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Submitted URL:
https://www.restek.com/technical-literature-library/articles/integrating-the-analysis-of-ultrashort-chain-PFAS/?utm_med...
Effective URL:
https://www.restek.com/row/technical-literature-library/articles/integrating-the-analysis-of-ultrashort-chain-PFAS/?utm...
Submission: On February 24 via api (February 24th 2023, 5:28:55 pm UTC) from US — Scanned from DE

Form analysis
10 forms found in the DOM

POST /PublicApi/InternalLogin

<form action="/PublicApi/InternalLogin" method="post" role="form" novalidate="novalidate"><input name="__RequestVerificationToken" type="hidden"
    value="DAEc1O92BoyN1cEyxL9RkzLBjgsv0vKenWtO0c4awhirQM7wsHQok9JSAUCkgcvw_P7EZ9HCZuVLHooWFGHvl89qUwTDGaLMIpg2RFdFF281"><input id="LoginViewModel_ReturnUrl" name="LoginViewModel.ReturnUrl" type="hidden" value="">
  <li class="offside-navbar--menu__item">
    <div class="form-group">
      <label class="label" for="LoginViewModel_UserName">Username:</label>
      <input autofocus="autofocus" class="textbox" data-val="true" data-val-required="Username is required" id="LoginViewModel_UserName" name="LoginViewModel.UserName" type="text" value="" data-uw-rm-form="nfx">
      <span class="field-validation-valid" data-valmsg-for="LoginViewModel.UserName" data-valmsg-replace="true"></span>
    </div>
  </li>
  <li class="offside-navbar--menu__item">
    <div class="form-group">
      <label class="label" for="LoginViewModel_Password">Password</label>
      <input class="textbox" data-val="true" data-val-required="Password is required" id="LoginViewModel_Password" name="LoginViewModel.Password" type="password" data-uw-rm-form="nfx">
      <span class="field-validation-valid" data-valmsg-for="LoginViewModel.Password" data-valmsg-replace="true"></span>
    </div>
  </li>
  <li class="offside-navbar--menu__item">
    <div class="form-check">
      <input class="form-check-input" data-val="true" data-val-required="The Remember me field is required." id="LoginViewModel_RememberMe" name="LoginViewModel.RememberMe" type="checkbox" value="true"><input name="LoginViewModel.RememberMe"
        type="hidden" value="false">
      <label class="form-check-label"> Remember Me </label>
    </div>
  </li>
  <li class="offside-navbar--menu__item">
    <div class="header-box__bottom">
      <button type="button" class="button-black jsUsersSigninBtn">
        <span>Login</span>
      </button>
    </div>
  </li>
  <li class="offside-navbar--menu__item">
    <a class="forgot-word" href="/row/pages/reset-password/" data-uw-rm-brl="false">Forgot your password?</a>
  </li>
</form>

POST /Locale/Set?language=en

<form action="/Locale/Set?language=en" method="post"><input name="__RequestVerificationToken" type="hidden" value="WchMWwen9khqrI08TN6bknyfPHjXi59HDI3FnBy9eRxAk9G7nyphnguqgbkF5PVw4u3GSuNfVZKwtdiMuqL1XMsOTGkTG21dgjsQ5EZDmnQ1"> <button
    class="btn btn-none locale-list__item jsSelectLocale">
    <img src="/app_themes/default/images/flags/en.gif" class="locale-selector__locale-icon" role="presentation" data-uw-rm-ima="un">
    <p class="locale-selector__locale-text">U.S. (ENGLISH)</p>
  </button>
</form>

POST /Locale/Set?language=fr

<form action="/Locale/Set?language=fr" method="post"><input name="__RequestVerificationToken" type="hidden" value="YlJMZEJKHpG6WipurfjTul5G3fuvEPzkW3TtRI_C88Ww4vnkcAQn0B4IBOQOMWxxKCLor5Blgyy31u9ngmLf7b7ifE4lNluruTddiMkgOs01"> <button
    class="btn btn-none locale-list__item jsSelectLocale">
    <img src="/app_themes/default/images/flags/fr.gif" class="locale-selector__locale-icon" role="presentation" data-uw-rm-ima="un">
    <p class="locale-selector__locale-text">FRANCE (FRANҪAIS)</p>
  </button>
</form>

POST /Locale/Set?language=it

<form action="/Locale/Set?language=it" method="post"><input name="__RequestVerificationToken" type="hidden" value="lBkS6GpRjCu_y3KZXTNlv2KbZ_0nE1toRue-B2Y0vUcPdFl7O8GbOZVLR5z0ljXCXawiE_Ix-T_YMnbMdAvnEhqyGUGmGOnlSiuWzyj1KlY1"> <button
    class="btn btn-none locale-list__item jsSelectLocale">
    <img src="/globalassets/world-flags/it_EZ.gif" class="locale-selector__locale-icon" role="presentation" data-uw-rm-ima="un">
    <p class="locale-selector__locale-text">ITALIA (ITALIANO)</p>
  </button>
</form>

