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HomeWastewater & Process Water​ TestingAnalysis of PFAS in Water according to EPA 1633

Analysis of PFAS in Water according to EPA 1633

Lara Rosenberger, Senior Scientist, Yannick Hövelmann, Senior Scientist, Olga Shimelis, Mgr Research & Development Sr., Katherine Stenerson, Lead Expert, Meghna Negi, Specialist

Abstract

Per- and polyfluoroalkyl substances (PFAS), known for their environmental persistence and potential health impacts, are a significant concern in water quality management. This study demonstrates the utilization of the EPA Method 1633 to analyze and quantify 40 PFAS chemicals in water samples. The technique utilizes liquid chromatography combined with tandem mass spectrometry (LC-MS/MS) after a solid-phase extraction (SPE) using Supelclean™ ENVI-WAX™ SPE cartridges. The procedure allows for highly sensitive detection and quantitation of PFAS analytes in various matrices. Performance evaluation demonstrated that recoveries for all 40 PFAS compounds and 24 isotopically labeled standards (EIS) were within the typical EPA acceptable range of 70-130% with low corresponding standard deviations, indicating high precision and robustness. The method's suitability for comprehensive PFAS analysis in environmental samples underscores its value for regulatory compliance and environmental monitoring.

Section Overview:

INTRODUCTION

Per- and polyfluoroalkyl substances (PFAS), also referred to as “forever chemicals,” are a broad category of more than 4700 synthetic fluorinated aliphatic compounds that have been applied in consumer goods since the 1950s. Known for their resistance to lipids and water, PFAS are highly stable due to the strong carbon-fluorine bond. They are commonly used as surface-active agents in products like stain repellents and firefighting foams, persist in the environment due to their slow degradation rate, however.

With their widespread use in various consumer and commercial applications, PFAS have drawn significant attention regarding the contamination of water, soil, and even the bloodstreams of humans and animals. This emphasizes their persistence and impact on environmental and human health. The United States Environmental Protection Agency (US EPA) and the European Union (EU) played key roles in developing stringent regulatory guidelines for PFAS testing, which are essential for protecting ecosystems and human populations.1,2,3

The US EPA adopted a comprehensive strategy, as demonstrated by the development of established analytical methods such as EPA Methods 533 and 537.1 for drinking water, to thoroughly evaluate PFAS levels in various environmental samples. At the same time, the EU has implemented strict regulations under the Registration, Evaluation, Authorization, and Restriction of Chemicals (REACH) framework.4 These regulations use advanced analytical tools such as liquid chromatography-tandem mass spectrometry (LC-MS/MS) to monitor PFAS in different chemicals substances, showing a dedication to improving analytical capabilities and safeguarding the environment and human health.

The EPA Method 16331 is a laboratory-validated approach that employs LC-MS/MS to analyze aqueous, solid, biosolid, and tissue samples for 40 PFAS across nine compound classes. This "performance-based" method allows for condition adjustments to improve performance if all requirements are met, providing a stable platform for precise calibration and quantification of PFAS analytes using isotopically labeled standards. With the inclusion of analytes from EPA drinking water Methods 533 and 537.1, EPA Method 1633 tackles emerging PFAS classes, filling important voids in testing consistency, scope, sensitivity, and applicability across different sample types, helping to address the complex challenges posed by PFAS contaminations and ensuring public health and environmental protection.

The objective of this application note is to demonstrate the determination of 40 PFAS analytes from PFAS-spiked water samples by solid-phase extraction (SPE) using Supelclean™ ENVI-WAX™ SPE cartridges on a PTFE-free Visiprep™ SPE vacuum manifold followed by LC/MS-MS analysis employing Fused-Core® Ascentis® Express PFAS columns (analytical and delay) and compare the obtained method performance characteristics to the criteria stated in EPA 1633.

EXPERIMENTAL

Solutions and Standards Preparation

The sample collection and preparation followed the EPA Method 1633 procedure.

