Development of a U.S. EPA Drinking Water Method for the Analysis of Selected Perfluoroalkyl Acids by Solid-Phase Extraction and LC-MS-MS

Abstract

A drinking water method for perfluoroalkyl acids (PFAAs) is presented that addresses the occurrence monitoring needs of the U.S. Environmental Protection Agency (EPA) for a future unregulated contaminant monitoring regulation (UCMR). This paper describes the challenges associated with developing an analytical method for 14 PFAAs that will be used for drinking water occurrence monitoring. The method employs solid-phase extraction with analysis by liquid chromatography-tandem mass spectrometry (LC-MS-MS). The final method preservation scheme requires that samples be stored in polypropylene bottles and that they be buffered and free chlorine removed with Trizma buffer. Mean recoveries of chlorinated surface water samples fortified with the PFAAs at 40-100 ng/L (except for the perfluorooctane-sulfonamido-acetic acids at 200 ng/L) are 85-112% with < 5% relative standard deviation. Single laboratory minimum reporting limits of 2.9-14 ng/L are demonstrated with this methodology. The final method meets all of the EPA UCMR survey requirements for sample collection and storage, precision, accuracy, and sensitivity and is expected to be proposed for use under a future UCMR.

Ecological risk assessment of perfluooroctane sulfonate to aquatic fauna from a bayou adjacent to former fire training areas at a US Air Force installation

“…Clearly, there are significant challenges to determining PFAS residues in environmental samples (Reiner et al ). Like many others, we used the lone standard USEPA method (537; Shoemaker et al ) available as the basis for analysis of surface water and sediment extracts, despite the method being limited to finished drinking water. For tissue samples, additional methods were developed, primarily quick, easy, cheap, effective, rugged, and safe–(QuEChERS) based tissue extractions (Lanza et al ; Karnjanapiboonwong et al ) prior to liquid chromatography–mass spectrometry analysis.…”

Occurrence investigation of perfluorinated compounds in surface water from East Lake (Wuhan, China) upon rapid and selective magnetic solid-phase extraction

“…In each site, three parallel water samples were collected at a depth of 10 cm under the water surface and loaded in a 1 L of PP bottle, respectively. The PP bottle was rinsed meticulously according to the method recommended by US EPA39. To eliminate the contamination derived from the used materials, all of the accessible polytetrafluoroethene (PTFE) and fluoropolymer were avoid seriously during the sample collection and preparation.…”

Recent Developments of PFAS-Detecting Sensors and Future Direction: A Review

“…PFASs from various aqueous matrices are typically extracted using solid-phase extraction (SPE) [ 21 , 22 , 51 , 52 ], but other methods, including liquid–liquid extraction (LLE) [ 23 ], ion-pair extraction (IPE) [ 24 ], solid-phase microextraction (SPME) [ 25 ], and dispersive liquid–liquid microextraction (DLLME) [ 26 ], have also been used in many studies. The most common protocol for off-line SPE (typically polystyrene divinylbenzene contained cartridges) involves extract elution using methanol followed by concentration to dryness with nitrogen before injecting the sample into the column and analyzing it using LC-MS/MS [ 53 , 54 ].…”

“…The occurrence of the large quantity of currently detected and future perfluorinated compounds makes it a very challenging task to monitor them in environmental matrices, requiring the time- and/or resource-consuming analytical methods to keep pace with the “never-ending” chemicals [ 62 ]. For instance, the USEPA first developed an SPE-LC-MS/MS method (Method 537, Rev 1) for the determination of 14 PFAAs in drinking water [ 51 ]. This was followed by an updated method (Method 537.1) in 2018 to include four more PFAAs [ 63 ].…”