POST /Locale/Set?language=ja

<form action="/Locale/Set?language=ja" method="post"><input name="__RequestVerificationToken" type="hidden" value="SDaSxIf2l42fRHV_2cR6OpM6XcvQNHR14kQPW1zEWlV-ytXnsO1cDf-t_dShKZEQqXU7pI1LK_0821QH04THhq3aN5V8uIQNmYuUa8lwxqg1"> <button
    class="btn btn-none locale-list__item jsSelectLocale">
    <img src="/globalassets/world-flags/ja_EZ.gif" class="locale-selector__locale-icon" role="presentation" data-uw-rm-ima="un">
    <p class="locale-selector__locale-text">日本 (日本語)</p>
  </button>
</form>

POST /Locale/Set?language=row

<form action="/Locale/Set?language=row" method="post"><input name="__RequestVerificationToken" type="hidden" value="vxk1mcumXYGwhyK97vSwpYUVaRN6aCqG9taISpwSE06fJrfoN49vUQELClA0I23gdcUcRRZLZ-FlWm_83gQ4LJ5FE46hhWh_ngaZ8a_PMMM1"> <button
    class="btn btn-none locale-list__item jsSelectLocale">
    <img src="/globalassets/world-flags/en_ROW.gif" class="locale-selector__locale-icon" role="presentation" data-uw-rm-ima="ai" alt="decorative">
    <p class="locale-selector__locale-text">GLOBAL (ENGLISH)</p>
  </button>
</form>