Native (40) and isotopically (31) labeled PFAS standards were used as methanolic 50 µg/mL stock solutions. The labeled compounds are either used as extracted internal standards (EIS, 24 compounds) or non-extracted internal standards (NIS, 7 compounds). Following the recommendations of the EPA1633 method, these stock solutions were used to prepare seven calibration solutions containing the native PFAS compounds in various concentrations (CS1 - CS7; compound specific concentrations ranging from 0.2 - 5 ng/mL for CS1 to 62.5 - 1560 ng/mL for CS7 as indicated in Table 4 of the EPA1633 method) to cover the working range of the MS instrument.

Sample Preparation

PFAS Analysis Method Performance Assessment

In accordance with the EPA 1633 method, the method performance was investigated for water samples. 500 mL of water (tap fresh water from a Milli-Q® system) was collected in HDPE bottles with liner-less polypropylene caps. The water sample was fortified at three different levels (2x CS1, 12.5x CS1, 40x CS1) with 40 native PFAS and spiked with 24 isotopically (13C or D) labeled standards (extracted internal standards – EIS) according to EPA 1633 (Table 3). For the extraction by SPE, Supelclean™ ENVI-WAX™ SPE tubes (500 mg/6 mL, 54057-U) were equipped with large volume SPE reservoirs (25 mL, 54258-U) and placed on a PTFE-free Visiprep™ vacuum manifold (57030-U). The tubes were conditioned with 15 mL of 1.0% NH4OH in MeOH and equilibrated with 5 mL of aqueous 0.3 M formic acid. After the water sample (500 mL) was loaded and passed through the cartridge, 2x 5 mL of water and 5 mL of 0.1M formic acid/methanol (1:1 (v/v)) were added as a washing step. The cartridge was subsequently dried for 1 min before 5 mL 1.0% NH4OH in MeOH was used to elute the analytes. For further clean-up 25 µL concentrated acetic acid and approximately 10 mg loose/bulk Supelclean™ ENVI-Carb™ (57210-U) were added to the eluate and mixed for less than 5 minutes using a vortex shaker, followed by centrifugation for 10 minutes at 4000 g. Subsequently, the supernatants were filtered using Millex® Nylon 0.2 µm syringe filters (SLGNX13) into collection tubes containing additional 7 isotopically labeled (13C or 18O) labeled standards (non-extracted internal standards – NIS) prior to LC-MS/MS analysis. The sample preparation represents an enrichment of 1:100 from the original water sample to the final extract.

Instrumental Analysis

LC-MS/MS analysis was performed using an Agilent 1290 Infinity II instrument coupled to an Agilent 6495C triple quadrupole mass spectrometer (Table 1). Chromatographic separation was achieved using an Ascentis® Express PFAS 90 Å (5 cm x 2.1 mm, 2.7 µm, 53557-U) analytical column. In addition, an Ascentis® Express PFAS Delay column 90 Å (5 cm x 3.0 mm, 2.7 µm, 53572-U) was installed after the mixing valve and before the autosampler to offset PFAS contamination potentially originating from the LC system (e.g. pump, tubing, fittings, filters). Polypropylene snap cap vials were used instead of standard glass vials to avoid possible PFAS adsorption to the glass surface.

For the quantification of the native PFAS based on stable-isotope dilution, the MRM transitions shown in Table 2 were used. The EIS compounds were allocated in accordance with what is stated in EPA1633.

