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LC-MS/MS and GC-MS Measurements of Extractables and Leachables (E&L) from Polymeric Materials

Published by National Institute of Standards and Technology | National Institute of Standards and Technology | Catalog Last Checked: September 02, 2026 at 07:19 PM | Dataset Last Updated: March 19, 2026
This mass spectrometry (MS) data set encompasses spectra of the extractables and leachables (E&L) of 100 polymer materials sourced from the Scientific Polymer Products Inc Polymer Samples Kit (see: SciPoly_PolymerSampleKit205_Items.xlsx). Extractions of these polymers were carried out using three HPLC-grade solvents of varying polarity (water, isopropanol, and hexane) with 10 mg polymer/mL solvent for 24 hours at 50 °C with shaking. To account for solvent volatility, extractions were carried out in 8 mL pressure tubes from Ace Glass Incorporated (Product #8648-25) (rated at 150 psig). Extraction solutions were subsequently analyzed using three ionization techniques: Electron Ionization (EI) with GC-MS and Electrospray Ionization (ESI) and Atmospheric Pressure Chemical Ionization (APCI) via LC-MS/MS on an Agilent QTOF 6530 and a Bruker timsTOF Pro 2, respectively. Several precautionary measures had to be taken following the extraction procedure. Extracts were centrifuged and filtered using 0.45-micron syringe filters to prevent prohibitively large particles from interfering with chromatography and MS analysis. Moreover, a guard column was used before the LC column to avoid contamination. As such, pressure build-up would often be a concern, so the LC and guard column had to be thoroughly flushed after each analysis batch. Thousands of spectra were processed using in-house software, generating lists of identifications using the most recent versions of the NIST MS libraries via both direct and hybrid search methods. Some monomers were detected under the given extraction conditions, and many plastic additives (e.g., plasticizers, antioxidants, and processing agents) could be identified; some common examples found in many of the polymer standards include oleamide and palmitamide. High-quality unidentified spectra obtained from the extracts are included in a library of annotated recurrent unidentified spectra (ARUS). LC Chromatographic Separation Method: LC runs were performed using reversed-phase chromatography with an ACQUITY UPLC CSH C18 column (130 Å (13.0 nm), 1.7 µm, 2.1 mm x 100 mm), mobile phase A: water, and mobile phase B: acetonitrile (both mobile phases containing 0.1 % formic acid). The chromatographic separation method was as follows: injection volume: 10 µL, column temperature: 35°C, flow rate: 0.400 mL/min, and gradient: initial condition of 1.00% B, hold for 1.00 min, linear ramp to 80.00% B in 8.00 min, linear ramp to 99.00% B in 3.00 min, hold for 1.50 min, linear ramp to 1.00% B in 0.50 min, hold for 1.00 min. GC Chromatographic Separation Method: Spectra were obtained using an Agilent 5977B instrument, with GC runs performed using a Restek Rxi-5Sil MS GC Capillary Column (15 m x 250 µm x 0.25 µm) under 2 mL/min He flow. The initial oven temperature was 40°C (held for 3 min), with a ramp rate of 20°C/min, final temperature of 320°C, and final hold time of 3.75 min. References: Berthelette, K.; Walter, T. H. Column screening for the UPLC separation of plastic additives as part of extractables and leachables workflows; 720006777EN; Waters Corporation, MA, USA, 2020. Lee, P. J.; Di Gioia, A. J. Rapid analysis of 25 common polymer additives; 720002488EN; Waters Corporation, Milford, MA, USA, 2008. Simón-Manso, Y.; Erisman, E. P.; Mak, T. D.; Burke, M. C.; Zuber, A.; Yang, X.; Liang, Y.; Neta, P.; Bukhari, T.; Williams, A. J.; et al. NIST Mass Spectral Libraries in the Context of the Circular Economy of Plastics. J Am Soc Mass Spectrom 2025, 36 (2), 439–445. DOI: 10.1021/jasms.4c00349.