POST /PublicApi/RegisterAccount

<form action="/PublicApi/RegisterAccount" method="post" role="form" novalidate="novalidate"><input name="__RequestVerificationToken" type="hidden"
    value="6M-r3RkgkPCu0PGXVga9_YQVA393dSYGQ6g6yJr5vKOILo_fTsfBDSgqYBEvYHo-tx6y7Xg2orhF_XgqE8BKHR7QUaqsa6a4LZfrvSVVtKo1"><input data-val="true" data-val-length="The field Name must be a string with a maximum length of 100." data-val-length-max="100"
    data-val-required="Name is required" id="RegisterAccountViewModel_Address_Name" name="RegisterAccountViewModel.Address.Name" type="hidden" value="Default Address">
  <li>
    <div class="form-group">
      <label class="label" for="RegisterAccountViewModel_Email">Email Address</label>
      <input class="textbox-small" data-val="true" data-val-regex="You have to enter a valid email address" data-val-regex-pattern="^([0-9a-zA-Z]([-.\w]*[0-9a-zA-Z])*@([0-9a-zA-Z][-\w]*[0-9a-zA-Z]\.)+[a-zA-Z]{2,9})$"
        data-val-required="Email is required" id="RegisterAccountViewModel_Email" name="RegisterAccountViewModel.Email" type="text" value="" data-uw-rm-form="nfx">
      <span class="field-validation-valid" data-valmsg-for="RegisterAccountViewModel.Email" data-valmsg-replace="true"></span>
    </div>
  </li>
  <li>
    <div class="form-group">
      <label class="label" for="RegisterAccountViewModel_Password">Password</label>
      <input class="textbox-small" data-val="true" data-val-length="Your password has to be between 5 and 100 characters long" data-val-length-max="100" data-val-length-min="5" data-val-required="Password is required"
        id="RegisterAccountViewModel_Password" name="RegisterAccountViewModel.Password" type="password" data-uw-rm-form="nfx">
      <span class="field-validation-valid" data-valmsg-for="RegisterAccountViewModel.Password" data-valmsg-replace="true"></span>
    </div>
  </li>
  <li>
    <div class="form-group">
      <label class="label" for="RegisterAccountViewModel_Password2">Confirm Password</label>
      <input class="textbox-small" data-val="true" data-val-length="Your password has to be between 5 and 100 characters long" data-val-length-max="100" data-val-length-min="5" data-val-required="Confirm Password is required"
        id="RegisterAccountViewModel_Password2" name="RegisterAccountViewModel.Password2" type="password" data-uw-rm-form="nfx">
      <span class="field-validation-valid" data-valmsg-for="RegisterAccountViewModel.Password2" data-valmsg-replace="true"></span>
    </div>
  </li>
  <li>
    <div class="form-group">
      <div class="row">
        <div class="col-md-6">
          <label class="label" for="RegisterAccountViewModel_Address_FirstName">First Name</label>
          <input class="textbox-small" id="RegisterAccountViewModel_Address_FirstName" name="RegisterAccountViewModel.Address.FirstName" type="text" value="" data-uw-rm-form="nfx">
          <span class="field-validation-valid" data-valmsg-for="RegisterAccountViewModel.Address.FirstName" data-valmsg-replace="true"></span>
        </div>
        <div class="col-md-6">
          <label class="label" for="RegisterAccountViewModel_Address_LastName">Last Name</label>
          <input class="textbox-small" id="RegisterAccountViewModel_Address_LastName" name="RegisterAccountViewModel.Address.LastName" type="text" value="" data-uw-rm-form="nfx">
          <span class="field-validation-valid" data-valmsg-for="RegisterAccountViewModel.Address.LastName" data-valmsg-replace="true"></span>
        </div>
      </div>
    </div>
  </li>
  <li>
    <div class="form-group">
      <label class="label" for="RegisterAccountViewModel_Address_Line1">Address Line 1</label>
      <input class="textbox-small" data-val="true" data-val-length="The field Address Line 1 must be a string with a maximum length of 35." data-val-length-max="35" data-val-required="Shipping address is required"
        id="RegisterAccountViewModel_Address_Line1" name="RegisterAccountViewModel.Address.Line1" type="text" value="" data-uw-rm-form="nfx">
      <span class="field-validation-valid" data-valmsg-for="RegisterAccountViewModel.Address.Line1" data-valmsg-replace="true"></span>
    </div>
  </li>
  <li>
    <div class="form-group">
      <label class="label" for="RegisterAccountViewModel_Address_Line2">Dept / Bldg / Room</label>
      <input class="textbox-small" data-val="true" data-val-length="The field Dept / Bldg / Room must be a string with a maximum length of 35." data-val-length-max="35" id="RegisterAccountViewModel_Address_Line2"
        name="RegisterAccountViewModel.Address.Line2" type="text" value="" data-uw-rm-form="nfx">
      <span class="field-validation-valid" data-valmsg-for="RegisterAccountViewModel.Address.Line2" data-valmsg-replace="true"></span>
    </div>
  </li>
  <li>
    <div class="form-group">
      <div class="row">
        <div class="col-md-8">
          <label class="label" for="RegisterAccountViewModel_Address_City">City</label>
          <input class="textbox-small" data-val="true" data-val-required="City is required" id="RegisterAccountViewModel_Address_City" name="RegisterAccountViewModel.Address.City" type="text" value="" data-uw-rm-form="nfx">
          <span class="field-validation-valid" data-valmsg-for="RegisterAccountViewModel.Address.City" data-valmsg-replace="true"></span>
        </div>
        <div class="col-md-4">
          <label class="label" for="RegisterAccountViewModel_Address_PostalCode">Postal Code</label>
          <input class="textbox-small" data-val="true" data-val-length="The field Postal Code must be a string with a maximum length of 20." data-val-length-max="20" data-val-required="Zip code is required"
            id="RegisterAccountViewModel_Address_PostalCode" name="RegisterAccountViewModel.Address.PostalCode" type="text" value="" data-uw-rm-form="nfx">
          <span class="field-validation-valid" data-valmsg-for="RegisterAccountViewModel.Address.PostalCode" data-valmsg-replace="true"></span>
        </div>
      </div>
    </div>
  </li>
  <li>
    <div class="form-group">
      <label class="label" for="RegisterAccountViewModel_Address_CountryCode">Country</label>
      <div class="row jsCountrySelectionContainer jsCountrySelectionRegisterUser">
        <input type="hidden" class="jsCountryOptionName" value="RegisterAccountViewModel.Address.CountryCode">
        <div class="col-12 jsCountryOptionListing">
          <div class="dropdown" style="">
            <div class="dropdown__selected">
              <span class="current">Click to expand</span>
              <span><svg xmlns="http://www.w3.org/2000/svg" width="24" height="24" viewBox="0 0 24 24" fill="none" stroke="currentColor" stroke-width="2" stroke-linecap="round" stroke-linejoin="round" class="feather feather-chevron-down">
                  <polyline points="6 9 12 15 18 9"></polyline>
                </svg></span>
            </div>
            <ul class="dropdown__group">
            </ul>
          </div>
        </div>
      </div>
      <span class="field-validation-valid" data-valmsg-for="RegisterAccountViewModel.Address.CountryCode" data-valmsg-replace="true"></span>
      <input id="address-htmlfieldprefix" name="address-htmlfieldprefix" type="hidden" value="RegisterAccountViewModel.Address">
    </div>
  </li>
  <li>
    <div class="form-group jsCountryRegionContainer">
    </div>
  </li>
  <li>
    <div class="form-check">
      <label class="form-check-label">
        <input class="form-check-input" data-val="true" data-val-required="The Newsletter field is required." id="RegisterAccountViewModel_Newsletter" name="RegisterAccountViewModel.Newsletter" type="checkbox" value="true"><input
          name="RegisterAccountViewModel.Newsletter" type="hidden" value="false"> Send me email updates about the latest products and promotions. </label>
    </div>
  </li>
  <li>
    <button type="submit" class="button-black--icon jsUsersSignupBtn" data-uw-rm-form="submit">Submit</button>
  </li>
</form>

