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HomeSmall Molecule HPLCLC-MS/MS Analysis of 40 Per- and Polyfluoroalkyl Substances (PFAS) in Solvents: A Modified EPA Method 1633A Approach

LC-MS/MS Analysis of 40 Per- and Polyfluoroalkyl Substances (PFAS) in Solvents: A Modified EPA Method 1633A Approach

Lara Rosenberger, Senior Scientist
Yannick Hövelmann, Senior Scientist

Abstract

A modified workflow based on EPA Method 1633A was applied for the analysis of 40 per- and polyfluoroalkyl substances (PFAS) in a range of solvents. Solid-phase extraction (SPE) combined with LC-MS/MS was used to assess the PFAS background of 19 solvent products, including water, acetonitrile, and methanol of different grades. Ensuring solvent purity was identified as essential for achieving reliable PFAS measurements and for preventing false positives or overestimation of PFAS concentrations.

Section Overview

Introduction

Per- and polyfluorinated alkyl substances (PFAS) are a class of synthetic compounds that have been widely used in consumer and commercial products for several decades because of their versatile physical and chemical properties (e.g., in water repellents, firefighting foams, cookware, and food packaging). Due to their chemical stability arising from the strong carbon-fluorine bond, their persistence, and their toxicity, these compounds have gained increasing attention with respect to contamination of water, soil, and food, along with the associated bioaccumulation in humans and animals.

Guidance for PFAS testing regulations has been issued by the United States Environmental Protection Agency (US EPA) and the European Union (EU) to support the protection of environmental and human health, including EPA methods 533, 537.1, and 1633A and FDA method C-010.03.1-6

In December 2024, the US EPA released the final version of EPA Method 1633A, which provides extensive guidance for environmental PFAS testing. The method was validated across multiple laboratories and includes the analysis of 40 PFAS compounds in a wide range of sample matrices, including aqueous samples such as wastewater, surface water, and groundwater, solid samples such as soil, sediment, and biosolids, and biological samples such as fish and other tissues. For PFAS analysis in food, advisories were issued by the U.S. Food and Drug Administration (FDA) by releasing the method C-010.03, which employs a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) procedure followed by dispersive solid phase extraction (dSPE) for clean-up before liquid chromatography-mass spectrometry (LC-MS) detection.

The analysis of PFAS can be performed using the analytical methods described in the guidance documents by following their established matrix-specific extraction protocols for detecting these contaminants in various sample matrices. A key requirement for the successful application of these methods is the high purity of the solvents used, such as water, acetonitrile, and methanol, which are required during both the analytical and preparative stages of the analysis, such as the preparation of the mobile phase, extraction reagent, and calibration standards. The high sensitivity of LC-MS instruments and the need for trace-level PFAS detection necessitate the use of solvents that are free of any PFAS contamination. Any PFAS present in these solvents can lead to misleading results in the form of false positives or overestimation of PFAS levels, which compromises the validity of the analytical results and the conclusions. Ensuring solvent purity is therefore essential for achieving accurate and reliable PFAS analysis.

This study describes the analysis of 40 PFAS analytes in bottled water, acetonitrile, and methanol from two portfolio brands (Supelco® and Sigma-Aldrich®) across various solvent grades, including HPLC grade, HPLC plus grade, gradient grade, UHPLC grade, and LC-MS grade. Solid-phase extraction (SPE) was performed using Supelclean™ ENVI-WAX™ SPE cartridges in combination with a PTFE-free Visiprep™ SPE vacuum manifold. The extracts were subsequently analyzed by LC-MS/MS using analytical and delay Fused-Core® Ascentis® Express PFAS columns.

Experimental

Solutions and Standards Preparation

40 native and 31 isotopically labeled PFAS standards  were used as methanolic 50 µg/mL stock solutions. Following the recommendations of the EPA 1633A method, these native and isotopically labeled standards were then diluted to prepare seven calibration solutions (CS1 - CS7). The calibration solutions contained the native PFAS compounds at concentrations ranging from 0.2 to 5 ng/mL for CS1 and from 62.5 to 1560 ng/mL for CS7, as specified in Table 4 of EPA Method 1633A, to establish the working range of the MS instrument.

