollutants)
POPs are compounds which have resistant to environmental degradation, and bioaccumulate with potential adverse impacts on human health and the environment.

Features

  • A trace amount of PFCs with 4 to 18 carbon chains can be highly recovered
Presep® PFC-Ⅱ Presep®-C Agri (Short)
Resin Divinylbenzene polymethacrylate resin Styrene divinylbenzene-methacrylate resin
Type Syringe Type
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Cartridge Type (Closed)
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Features ・Can recover trace PFCs with 4-18 carbon chains. ・Ideal to concentrate hydrophobic trace pesticides in water samples.
・High recovery rate in pesticides even in polar metal coordinating compounds such as Ashram and Oxine copper.
Can recover PFOA・PFOS in high yield !

Additive Recovery Test (PFOA, PFOS)

  • Collection/Concentration Operation
    Water (500 mL) + Standard and Internal Standard
    Presep® PFC-Ⅱ or Presep®-C Agri (Flow rate 5 mL/min)
    Washing(H2O 5 mL)
    Dry(N2 purge)
    Extraction(0.1%NH3 in CH3OH 5 mL)
    Concentrated(→0.5 mL)
    LC/MS/MS
  • Column Conditioning
    1. 0.1%NH3 in CH3OH 4 mL
    2. CH3OH 4 mL
    3. H2O 4 mL
LC/MS/MS Conditions
  • Column: Wakopak® Ultra C18-3 2.0 mm×150 mm
    Eluent: A)10 mM CH3COONH4 in H2O, B)CH3CN
    LC/MS/MS: Prominence LC-20ADXR / LCMS 8030 plus

  • Gradient:

    Time (min) B conc. (%)
    0-1 25
    1-26 25-100
    26-30 100
    30-30.01 100-25
    30.01-35 25

Result

  • Chromatogram
    00353_img05.png

  • Recovery Result
    Monitoring Ions (m/z) Recovery Rate
    Precursor Product Presep® PFC-Ⅱ Presep®-C Agri
    PFOS 498.8 80.0 99.2% 100.9%
    PFOA 412.9 169.1 101.5% 95.0%

Additive Recovery Test (6 PFCs)*1

Collection/Concentration Operation*2

Sample
Ultrapure Water: for PFOS-PFOA Analysis
Analytical Standard: PFCs Mixture Standard Solution (PFHxS: 92 μg/L (linear), PFOS: 84 μg/L (linear), Others: each 100 μg/L (linear))
Internal Standard: Mixture Solution of 13C6 PFHxS, 13C8 PFOS, 13C8 PFOA (each 100 μg/L (linear))*3

Result

  • Chromatogram
    00353_img09.png
  • • Recovery Result
    Monitoring Ions (m/z) Recovery Rate
    Precursor Product Presep® PFC-Ⅱ
    PFHxS 398.8 80.0 101%
    PFOS 498.8 80.0 100%
    PFHxA 313.0 269.0 100%
    PFHpA 363.1 319.0 100%
    PFOA 412.9 169.1 99%
    PFNA 463.1 419.0 101%

*1 This data is an example of analysis and does not assure the analytical results using these products.
*2 Conditioning, loading, and LC/MS/MS measurement were performed in the same procedure as in above (Additive Recovery Test (PFOA, PFOS)).
*3 PFHxA, PFHpA and PFNA were corrected with 13C8 PFOA.

Additive Recovery Test (PFCs with 4-18 carbon chains)

Analysis PFC samples (16 mixture) by Wakopak® Wakosil®-II 3C18 RS

Column Wakopak® Wakosil®-II 3C18RS 2.0 mmφ, L=150 mm
Eluent A) 1 0mM CH3COONH4 in H2O, B) CH3CN
Gradient B=35-90%/0-10 min. → B=35%/10-15 min.
Detect MS/MS: 3200 Q TRAP (ABI)

Result

  • Chromatogram
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  • Recovery Result
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Product List

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Solid-Phase Extraction Columns

Presep® PFC-Ⅱ: Syringe Type
Presep®-C Agri: Cartridge Type (Closed)

HPLC Column

Solvents

※Confirmed the analytical compatibility of PFOS and PFOA

Analytical Standard

Author: Y. Nakamura

For research use or further manufacturing use only. Not for use in diagnostic procedures.

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