GET /row/site-search-results/

<form class="w-75 mt-4 js-bravo-site-search-form" method="GET" action="/row/site-search-results/">
  <div class="input-group">
    <input class="js-bravo-sync-query js-bravo-autocomplete-open-trigger form-control border-right-0 rounded-0" placeholder="Search Products, Resources, Articles, and more." name="query" aria-label="search products, resources, articles, and more."
      data-uw-rm-form="fx">
    <div class="input-group-append">
      <button class="input-group-text border-left-0 rounded-0 bg-transparent js-bravo-search-submit-button" disabled="" aria-label="search" data-uw-rm-empty-ctrl="">
        <svg xmlns="http://www.w3.org/2000/svg" width="20" height="20" viewBox="0 0 24 24" fill="none" stroke="currentColor" stroke-width="2" stroke-linecap="round" stroke-linejoin="round" class="feather feather-search icon-right"
          style="color: #999;">
          <circle cx="11" cy="11" r="8"></circle>
          <line x1="21" y1="21" x2="16.65" y2="16.65"></line>
        </svg>
      </button>
    </div>
  </div>
</form>

POST /api/email/SendEmail

<form action="/api/email/SendEmail" method="post" data-block-guid="98425bd8-aa2e-44b8-9bd2-f346b993eaf6" class="js-email-form js-email-form-98425bd8-aa2e-44b8-9bd2-f346b993eaf6">
  <div role="document" class="modal-dialog modal-lg modal-dialog-scrollable">
    <div class="modal-content rounded-0">
      <div class="modal-header">
        <h5 class="modal-title" data-uw-rm-heading="level" role="heading" aria-level="4">Restek Help</h5> <button type="button" data-dismiss="modal" aria-label="Close" class="close"><span aria-hidden="true">×</span></button>
      </div>
      <div class="modal-body"><input type="hidden" name="contentId" value="98425bd8-aa2e-44b8-9bd2-f346b993eaf6"> <input type="hidden" name="languageId" value="en-001">
        <div class="form-group js-input-group-subject"><label for="subject" class=" is-required"> Subject </label> <input type="text" id="subject" name="subject" required="required" value="" class="form-control js-subject" data-uw-rm-form="nfx">
          <div class="invalid-feedback"> Invalid value entered </div>
        </div>
        <div class="form-group js-input-group-message"><label for="message" class=" is-required"> Message </label> <textarea id="message" name="message" required="required" class="form-control js-message" data-uw-rm-form="nfx"></textarea>
          <div class="invalid-feedback"> Invalid value entered </div>
        </div>
        <div class="form-group js-input-group-fullname"><label for="fullname" class=" is-required"> Your Full Name </label> <input type="text" id="fullname" name="fullname" required="required" value="" class="form-control js-fullname"
            data-uw-rm-form="nfx">
          <div class="invalid-feedback"> Invalid value entered </div>
        </div>
        <div class="form-group js-input-group-email"><label for="email" class=" is-required"> Your Email </label> <input type="email" id="email" name="email" required="required" value="" class="form-control js-email" data-uw-rm-form="nfx">
          <div class="invalid-feedback"> Invalid value entered </div>
        </div>
        <div class="form-group js-input-group-phoneNumber"><label for="phoneNumber" class=" "> Phone Number </label> <input type="text" id="phoneNumber" name="phoneNumber" value="" class="form-control js-phoneNumber" data-uw-rm-form="nfx">
          <div class="invalid-feedback"> Invalid value entered </div>
        </div>
        <div class="form-group js-input-group-company"><label for="company" class=" is-required"> Company Name </label> <input type="text" id="company" name="company" required="required" value="" class="form-control js-company" data-uw-rm-form="nfx">
          <div class="invalid-feedback"> Invalid value entered </div>
        </div>
        <div class="form-group js-input-group-address"><label for="address" class=" is-required"> Address </label> <input type="text" id="address" name="address" required="required" value="" class="form-control js-address" data-uw-rm-form="nfx">
          <div class="invalid-feedback"> Invalid value entered </div>
        </div>
        <div class="form-group js-input-group-address2"><label for="address2" class=" "> Address 2 </label> <input type="text" id="address2" name="address2" value="" class="form-control js-address2" data-uw-rm-form="nfx">
          <div class="invalid-feedback"> Invalid value entered </div>
        </div>
        <div class="form-group js-input-group-city"><label for="city" class=" is-required"> City </label> <input type="text" id="city" name="city" required="required" value="" class="form-control js-city" data-uw-rm-form="nfx">
          <div class="invalid-feedback"> Invalid value entered </div>
        </div>
        <div class="form-group js-input-group-stateProvince"><label for="stateProvince" class=" is-required"> State / Province </label> <input type="text" id="stateProvince" name="stateProvince" required="required" value=""
            class="form-control js-stateProvince" data-uw-rm-form="nfx">
          <div class="invalid-feedback"> Invalid value entered </div>
        </div>
        <div class="form-group js-input-group-postalCode"><label for="postalCode" class=" is-required"> Postal Code </label> <input type="text" id="postalCode" name="postalCode" required="required" value="" class="form-control js-postalCode"
            data-uw-rm-form="nfx">
          <div class="invalid-feedback"> Invalid value entered </div>
        </div>
        <div class="form-group js-input-group-country"><label for="country" class=" is-required"> Country </label> <input type="text" id="country" name="country" required="required" value="" class="form-control js-country" data-uw-rm-form="nfx">
          <div class="invalid-feedback"> Invalid value entered </div>
        </div> <label for="attachments" class="font-weight-bold"> Attachment(s) <span class="font-weight-normal">optional)</span></label>
        <div class="input-group mb-3">
          <div class="custom-file"><input type="file" id="attachments" name="attachments" multiple="multiple" class="custom-file-input"> <label for="attachments" aria-describedby="attachments" class="custom-file-label">Choose File(s)</label></div>
        </div>
        <div> * = required </div>
        <div class="form-group" style="position: absolute; width: 0px; height: 0px; top: 0px; left: 0px; overflow: hidden; z-index: -1;"><label for="AdditionalData">Leave this field blank</label> <input aria-hidden="true" name="AdditionalData"
            tabindex="-1" type="text" class="form-control" data-uw-rm-form="fx"></div>
      </div>
      <div class="modal-footer"><button type="submit" class="js-submit-form btn btn-primary w-100" data-uw-rm-form="submit">Submit</button></div>
    </div>
  </div>
</form>

