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Presep® PFC-Ⅱ

SPE Column for PFCs Analysis

These 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. They can be used as clean-up columns for PFCs, such as perfluorooctanoic acid (PFOA) and perfluorooctanesulfonic acid (PFOS).

Features

  • Trace PFCs in water can be efficiently recovered. Presep® PFC-II can recover 16 PFCs.
  • 16 components can be analyzed simultaneously and quickly by combining with Wakopak® Wakosil-II 3C18 RS.
  • Blank caused by solvent can be reduced by combining with a solvent for PFOS or PFOA analysis.

Additive Recovery Test

  • Solid phase extraction conditions

    Column conditioning

    column: Presep® PFC-Ⅱ

    1. CH3OH with 0.1 %NH4OH 10 mL
    2. CH3OH 5 mL
    3. H2O 5 mL*1

    column: Presep®-C PFC

    1. CH3OH 10 mL
    2. H2O 5 mL*1

    Collection/concentration procedure

    1) Water sample (additive recovery experiment: Addition of standard to 1 L of purified water)
    2) Charge of water into column (flow: 10-20 mL/min)
    3) Drying (air purging*2 or nitrogen gas purging)
    4) Elution: Amount of solvent: 2 mL*3
    5) LC-MS/MS measurement

    *1: Ion exchange water fed into unused Presep® cartridge which has been exposed to recovery experiment is used. Ultrapure water for PFOs/PFOA analysis (212-01363) can be used.]

    *2: Contamination from air can be prevented by connecting unused Presep® in the previous stage of the column which has collected the sample and sucking air.

    *3: The eluate is concentrated by nitrogen gas purging according to the measurement sensitivity, and the quantity is measured.
    (Eluent: Presep® PFC-Ⅱ=CH3OH with 0.1 %NH4OH 2 mL, Presep®-C PFC=CH3OH 2 mL)

  • Results of recovery

    Peak No. Sample Name Presep®PFC-Ⅱ
    Recovery (%)
    Presep®C-PFC
    Recovery (%)
    Q1/Q3
    4 PFBS 106 - 298.8/ 79.6
    7 PFHxS 116 76 398.8/ 79.6
    10 PFOS 107 86 498.8/ 79.6
    13 PFDS 107 91 598.9/ 79.9
    1 PFBA 120 - 212.9/168.9
    2 PFPeA 116 - 262.8/219.1
    3 PFHxA 109 - 312.9/268.6
    5 PFHpA 110 - 362.8/318.7
    6 PFOA 110 88 412.9/368.9
    8 PFNA 109 96 462.7/418.8
    9 PFDA 110 91 512.9/469.0
    11 PFUnDA 108 90 562.9/519.0
    12 PFDoDA 109 89 612.9/568.9
    14 PFTeDA 97 - 712.9/669.0
    15 PFHexDA 105 - 812.9/769.0
    16 PFODA 103 - 912.8/168.9

    *The components indicated by boldface are assayed in product test.

Result by LC-MS/MS

00994_img01.png
  • HPLC conditions
    Column :Wakopak® Wakosil-Ⅱ 3C18 RS, 2.0 mmφ x 150 mm
    Eluent :A)10 mM CH3COONH4 in H2O B)CH3CN
    Gradient :0-10 min. B 35-90 %, 10-15min. B 35 %
    Flow Rate :0.2 mL/min, at 40 ℃
    Injection Vol. :5 μL each 10 ng/mL (CH3OH)(PFBA: 50 ng/mL, PFODA: 20 ng/mL)
    Sample : 1)PFBA, 2)PFPeA, 3)PFHxA, 4)PFBS, 5)PFHpA, 6)PFOA, 7)PFHxS, 8)PFNA, 9)PFDA, 10)PFOS, 11)PFUnDA, 12)PFDoDA, 13)PFDS, 14)PFTeDA, 15)PFHexDA, 16)PFODA
  • MS/MS conditions
    ESI, MRM
    Ion Spray Voltage : -4500V (neg)
    Temperature : 400 ℃
    Curtain Gas : 30
    Collision Gas : 3
    Ion Source Gas 1 : 70
    Ion Source Gas 2 : 80

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Author: Y. Higai

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