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Complete Metadata
@type dcat:Dataset
accessLevel public
accrualPeriodicity irregular
bureauCode 
[
  "006:55"
]
contactPoint 
{
  "fn": "Yamil Simon",
  "hasEmail": "mailto:yamil.simon@nist.gov"
}
description This mass spectrometry (MS) data set encompasses spectra of the extractables and leachables (E&L) of 100 polymer materials sourced from the Scientific Polymer Products Inc Polymer Samples Kit (see: SciPoly_PolymerSampleKit205_Items.xlsx). Extractions of these polymers were carried out using three HPLC-grade solvents of varying polarity (water, isopropanol, and hexane) with 10 mg polymer/mL solvent for 24 hours at 50 °C with shaking. To account for solvent volatility, extractions were carried out in 8 mL pressure tubes from Ace Glass Incorporated (Product #8648-25) (rated at 150 psig). Extraction solutions were subsequently analyzed using three ionization techniques: Electron Ionization (EI) with GC-MS and Electrospray Ionization (ESI) and Atmospheric Pressure Chemical Ionization (APCI) via LC-MS/MS on an Agilent QTOF 6530 and a Bruker timsTOF Pro 2, respectively. Several precautionary measures had to be taken following the extraction procedure. Extracts were centrifuged and filtered using 0.45-micron syringe filters to prevent prohibitively large particles from interfering with chromatography and MS analysis. Moreover, a guard column was used before the LC column to avoid contamination. As such, pressure build-up would often be a concern, so the LC and guard column had to be thoroughly flushed after each analysis batch. Thousands of spectra were processed using in-house software, generating lists of identifications using the most recent versions of the NIST MS libraries via both direct and hybrid search methods. Some monomers were detected under the given extraction conditions, and many plastic additives (e.g., plasticizers, antioxidants, and processing agents) could be identified; some common examples found in many of the polymer standards include oleamide and palmitamide. High-quality unidentified spectra obtained from the extracts are included in a library of annotated recurrent unidentified spectra (ARUS). LC Chromatographic Separation Method: LC runs were performed using reversed-phase chromatography with an ACQUITY UPLC CSH C18 column (130 Å (13.0 nm), 1.7 µm, 2.1 mm x 100 mm), mobile phase A: water, and mobile phase B: acetonitrile (both mobile phases containing 0.1 % formic acid). The chromatographic separation method was as follows: injection volume: 10 µL, column temperature: 35°C, flow rate: 0.400 mL/min, and gradient: initial condition of 1.00% B, hold for 1.00 min, linear ramp to 80.00% B in 8.00 min, linear ramp to 99.00% B in 3.00 min, hold for 1.50 min, linear ramp to 1.00% B in 0.50 min, hold for 1.00 min. GC Chromatographic Separation Method: Spectra were obtained using an Agilent 5977B instrument, with GC runs performed using a Restek Rxi-5Sil MS GC Capillary Column (15 m x 250 µm x 0.25 µm) under 2 mL/min He flow. The initial oven temperature was 40°C (held for 3 min), with a ramp rate of 20°C/min, final temperature of 320°C, and final hold time of 3.75 min. References: Berthelette, K.; Walter, T. H. Column screening for the UPLC separation of plastic additives as part of extractables and leachables workflows; 720006777EN; Waters Corporation, MA, USA, 2020. Lee, P. J.; Di Gioia, A. J. Rapid analysis of 25 common polymer additives; 720002488EN; Waters Corporation, Milford, MA, USA, 2008. Simón-Manso, Y.; Erisman, E. P.; Mak, T. D.; Burke, M. C.; Zuber, A.; Yang, X.; Liang, Y.; Neta, P.; Bukhari, T.; Williams, A. J.; et al. NIST Mass Spectral Libraries in the Context of the Circular Economy of Plastics. J Am Soc Mass Spectrom 2025, 36 (2), 439–445. DOI: 10.1021/jasms.4c00349.
distribution 
[
  {
    "title": "README",
    "format": ".txt",
    "mediaType": "text/plain",
    "description": "The file contains a description of the dataset directory.",
    "downloadURL": "https://data.nist.gov/od/ds/mds2-4147/4147_README.txt"
  },
  {
    "title": "GC_MS_single_quad",
    "mediaType": "application/zip",
    "downloadURL": "https://data.nist.gov/od/ds/mds2-4147/GC_MS_single_quad.zip"
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  {
    "title": "QTOF_ESI",
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    "downloadURL": "https://data.nist.gov/od/ds/mds2-4147/QTOF_ESI.zip"
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    "title": "timsTOF_APCI",
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    "downloadURL": "https://data.nist.gov/od/ds/mds2-4147/timsTOF_APCI.zip"
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identifier ark:/88434/mds2-4147
issued 2026-05-13
keyword 
[
  "APCI-LC-MS/MS",
  "ESI-LC-MS/MS",
  "GC-MS",
  "extractables and leachables",
  "ion mobility",
  "mass spectrometry",
  "plastic-related compounds",
  "plastics",
  "polymers",
  "tandem mass spectrometry"
]
landingPage https://data.nist.gov/od/id/mds2-4147
language 
[
  "en"
]
license https://www.nist.gov/open/license
modified 2026-03-19 00:00:00
programCode 
[
  "006:045"
]
publisher 
{
  "name": "National Institute of Standards and Technology",
  "@type": "org:Organization"
}
theme 
[
  "Chemistry",
  "Chemistry:Analytical chemistry",
  "Environment"
]
title LC-MS/MS and GC-MS Measurements of Extractables and Leachables (E&L) from Polymeric Materials

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