<form class="js-quick-order-modal-form">
  <div class="row">
    <div class="col-8">
      <div class="form-group">
        <label class="is-required" for="Sku">Sku</label>
        <input class="form-control" id="Sku" name="Sku" type="text" required="" data-uw-rm-form="nfx">
        <div class="invalid-feedback js-err-msg d-none"></div>
      </div>
    </div>
    <div class="col-4">
      <div class="form-group">
        <label class="is-required" for="Qty">Qty</label>
        <input class="form-control" id="Qty" name="Qty" type="text" value="1" required="" data-uw-rm-form="nfx">
        <div class="invalid-feedback js-err-msg d-none"></div>
      </div>
    </div>
  </div>
</form>

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 * Home
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 * Integrating the Analysis of Ultrashort-Chain PFAS


INTEGRATING THE ANALYSIS OF ULTRASHORT-CHAIN PFAS


METHOD DEVELOPMENT FOR SIMULTANEOUS ANALYSIS OF ULTRASHORT-CHAIN, ALTERNATIVE,
AND LEGACY PFAS

By Shun-Hsin Liang and Mike Chang

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ABSTRACT

A simple direct injection LC-MS/MS method was developed and evaluated for the
simultaneous analysis of ultrashort-chain, alternative, and legacy per- and
polyfluoroalkyl substances (PFAS) in various water samples. This method is
recommended for labs wanting to use a single procedure to analyze compounds from
all three PFAS categories in potable and non-potable waters.


INTRODUCTION

LC-MS/MS methods for the analysis of legacy short-chain (C4, C5) and long-chain
(>C5) per- and polyfluoroalkyl substances (PFAS) based on reversed-phase (RP)
chromatography are well established. With proper modification, these methods
often can also be used for LC-MS/MS analysis of alternative PFAS, such as
HFPO-DA (GenX) and ADONA, which are perfluoroalkyl ether carboxylic acids used
as PFOA substitutes. Similarly, F-53B is a PFOS alternative produced in China
that contains two polyfluoroalkyl ether sulfonate components, 9Cl-PF3ONS and
11Cl-PF3OUdS, which are included as analytes in the updated EPA 537.1 method.
However, current LC methods may not be suitable for the analysis of newly
trending ultrashort-chain (C2, C3) PFAS, mainly due to their insufficient
retention on typical RP columns.