Sample Preparation for Solvent testing

Sample collection and preparation were performed according to EPA Method 1633A with slight modifications. Three solvents, namely water, acetonitrile, and methanol (1 L bottle size), were examined for potential PFAS contamination across the grades listed in Tables 3 to 5. Volumes of 500 mL of water, 250 mL of acetonitrile, or 250 mL of methanol were transferred into HDPE bottles fitted with linerless polypropylene caps. To the acetonitrile and methanol samples, 500 mL or 250 mL of UHPLC grade water (1.03728) were added, respectively, to dilute the organic solvents and prevent poor recovery of selected PFAS compounds due to insufficient retention during the SPE loading step. The samples were fortified with 24 isotopically labeled standards (13C or D), which served as extracted internal standards (EIS).

For SPE, Supelclean™ ENVI-WAX™ SPE tubes (500 mg/6 mL, 54057-U) were fitted 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 methanol and equilibrated with 5 mL of aqueous 0.3 M formic acid. The samples (500 mL of water, 500 mL of diluted methanol or 750 mL of diluted acetonitrile as described above) were then loaded and passed through the cartridges. The washing step consisted of two rinses with 5 mL of water followed by 5 mL of 0.1 M formic acid in water/methanol (1:1, v/v). The cartridges were subsequently dried for 1 min before elution of the analytes with 5 mL of 1.0% NH4OH in methanol into collection tubes that contained seven additional isotopically labeled standards. These standards, used as non-extracted internal standards (NIS), were included to evaluate the recovery of the EIS compounds and assess the applicability of the method. Prior to LC-MS/MS analysis described below, 25 µL of concentrated acetic acid (5.33001) were added to the eluates.

Instrumental Analysis

LC-MS/MS analysis was performed using an Agilent 1290 Infinity II instrument coupled to an Agilent 6495C triple quadrupole mass spectrometer. Analyte separation was achieved on an Ascentis® Express PFAS 90 Å column (5 cm x 2.1 mm, 2.7 µm, 53557-U) used as the analytical column. An Ascentis® Express PFAS Delay 160 Å column (5 cm x 3.0 mm, 2.7µm, 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 adsorption of PFAS to glass surface. The LC-MS employed for the analysis are summarized in Tables 1 and 2, including the used MRM transitions for quantification of the native PFAS by stable-isotope dilution. The allocation of extracted internal standards followed the specifications of EPA Method 1633A.

LC Conditions

Instrument:

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

Columns:

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

Delay Column: Ascentis® Express PFAS Delay 160 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 the gradient table

Column temp.:

40 °C

Detector:

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

Injection:

2 µL

Sample(s):