LC Conditions

 

Instrument:

Agilent 1290 Infinity II LC system and Agilent 6495C triple quadrupole mass spectrometer

Columns:

Ascentis® Express PFAS 90 Å; 2.7 µm, 5 cm x 2.1 mm (53557-U)

Delay Column: Ascentis® Express PFAS Delay 90 Å, 2.7 µm, 5 cm x 3.0 mm (53572-U)

Mobile phase:

[A] 2 mM Ammonium acetate in 95:5 water/acetonitrile (v/v);

[B] Acetonitrile

Gradient:

Time (min)

A%

B%

Flow rate [mL/min]

 

0.0

98.0

2.0

0.35

 

0.2

98.0

2.0

0.35

 

4.0

70.0

30.0

0.40

 

7.0

45.0

55.0

0.40

 

9.0

25.0

75.0

0.40

 

10.0

5.0

95.0

0.40

 

10.4

98.0

2.0

0.40

 

11.8

98.0

2.0

0.40

 

12.0

98.0

2.0

0.35

Flow rate:

See gradient table

Pressure:

195 bar

Column temp.:

40 °C

Detector:

MS (ESI-), MRM (see Table 2 for details)

Injection:

2 µL

Sample(s):

See text

Table 1.LC Conditions used for analysis of 40 PFAS compounds

Peak

Acronym

Compound

MRM Transition

(Quantifier)

Collision energy (eV)

RT (min)

R2

1

PFBA

Perfluorobutanoic acid

213.0→169.0

8

1.6

0.9998

2

PFMPA

Perfluoro-3-methoxypropanoic acid

229.0→85.0

12

2.4

0.9997

3

3:3FTCA

3-Perfluoropropyl propanoic acid

241.0→177.0

3

2.8

0.9992

4

PFPeA

Perfluoropentanoic acid

263.0→219.0

4

3.3

0.9999

5

PFMBA

Perfluoro-4-methoxybutanoic acid

279.0→85.0

8

3.6

0.9999

6

4:2FTS

1H,1H, 2H, 2H-Perfluorohexane sulfonic acid

327.0→307.0

20

4.0

0.9962

7

NFDHA

Nonafluoro-3,6-dioxaheptanoic acid

295.0→201.0

4

4.1

0.9990

8

PFBS

Perfluorobutanesulfonic acid

299.0→80.0

48

4.2

0.9982

9

PFHxA

Perfluorohexanoic acid

313.0→269.0

4

4.2

0.9989

10

HFPO-DA

Hexafluoropropylene oxide dimer acid

285.0→169.0

4

4.5

0.9998

11

PFEESA

Perfluoro(2-ethoxyethane)sulfonic acid

315.0→135.0

28

4.6

0.9978

12

5:3FTCA

2H,2H,3H,3H-Perfluorooctanoic acid

341.0→237.0

11

4.7

0.9990

13

PFHpA

Perfluoroheptanoic acid

363.0→319.0

8

5.0

0.9996

14

PFPeS

Perfluoropentanesulfonic acid

349.0→80.0

44

5.0

0.9988

15

ADONA

4,8-Dioxa-3H-perfluorononanoic acid

377.0→251.0

8

5.2

0.9998

16

6:2FTS

1H,1H, 2H, 2H-Perfluorooctane sulfonic acid

427.0→407.0

24

5.3

0.9926

17

PFOA

Perfluorootanoic acid

413.0→369.0

8

5.5

0.9999

18

PFHxS

Perfluoropentanesulfonic acid

399.0→80.0

52

5.6

0.9991

19

7:3FTCA

3-Perfluoroheptyl propanoic acid

441.0→337.0

11

6.0

0.9990

20

PFNA

Perfluoronanoic acid

463.0→419.0

8

6.0

0.9999

21

PFHpS

Perfluoroheptanesulfonic acid

449.0→80.0

68

6.2

0.9981

22

8:2FTS

1H,1H, 2H, 2H-Perfluorodecane sulfonic acid

527.0→507.0

28

6.3

0.9982

23

PFDA

Perfluorodecanoic acid

513.0→469.0

8

6.5

0.9998

24

NMeFOSAA

N-methyl perfluorooctanesulfonamidoacetic acid

570.0→419.0

19

6.6

0.9998

25

PFOS

Perfluorooctanesulfonic acid

499.0→80.0

72

6.6

0.9976

26

NEtFOSAA

N-ethyl perfluorooctanesulfonamidoacetic acid

584.0→419.0

19

6.7

0.9995

27

PFUnA

Perfluoroundecanoic acid

563.0→519.0

8

6.9

0.9992

28

9Cl-PF3ONS

9-Chlorohexadecafluoro-3-oxanonane-1-sulfonic acid

531.0→351.0

 