While the use of short-chain PFAS (PFBA and PFBS) is intentional, numerous
studies have shown the ubiquitous occurrence of C2 and C3 PFAS in aqueous
environmental samples [1,2]. These include trifluoroacetic acid (TFA),
perfluoropropanoic acid (PFPrA), perfluoroethane sulfonate (PFEtS), and
perfluoropropane sulfonate (PFPrS). It was shown that PFPrA is the predominant
PFAS (up to 45% of total detectable PFAS) in rain and snow samples collected
from the U.S., France, and Japan [3]. To date, there is no definitive
identification of contamination sources and levels for these ultrashort-chain
PFAS, but a recent study detected PFEtS and PFPrS in aqueous film-forming foams
(AFFFs) and groundwaters from 11 military bases in the U.S. (often used for fire
department training exercises) [4], indicating AFFF firefighting foam may be a
source of ultrashort-chain PFAS.

Currently, methods that allow the desired combined analysis of ultrashort-chain
PFAS with alternative and legacy PFAS are very rare. To fill this gap, we
developed a procedure for the simultaneous quantification of a wide range of
chain lengths and structures including C3, C4, C8, and alternative PFAS in a
variety of water samples.


EXPERIMENTAL


SAMPLE PREPARATION

In a polypropylene vial, 250 µL water sample aliquots were mixed with 250 µL of
40:60 reagent water:methanol and 5 µL of internal standard solution (5 ng/mL
of 13C2-PFHxA, 13C2-PFOA, 13C4-PFOS in methanol). The vial was capped with a
polyethylene cap and injected for analysis.


CALIBRATION STANDARDS AND QUALITY CONTROL SAMPLES

Calibration standards were prepared by fortifying reagent water (Optima LC-MS
water) with ten PFAS analytes across a range of 5–400 ng/L. The calibration
standard solutions were then processed as described in the sample preparation
procedure.


FORTIFIED WATER SAMPLES

Samples of tap water collected from the Restek facility and three diverse water
types (Chicago river water, groundwater, and publicly owned treatment works
[POTW] effluent water) supplied by the U.S. EPA were included in this study.
Each water type was fortified at 10 (20 ppt for PFPrA) and 80 ppt in duplicate
per batch with a total of three batches being prepared and analyzed on different
days. Unfortified and fortified water samples were processed through the sample
preparation procedure for chromatographic analysis and quantification.


INSTRUMENT CONDITIONS

LC-MS/MS analysis of ultrashort-chain PFAS concurrently with alternative and
legacy PFAS was performed using a Raptor C18 analytical column and a Shimadzu
Nexera X2 HPLC coupled to a SCIEX 4500 MS/MS. A PFAS delay column (cat.# 27854)
was installed between the pump mixer and the injector in order to prevent
coelution of any instrument-related PFAS with target analytes in the sample.
Instrument conditions were as follows and analyte transitions are provided in
Table I.

Analytical column: Raptor C18 2.7 µm, 100 mm x 3.0 mm (cat.# 9304A1E) Delay
column: PFAS delay column (cat.# 27854) Mobile phase A: 5 mM ammonium acetate in
water Mobile phase B: Methanol Gradient Time (min) %B   0.00 20   7.00 95   9.00
95   9.01 20   11.0 20 Flow rate: 0.25 mL/min Run time: 11 min Injection volume:
10 µL Column temp.: 40 °C Ion mode: Negative ESI Ion spray voltage: -2000 Source
temp.: 450 °C

 

Table I: Ion Transitions for LC-MS/MS Analysis of Ultrashort-Chain PFAS
Concurrently with Alternative and Legacy PFAS.

Peak ID

Compound

Precursor Ion

Product Ion

Internal Standard

1

PFPrA

162.9

119.0

13C2-PFHxA

2

PFBA

212.8

169.0

13C2-PFOA

3

PFPrS

248.8

79.6

13C2-PFHxA

4

PFBS

298.8

79.9

13C2-PFHxA

5

13C2-PFHxA

314.9

270.0

—

6

HFPO-DA

285.0

168.9

13C2-PFOA

7

ADONA

376.9

250.7

13C2-PFOA

8

PFOA

413.1

368.9

13C2-PFOA

9

13C2-PFOA

415.0

370.0

—

10

PFOS

498.8

80.0

13C4-PFOS

11

13C4-PFOS

503.0

80.0

—

12

9Cl-PF3ONS

530.8

350.7

13C4-PFOS

13

11Cl-PF3OUdS

630.7

451.0

13C4-PFOS

 


RESULTS AND DISCUSSION


CHROMATOGRAPHIC PERFORMANCE

Analyte peak shapes, retention, and intensity were similar across the reagent
water and field water samples. There was a higher baseline for the PFPrA signal
in all field water samples (Figure 1), but this did not have a negative impact
on peak integration and quantification of PFPrA. No matrix interference was
observed for all water samples prepared by two-fold dilution.