See text

Table 1.LC-MS 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

0.9995

2

PFMPA

Perfluoro-3-methoxypropanoic acid

229.0 → 85.0

12

2.4

0.9994

3

3:3FTCA

3-Perfluoropropyl propanoic acid

241.0 → 177.0

3

2.8

0.9978

4

PFPeA

Perfluoropentanoic acid

263.0 → 219.0

4

3.3

0.9995

5

PFMBA

Perfluoro-4-methoxybutanoic acid

279.0 → 85.0

8

3.6

0.9996

6

4:2FTS

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

327.0 → 307.0

20

4.0

0.9930

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

0.9985

9

PFHxA

Perfluorohexanoic acid

313.0 → 269.0

4

4.2

0.9993

10

HFPO-DA

Hexafluoropropylene oxide dimer acid

285.0 → 169.0

4

4.5

0.9984

11

PFEESA

Perfluoro(2-ethoxyethane)sulfonic acid

315.0 → 135.0

28

4.6

0.9982

12

5:3FTCA

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

341.0 → 237.0

11

4.7

0.9994

13

PFHpA

Perfluoroheptanoic acid

363.0 → 319.0

8

5.0

0.9993

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

0.9993

16

6:2FTS

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

427.0 → 407.0

24

5.3

0.9932

17

PFOA

Perfluorooctanoic acid

413.0 → 369.0

8

5.5

0.9992

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

0.9995

20

PFNA

Perfluoronanoic acid

463.0 → 419.0

8

6.0

0.9991

21

PFHpS

Perfluoroheptanesulfonic acid

449.0 → 80.0

68

6.2

0.9990

22

8:2FTS

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

527.0 → 507.0

28

6.3

0.9937

23

PFDA

Perfluorodecanoic acid

513.0 → 469.0

8

6.5

0.9987

24

NMeFOSAA

N-methyl perfluorooctanesulfonamidoacetic acid

570.0 → 419.0

19

6.6

0.9981

25

PFOS

Perfluorooctanesulfonic acid

499.0 → 80.0

72

6.6

0.9995

26

NEtFOSAA

N-ethyl perfluorooctanesulfonamidoacetic acid

584.0 → 419.0

19

6.7

0.9993

27

PFUnA

Perfluoroundecanoic acid

563.0 → 519.0

8

6.9

0.9994

28

9Cl-PF3ONS

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

531.0 → 351.0

 

28

7.0

0.9989

29

PFNS

Perfluorononanesulfonic acid

549.0 → 80.0

79

7.1

0.9992

30

PFDoA

Perfluorododecanoic acid

613.0 → 569.0

8

7.3

0.9990

31

PFDS

Perfluorodecanesulfonic acid

599.0 → 80.0

79

7.5

0.9985

32

PFTrDA

Perfluorotridecanoic acid

663.0 → 619.0

11

7.7

0.9989

33

11Cl-PF3OUdS

 

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

630.9 → 451.0

 

32

7.8

0.9985

34

PFOSA

Perfluorooctanesulfonamide

498.0 → 78.0

35

8.1

0.9990

35

PFTeDA

Perfluorotetradecanoic acid

713.0 → 669.0

11

8.1

0.9982

36

PFDoS

Perfluorododecanesulfonic acid

699.0 → 80.0

80

8.3

0.9996

37

NMeFOSE

N-methyl perfluorooctanesulfonamidoethanol

616.0 → 59.0

11

9.2

0.9985

38

NMeFOSA

N-methyl perfluorooctanesulfonamide

512.0 → 169.0

27

9.4

0.9985

39

NEtFOSE

N-ethyl perfluorooctanesulfonamidoethanol

630.0 → 59.0

15

9.6

0.9988

40

NEtFOSA

N-ethyl perfluorooctanesulfonamide

526.0 → 169.0

27

9.7

0.9991

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

Results & Discussion

A representative chromatogram of the calibration solution 5 (CS5) containing the 40 native compounds is shown in Figure 1. As indicated in Table 2, linear calibration curves with R2 ≥0.99 were obtained for all PFAS analytes.

Chromatogram showing separated peaks of 40 PFAS analytes from CS5 measured by LC-MS/MS in methanol with water, ammonium hydroxide, and acetic acid.

Figure 1.LC-MS/MS chromatogram of 40 PFAS compounds obtained for CS5 in methanol containing 4% water, 1% ammonium hydroxide, and 0.6% acetic acid (Peak IDs see Table 2).

Potential PFAS contamination in the solvents was quantified by stable-isotope dilution using extracted internal standards (EIS) that were added to the sample (n = 2) prior to SPE. Recovery of the EIS surrogates was assessed using the non-extracted internal standards (NIS), which were spiked into the concentrated extract after the SPE step. The PFAS evaluation of the three solvents across the various grades revealed negligible levels of all investigated PFAS compounds, as all measured values were below the respective lower limits of quantification (LOQ) specified in EPA method 1633A (Table 3) for each of the compounds. To account for the varying analyzed sample volumes (500 mL of water, 250 mL of pure methanol, and 250 mL of pure acetonitrile) which result in different LOQs for each solvent, the LOQ for each PFAS compound was additionally calculated for a 1 L bottle size and expressed in parts per trillion (ppt) to improve comparability of the data (Table 4).

