Page 52 - Application Notebook - PFAS Analysis

No. SSI-HPLC-037

High Performance Liquid Chromatography
Extraction and LC-MS/MS

Analysis of PFAS Compounds in Fish
Tissue Using Offline Supercritical Fluid

No. HPLC-037

■ Introduction
Per and Poly-fluoroalkyl substances (PFAS) are Optimized extraction conditions to maximize PFAS
synthetic compounds that are found in a wide range recoveries are shown in Table 1. After extraction, the
of industrial and consumer products. Due to the sample was dried down under nitrogen and
strong nature of the carbon-fluorine bond, these reconstituted with 1 mL of methanol. The sample
compounds are resistant to degradation and have was centrifuged and the supernatant was transferred
been found to accumulate in fish, wildlife and to an LC vial. 1 uL of the supernatant was injected
multiple environmental samples (ex. water, soil…), for LC-MS/MS analysis. Table 2 shows the LC-MS/MS
posing a significant health risk to humans. Current conditions used for the Shimadzu LCMS-8050 for
sample preparation techniques for PFAS analysis are this study; a representative chromatogram is
laborious and not easily automated. In this study, included in Figure 2.
supercritical fluid extraction (SFE) was evaluated as
an alternative sample preparation technique for the Table 1: SFE optimized method conditions

extraction of eighteen PFAS compounds from fish Item Value
tissue, as a preconcentration step prior to their Mobile phase CO2/MeOH
analysis by LC-MS/MS. Modifier concentration 20% MeOH
Flow rate 5 mL/min
■ Experimental Approach Vessel temperature 60 ℃
For this study, the Shimadzu Nexera UC offline SFE Extraction cycles 3
system (configuration shown in Figure 1) was Back pressure 20 MPa
45 minutes
Extraction time
employed. 0.5 grams of freeze-dried fish tissue was
milled and mixed with 1 packet (1 gram) of Miyazaki
Hydro-Protect and placed into a 5 mL extraction
vessel for extraction.

CO2 SFE BPR Gas liquid
separator

Fraction
Collector
Modifier
pump

Figure 1: System Configuration of offline SFE system for direct collection method.
CO2: CO2 pump; SFE: Supercritical Fluid Extraction Module; BPR: Back pressure regulator