Figure 1: Good chromatographic peak shapes and adequate retention were obtained
for the simultaneous LC-MS/MS analysis of ultrashort-chain PFAS along with
alternative and legacy PFAS in various reagent and field water samples.

80 ppt Reagent Water Standard

LC_EV0555

PeakstR (min)Conc.
(ng/L)Precursor IonProduct Ion 1.Perfluoropropanoic acid (PFPrA)2.7480162.9119.0
2.Perfluorobutanoic acid (PFBA)4.6980212.8169.0 3.Perfluoropropanesulfonic acid
(PFPrS)5.1380248.879.6 4.Perfluorobutanesulfonic acid (PFBS)6.1480298.879.9
5.Perfluoro-n-[1,2-13C2]hexanoic acid (13C2-PFHxA)6.7550314.9270.0
6.Hexafluoropropylene oxide-dimer acid (HFPO-DA)6.9280285.0168.9

PeakstR (min)Conc.
(ng/L)Precursor IonProduct Ion 7.Ammonium 4,8-dioxa-3H-perfluorononanoate
(ADONA)7.3380376.9250.7 8.Perfluorooctanoic acid (PFOA)7.7080413.1368.9
9.Perfluoro-[1,2-13C2]octanoic acid (13C2-PFOA)7.7050415.0370.0
10.Perfluorooctanesulfonic acid (PFOS)8.0180498.880.0
11.Perfluoro-[1,2,3,4-13C4]octanesulfonic acid (13C4-PFOS)8.0150503.080.0
12.9-Chlorohexadecafluoro-3-oxanonane-1-sulfonate (9Cl-PF3ONS)8.1580530.8350.7
13.11-Chloroeicosafluoro-3-oxanonane-1-sulfonate (11Cl-PF3OUdS)8.6180630.7451.0

Download PDF

80 ppt Fortified Groundwater Sample

LC_EV0556


ColumnRaptor C18 (cat.# 9304A1E)Dimensions:100 mm x 3 mm IDParticle Size:2.7
µmPore Size:90 ÅTemp.:40 °CStandard/SampleConc.:80 pptInj. Vol.:10 µL Mobile
PhaseA:Water, 5 mM ammonium acetate B:Methanol

Time (min)Flow
(mL/min)%A%B0.000.2580207.000.255959.000.255959.010.25802011.00.258020

DetectorMS/MSIon Mode:ESI- Mode:MRM InstrumentUHPLCSample PreparationIn a
polypropylene vial, 250 µL of groundwater sample (fortified at 80 ppt) was mixed
with 250 µL of 40:60 reagent water:methanol and 5 µL of internal standard
solution (5 ng/mL of 13C2-PFHxA, 13C2-PFOA, 13C4-PFOS in methanol). The vial was
capped with a polyethylene cap prior to analysis. NotesA PFAS delay column
(cat.# 27854) was installed between the pump mixer and the injector.



Download PDF


LINEARITY

In this LC-MS/MS method for the simultaneous analysis of ultrashort-chain PFAS
along with alternative and legacy PFAS, the calibration range was 10-400 ppt for
PFPrA and 5-400 ppt for all other analytes. All compounds showed acceptable
linearity with r values ≥ 0.999 and deviations of <20%. 11Cl-PF3OUdS is the only
analyte that was quantified using a quadratic regression (1/x weighted) standard
curve. All other analytes were quantified using a 1/x weighted linear regression
(Figure 2).

Figure 2: Standard Curves.




ACCURACY AND PRECISION

The unfortified water samples showed various levels of C3, C4, and C8 PFAS with
no detectable PFPrS, ADONA, HFPO-DA, 9Cl-PF3ONS, and 11Cl-PF3OUdS (Table II).
For accuracy (%recovery) calculation, the measured amount of analyte in the
fortified sample was adjusted based on the unfortified concentration. Table III
shows the accuracy and precision results calculated across all three batches of
data. Method accuracy was demonstrated by recovery values that were within 20%
of the nominal concentration for both fortified sample levels, as well as for
the LLOQ concentration standard prepared in reagent water. The %RSD was <15%,
indicating acceptable method precision.

Table II: PFAS Concentrations in Unfortified Water Samples.

Detected Concentration (ng/L)  

PFPrA

PFBA

PFPrS

PFBS

HFPO-DA

ADONA

PFOA

PFOS

9Cl-PF3ONS

11Cl-PF3OUdS

Tap Water

ND

1.1

ND

ND

ND

ND

ND

ND

ND

ND

River Water

ND

1.6

ND

ND

ND

ND

ND

ND

ND

ND

Groundwater

9.0

3.4

ND

2.6

ND

ND

ND

ND

ND

ND

POTW Water

11.7

10.6

ND

3.0

ND

ND

15.0

6.0

ND

ND

Table III: Accuracy and Precision.