28

7.0

0.9975

29

PFNS

Perfluorononanesulfonic acid

549.0→80.0

79

7.1

0.9980

30

PFDoA

Perfluorododecanoic acid

613.0→569.0

8

7.3

0.9985

31

PFDS

Perfluorodecanesulfonic acid

599.0→80.0

79

7.5

0.9985

32

PFTrDA

Perfluorotridecanoic acid

663.0→619.0

11

7.7

0.9986

33

11Cl-PF3OUdS

 

11-Chloroeicosafluoro-3-oxaundecane-1-sulfonic acid

630.9→451.0

 

32

7.8

0.9994

34

PFOSA

Perfluorooctanesulfonamide

498.0→78.0

35

8.1

0.9999

35

PFTeDA

Perfluorotetradecanoic acid

713.0→669.0

11

8.1

0.9996

36

PFDoS

Perfluorododecanesulfonic acid

699.0→80.0

80

8.3

0.9973

37

NMeFOSE

N-methyl perfluorooctanesulfonamidoethanol

616.0→59.0

11

9.2

0.9999

38

NMeFOSA

N-methyl perfluorooctanesulfonamide

512.0→169.0

27

9.4

0.9996

39

NEtFOSE

N-ethyl perfluorooctanesulfonamidoethanol

630.0→59.0

15

9.6

0.9998

40

NEtFOSA

N-ethyl perfluorooctanesulfonamide

526.0→169.0

27

9.7

0.9988

Table 2.MRM (ESI-) chromatographic and linearity (R2, 1/x weighting, 6 calibrants for FTS compounds and 7 for all other) data for the 40 native PFAS analytes

RESULTS AND DISCUSSION

A chromatogram of the calibration solution 5 (CS5) containing the 40 native compounds is shown in Figure 1; as evident from Table 3, linear calibration curves with R2 ≥ 0.99 were obtained for all PFAS analytes.

A chromatogram displaying the separation of 40 per- and polyfluoroalkyl substances (PFAS) over a retention time range of approximately 0 to 12 minutes. The x-axis represents retention time in minutes, while the y-axis represents response intensity in counts per second (cps). Each peak corresponds to a different PFAS compound, numbered from 1 to 40. The peaks are color-coded, including orange, purple, green, pink, blue, and black, signifying different compounds or groups. A significant black peak at retention time 5.5 minutes (labeled as 15) exhibits the highest intensity among all detected compounds. Smaller peaks of varying intensities appear throughout the chromatogram, with some closely clustered between 3 and 7 minutes and others appearing later, around 8 to 10 minutes. The background gridlines enhance readability, allowing precise visualization of peak retention times and intensities. The overall distribution suggests a successful chromatographic separation of the PFAS mixture in the given solvent system.

Figure 1.40 PFAS compounds at CS5 concentration in methanol with 4% water, 1% ammonium hydroxide and 0.6% acetic acid (Peak IDs see Table 2).

The targeted native PFAS analytes were quantified based on stable-isotope dilution using extracted internal standards (EIS) which were added to the sample before the SPE extraction. The recovery of the EIS surrogates was determined using the non-extracted internal standards (NIS) which were spiked to the concentrated extract after the clean-up step; IS allocation was in accordance with the EPA 1633 method. Tables 3 and 4 display the recoveries and RSDs from the experimental study where 40 native PFAS compounds (Table 2) were spiked to the water samples at three different concentration levels and 24 EIS surrogates (Table 4) were added prior to extraction. All recoveries were between 84.0% and 110.7% and RSDs ranged from 0.2% to 18.1%. All were well within the acceptance limits for recovery from aqueous matrices as listed in Tables 5 and 6 of EPA Method 1633. 

