Online Solid-Phase Extraction LC-MS/MS: A Rapid and Valid Method for the Determination of Perfluorinated Compounds at Sub ng·L⁻¹ Level in Natural Water

Abstract

In this research paper, we report a method able to detect perfluorinated compound at pg·L−1 levels in superficial and underground water samples. An online solid phase extraction HPLC-MS/MS method was developed for the analysis of 12 perfluoroalkyl acids (PFASs). The method is based on injection of 5000 µL of water sample in SPE online WAX column followed by chromatography separation and mass spectrometry determination. SPE online elution was performed by water + 0.05% NH4OH and methanol + 0.05% NH4OH, while separation of target compounds was achieved within 10 min by Gemini chromatographic column operating from 1 to 12 pH range and using a mixture of water-methanol + 0.05% NH4OH. Sub ng·L−1 method detection limits (from 0.2 to 5 ng·L−1), linearity (from 0.2 to 250 ng·L−1), accuracy (from 80 to 120%), and precision (RSD less than 15% at LOQs levels) were achieved. The method is capable of measuring PFAS at trace levels, but above all it can reach the limit of 200 pg·L−1 required by European regulation for PFOS determination in surface and underground waters. The method was validated for quantitative analysis of PFASs in real water samples.

Distribution and Bioaccumulation of Perfluoroalkyl Acids in Xiamen Coastal Waters

“…e PFAs in sediments and organisms were extracted by the ion-pairing agent extracted method with some modifications [22][23][24]. A total of 2 mL of Na 2 CO 3 (0.25 M), 1 mL of the ion-pairing agent tetrabutylammonium hydrogensulfate (0.5 M, adjusted to pH 10), 2 mL of MTBE, and 100 μL (10 ng) of MPFOA (as an internal standard) were added into the centrifuge tubes containing the samples in turn.…”

Hyphenated High Performance Liquid Chromatography–Tandem Mass Spectrometry Techniques for the Determination of Perfluorinated Alkylated Substances in Lombardia Region in Italy, Profile Levels and Assessment: One Year of Monitoring Activities During 2018

“…Elution conditions and Mass Spectrometry optimal parameters were reported in a previous paper concerning method validation [14].…”

“…Ten mL of samples were transferred to a 10 mL vial, then 0.1 mL Internal Standard (IS) solutions at 5000 ng L −1 were added in order to obtain a final IS concentration of 50 ng L −1 ; they were manually mixed and stored in a refrigerated autosampler system at 4 • C. 5 mL of sample was injected by using a SPE online system as discussed in previous paper [14]. The samples were injected directly without filtration step.…”

“…In recent years, Environmental Protection Agency of Lombardia Region (ARPA Lombardia) form Italy has invested economical sources in monitoring activities, and recently, laboratories have developed an environmentally green analytical chemistry methods, by hyphenated techniques. In detail, the method consists of a concentration by online solid phase extraction coupled with ultra-high-performance liquid chromatography-tandem mass spectrometry, in order to quantify PFASs at very low limit of quantifications [14].…”

UPLC-MS/MS Identification and Quantification of Withanolides from Six Parts of the Medicinal Plant Datura Metel L.

“…Its high sensitivity and fast scanning speed make it a preferred analytical method. To eliminate the effects of the matrix effect in quantitative analysis, the multiple reaction monitoring (MRM) mode in triple quadrupole mass spectrometry (UPLC-QQQ-MS/MS) is frequently employed [14,15]. This method does not require complete separation of the chromatographic peaks of multiple components, as long as the target analysis is non-interfering with each other.…”