Conc. (ng/L)

Average %Recovery (%RSD)

Tap Water

River Water

Groundwater

POTW Water

Reagent Water

10*

80

10*

80

10*

80

10*

80

5**
(LLOQ)

PFPrA

96.9 (11.0)

105 (3.91)

105 (6.57)

95.4 (6.84)

92.0 (9.54)

99.4 (7.40)

94.2 (5.29)

87.2 (8.18)

103
(10.9)

PFBA

99.3 (9.19)

108 (1.81)

108 (5.20)

110 (1.70)

104 (8.21)

108 (6.68)

108 (8.12)

97.1 (8.17)

97.9
(12.0)

PFPrS

100 (4.24)

107 (3.14)

103 (6.71)

105 (2.64)

105 (8.48)

109 (6.68)

109 (5.65)

103 (9.28)

99.1
(8.59)

PFBS

101 (5.20)

106 (1.84)

99.7 (7.54)

105 (2.10)

100 (6.57)

106 (2.82)

103 (1.93)

97.8 (5.85)

96.0
(8.75)

HFPO-DA

96.2 (7.86)

102 (4.64)

96.2 (4.99)

105 (3.94)

95.0 (3.59)

101 (8.92)

92.9 (4.87)

90.3 (7.77)

99.3
(8.54)

ADONA

101 (6.23)

106 (3.82)

97.6 (6.36)

106 (2.32)

98.4 (2.68)

105 (4.08)

98.2 (7.09)

98.2 (7.09)

102
(10.3)

PFOA

105 (8.65)

105 (3.70)

108 (12.1)

107 (3.63)

108 (9.66)

105 (5.26)

99.9 (10.5)

94.5 (7.24)

100
(9.05)

PFOS

99.3 (2.10)

108 (4.24)

112 (1.87)

107 (4.93)

101 (2.96)

102 (2.31)

104 (4.46)

98.3 (5.82)

94.3 (8.85)

9Cl-PF3ONS

95.6 (4.60)

106 (5.93)

105 (5.37)

110 (8.20)

97.2 (4.52)

107 (7.41)

101 (6.52)

99.8 (4.89)

98.8
(5.47)

11Cl-PF3OUdS

114 (8.78)

112 (8.91)

102 (15.0)

91.5 (2.34)

96.7 (5.99)

105 (15.2)

115 (2.67)

103 (8.45)

105
(8.04)

*20 ng/L for PFPrA
**10 ng/L for PFPrA


CONCLUSION

A robust LC-MS/MS method for quantitating a diverse range of PFAS of various
chain lengths and structures utilizing a simplified direct injection approach
was successfully evaluated in different water sample matrices. Using a Raptor
C18 (2.7 µm) 100 x 3.0 mm column with a PFAS delay column, the analytical method
was demonstrated to be fast, rugged, and sensitive with acceptable accuracy and
precision. This method is suitable for labs needing to report an extended list
of PFAS compounds, including the analysis of ultrashort-chain PFAS, for potable
and non-potable water testing.


REFERENCES

 1. S. Taniyasu, K. Kannan, L.W.Y. Yeung, K.Y. Kwok, P.K.S Lam, N. Yamashita,
    Analysis of trifluoroacetic acid and other short-chain perfluorinated acids
    (C2-C4) in precipitation by liquid chromatography-tandem mass spectrometry:
    comparison to patterns of long-chain perfluorinated acids (C5-C18), Anal.
    Chim. Acta. 619 (2008) 221-230.
 2. J. Janda, K. Nodler, H-J. Brauch, C. Zwiener, F.T. Lange, Robust trace
    analysis of polar (C2-C8) perfluorinated carboxylic acids by liquid
    chromatography-tandem mass spectrometry: method development and application
    to surface water, groundwater, and drinking water, Environ. Sci. Pollut.R.
    26 (2018) 7326-7336.
 3. K.Y. Kwok, S. Taniyasu, L.W.Y. Yeung, M.B. Murphy, P.K.S. Lam, Y. Horii, K.
    Kannan, G. Petrick, R.K. Sinha, N. Yamashita, Flux of perfluorinated
    chemicals through wet deposition in Japan, the United States, and other
    countries, Environ. Sci. Technol. 44 (2010) 7043-7049.
 4. K.A. Barzen-Hanson, J.A. Field, Discovery and implications of C2 and C3
    perfluoroalkyl sulfonates in aqueous film-forming foams and groundwater,
    Environ. Sci. Technol. Lett. 5 (2015) 95-99.

EVAN3073-UNV


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