Native PFAS compounds

Recovery in %

 

 

2x CS1

12.5x CS1

40x CS1

 

Perfluoroalkyl carboxylic acids

 

Spike levels*

0.4 ng/mL,

except PFBA 1.6 ng/mL & PFPeA 0.8 ng/mL

2.5 ng/mL,

except PFBA 10 ng/mL & PFPeA 5 ng/mL

8 ng/mL,

except PFBA 32 ng/mL & PFPeA 16 ng/mL

 

PFBA

101.6 ± 6.0

99.6 ± 2.2

98.6 ± 1.3

 

PFPeA

100.1 ± 4.6

100.8 ± 1.7

98.3 ± 0.5

 

PFHxA

105.1 ± 6.5

97.9 ± 3.7

97.7 ± 2.5

 

PFHpA

101.1 ± 5.3

99.2 ± 2.6

99.9 ± 2.5

 

PFOA

97.6 ± 3.0

96.7 ± 1.1

96.1 ± 1.8

 

PFNA   

98.8 ± 12.9

99.1 ± 6.9

96.1 ± 2.3

 

PFDA

92.5 ± 13.5

94.9 ± 2.4

95.5 ± 1.7

 

PFUnA

90.5 ± 3.3

100.8 ± 4.2

97.0 ± 5.2

 

PFDoA

107.1 ± 12.6

99.0 ± 6.1

100.6 ± 2.2

 

PFTrDA

93.6 ± 7.7

107.9 ± 1.6

104.1 ± 0.9

 

PFTeDA

94.8 ± 6.2

103.5 ± 2.2

101.9 ± 1.6

 

Perfluoroalkyl sulfonic acids

 

Spike levels*

0.4 ng/mL

2.5 ng/mL

8 ng/mL

 

PFBS

109.8 ± 3.7

94.9 ± 5.9

91.5 ± 0.8

 

PFPeS

103.1 ± 5.7

103.0 ± 4.5

98.7 ± 2.8

 

PFHxS

97.0 ± 8.0

94.0 ± 3.3

99.9 ± 1.9

 

PFHpS

90.7 ± 12.8

88.8 ± 3.7

91.6 ± 5.8

 

PFOS

101.3 ± 10.6

94.2 ± 6.2

93.8 ± 5.0

 

PFNS

107.1 ± 11.0

97.2 ± 4.7

94.7 ± 4.6

 

PFDS

110.7 ± 7.5

100.4 ± 5.2

93.8 ± 6.3

 

PFDoS

88.6 ± 8.8

87.1 ± 4.0

84.0 ± 5.6

 

Fluorotelomer sulfonic acids

 

Spike levels*

1.6 ng/mL

10 ng/mL

32 ng/mL

 

4:2FTS

97.9 ± 2.9

108.1 ± 1.3

109.6 ± 4.9

 

6:2FTS

101.7 ± 5.9

114.9 ± 5.2

109.2 ± 1.3

 

8:2FTS

103.8 ± 4.3

113.7 ± 3.7

99.8 ± 2.0

 

Perfluorooctane sulfonamides

 

Spike levels*

0.4 ng/mL

2.5 ng/mL

8 ng/mL

 

PFOSA

95.1 ± 10.8

94.1 ± 2.9

98.3 ± 1.8

 

NMeFOSA        

91.1 ± 28.5

93.7 ± 6.3

100.6 ± 0.2

 

NEtFOSA

88.7 ± 18.1

98.5 ± 2.5

98.3 ± 2.0

 

Perfluorooctane sulfonamidoacetic acids

 

Spike levels*

0.4 ng/mL

2.5 ng/mL

8 ng/mL

 

NMeFOSAA

84.1 ± 9.9

96.7 ± 5.3

100.5 ± 1.3

 

NEtFOSAA

97.7 ± 6.7

102.3 ± 0.4

95.3 ± 3.5

 

Perfluorooctane sulfonamide ethanols

 

Spike levels*

4 ng/mL

25 ng/mL

80 ng/mL

 

NMeFOSE

96.2 ± 3.0

100.3 ± 0.2

100.9 ± 2.0

 

NEtFOSE

96.7 ± 8.0

101.0 ± 1.7

100.6 ± 1.0

 

Per- and polyfluoroether carboxylic acids

Spike levels*

0.8 ng/mL,

except HFPO-DA & ADONA 1.6 ng/mL

5 ng/mL,

except HFPO-DA & ADONA 10 ng/mL

16 ng/mL,

except HFPO-DA & ADONA 32 ng/mL

HFPO-DA

95.3 ± 10.6

101.6 ± 2.9

102.2 ± 2.0

ADONA

100.0 ± 9.7

108.4 ± 0.5

109.6 ± 1.9

PFMPA

98.5 ± 6.4

99.6 ± 1.1

96.5 ± 0.6

PFMBA

98.7 ± 7.0

100.8 ± 2.6

98.3 ± 0.5

NFDHA

102.8 ± 9.6

106.2 ± 3.4

102.0 ± 3.4

Ether sulfonic acids

Spike levels*

1.6 ng/mL,

except PFEESA 0.8 ng/mL

10 ng/mL,

except PFEESA 5 ng/mL

32 ng/mL,

except PFEESA 16 ng/mL

9Cl-PF3ONS

93.9 ± 9.4

103.1 ± 1.5

102.3 ± 1.4

11Cl-PF3OUdS

91.2 ± 3.3

99.2 ± 2.0

100.4 ± 1.4

PFEESA

95.1 ± 13.1

106.6 ± 2.5

107.6 ± 1.2

Fluorotelomer carboxylic acids

 

Spike levels*

10 ng/mL,

except 3:3 FTCA 2 ng/mL

62.5 ng/mL,

except 3:3 FTCA 12.5 ng/mL

200 ng/mL,

except 3:3 FTCA 40 ng/mL

3:3FTCA

102.6 ± 8.9

98.4 ± 2.5

98.9 ± 2.6

5:3FTCA

103.0 ± 6.0

100.9 ± 1.2

103.0 ± 1.7

7:3FTCA

90.7 ± 8.5

96.9 ± 3.2

105.8 ± 3.0

*The concentration of the spikes, which correspond to the lowest calibration standard, CS1, refers to the concentration in the final extract. The spiked sample concentration in the actual water samples is 100 times lower due to the 100-fold enrichment resulting from the sample preparation.

Table 3.Recovery and precision (n = 3) of native PFAS compounds at 3 spike levels (2x CS1, 12.5x CS1, 40x CS1) listed by compound class.

EIS compounds

Recovery in %

 

2x CS1*

12.5x CS1*

40x CS1*

13C4-PFBA

95.1 ± 2.7

96.6 ± 1.6

97.4 ± 1.1

13C5-PFPeA

98.2 ± 2.2

97.8 ± 1.0

98.0 ± 0.7

13C5-PFHxA

97.2 ± 1.4

97.6 ± 1.9

98.0 ± 2.3

13C4-PFHpA

102.0 ± 2.1

102.2 ± 3.0

102.0 ± 3.5

13C8-PFOA

95.8 ± 4.7

102.4 ± 1.7

99.0 ± 2.8

13C9-PFNA

98.0 ± 2.8

97.3 ± 5.2

99.1 ± 4.5

13C6-PFDA

98.1 ± 2.8

100.0 ± 1.1

100.9 ± 2.3

13C7-PFUnA

95.2 ± 0.7

97.3 ± 3.8

97.1 ± 1.5

13C2-PFDoA

92.5 ± 4.9

93.4 ± 2.7

92.5 ± 1.1

13C2-PFTeDA

89.3 ± 4.1

89.8 ± 3.9

87.9 ± 3.3

13C3-PFBS

95.0 ± 7.2

100.3 ± 2.1

97.4 ± 1.1

13C3-PFHxS

92.4 ± 6.1

102.7 ± 1.8

100.0 ± 3.7

13C8-PFOS

98.4 ± 2.3

101.4 ± 2.6

106.2 ± 5.4

13C2-4:2FTS

84.4 ± 9.2

99.4 ± 4.8

92.8 ± 3.1

13C2-6:2FTS

82.9 ± 5.2

91.9 ± 5.2

95.5 ± 0.4

13C2-8:2FTS

78.0 ± 5.6

83.0 ± 5.9

91.0 ± 2.1

13C8-PFOSA

89.8 ± 7.6

95.4 ± 2.7

95.3 ± 3.1

D3-NMeFOSA

76.1 ± 12.1

76.9 ± 3.1

80.9 ± 2.0

 

D5-NEtFOSA

77.9 ± 11.1

74.9 ± 1.5

81.1 ± 2.5

 

D3-NMeFOSAA

87.2 ± 3.2

90.9 ± 1.8

93.0 ± 1.4

 

D5-NEtFOSAA

84.3 ± 5.0

87.6 ± 1.9

94.8 ± 0.5

 

D7-NMeFOSE

87.5 ± 5.6

89.3 ± 1.5

92.6 ± 1.9

 

D9-NEtFOSE

89.0 ± 6.6

90.7 ± 0.1

95.5 ± 1.3

 

13C3-HFPO-DA

101.0 ± 2.5

100.2 ± 0.5

100.1 ± 2.8

 

*The concentration of the native PFAS varied between the spiking levels; however, the spiking levels of the EIS standards were the same in each.

 

Table 4.Recovery and precision (n = 3) of Extracted Internal Standards (EIS) calculated for the water samples spiked with the native PFAS at three different concentration levels (2x CS1, 12.5x CS1, 40x CS1)

CONCLUSIONS

This application note presents the workflow for EPA method 1633 to analyze 40 PFAS compounds in water samples by applying SPE extraction using a Supelclean™ ENVI-WAX™ cartridge, followed by additional dispersive clean-up with bulk Supelclean™ ENVI-Carb™ adsorbents and quantification by LC-MS/MS employing Ascentis® Express PFAS analytical and delay columns. The method demonstrated robust performance with excellent recoveries for all 40 PFAS compounds and 24 extracted internal standards (EIS) well within acceptance limits for aqueous matrices listed in the method at the three recommended fortification levels. The calculated RSDs were below 20%, further indicating a satisfactory precision. This proves the suitability of PTFE-free Visiprep™ SPE Vacuum Manifold with Supelclean™ ENVI-WAX™ SPE cartridges for the extraction of PFAS compounds from water samples and of Supelclean™ ENVI-Carb™ for clean-up prior to subsequent LC-MS/MS analysis according to EPA 1633.

See more on PFAS testing at SigmaAldrich.com/PFAS

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REFERENCES

1.
EPA Method 1633, Revision A, Analysis of Per- and Polyfluoroalkyl Substances (PFAS) in Aqueous, Solid, Biosolids, and Tissue Samples by LC-MS/MS. U.S. EPA. 2024. . [Internet]. Available from: www.epa.gov/system/files/documents/2024-12/method-1633a-december-5-2024-508-compliant.pdf
2.
US EPA. CWA Analytical Methods for Per- and Polyfluorinated Alkyl Substances (PFAS). [accessed 2024 Oct 2]. [Internet]. Available from: https://www.epa.gov/cwa-methods/cwa-analytical-methods-and-polyfluorinated-alkyl-substances-pfas
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