Tables 5, 6, and 7 present the recoveries determined for the 24 EIS surrogates in the investigated solvents, calculated using the seven NIS compounds that were spiked after extraction. The EPA requirements for acceptable recoveries were met for all analytes examined, as outlined in Table 6 of EPA Method 1633A1, with most compounds exhibiting recoveries between 73.4% and 109.8%. Lower recoveries between 20.7% and 39.0% were observed for d7-NMeFOSE and d9-NEtFOSE in acetonitrile, which may be attributed to insufficient retention during the SPE loading step caused by the higher eluotropic strength of the acetonitrile samples despite prior dilution.

Solvent (Brand)

Grade

Cat. No.

Results for each of the 40 PFAS analytes following EPA method 1633A

 

Acetonitrile (Supelco®)

HPLC grade

1.14291

< LOQ

Gradient grade

1.00030

< LOQ

UHPLC grade

1.03725

< LOQ

LC-MS grade

1.00029

< LOQ

Acetonitrile (Sigma-Aldrich®)

Gradient grade

34851

< LOQ

UHPLC grade

900667

< LOQ

Methanol (Supelco®)

HPLC grade

MX0475

< LOQ

Gradient grade

MX0488

< LOQ

UHPLC grade

1.03726

< LOQ

LC-MS grade

1.06035

< LOQ

Methanol (Sigma-Aldrich®)

HPLC grade

34860

< LOQ

HPLC plus grade

646377

< LOQ

Gradient grade

34885

< LOQ

UHPLC grade

900688

< LOQ

Water (Supelco®)

UHPLC grade

1.03728

< LOQ

LC-MS grade

1.15333

< LOQ

Water (Sigma-Aldrich®)

HPLC grade

270733

< LOQ

Gradient grade

34877

< LOQ

UHPLC grade

900682

< LOQ

Table 3.Overview of the investigated solvent grades and the corresponding results for the PFAS compounds

Native PFAS compounds

Water Samples LOQ (ppt)

Methanol Samples LOQ (ppt)

Acetonitrile Samples LOQ (ppt)

PFBA

8

16

16

PFPeA

4

8

8

PFHxA

2

4

4

PFHpA

PFOA

PFNA

PFDA

PFUnA

PFDoA

PFTrDA

PFTeDA

Native PFAS compounds

Water Samples LOQ (ppt)

Methanol Samples LOQ (ppt)

Acetonitrile Samples LOQ (ppt)

PFBS

2

4

4

PFPeS

PFHxS

PFHpS

PFOS

PFNS

PFDS

PFDoS

Native PFAS compounds

Water Samples LOQ (ppt)

Methanol Samples LOQ (ppt)

Acetonitrile Samples LOQ (ppt)

4:2FTS

8

16

16

6:2FTS

8:2FTS

Native PFAS compounds

Water Samples LOQ (ppt)

Methanol Samples LOQ (ppt)

Acetonitrile Samples LOQ (ppt)

PFOSA

2

4

4

NMeFOSA

NEtFOSA

Native PFAS compounds

Water Samples LOQ (ppt)

Methanol Samples LOQ (ppt)

Acetonitrile Samples LOQ (ppt)

NMeFOSAA

2

4

4

NEtFOSAA

Native PFAS compounds

Water Samples LOQ (ppt)

Methanol Samples LOQ (ppt)

Acetonitrile Samples LOQ (ppt)

NMeFOSE

20

40

40

NEtFOSE

Native PFAS compounds

Water Samples LOQ (ppt)

Methanol Samples LOQ (ppt)

Acetonitrile Samples LOQ (ppt)

HFPO-DA

8

16

16

ADONA

PFMPA

4

8

8

PFMBA

NFDHA

Native PFAS compounds

Water Samples LOQ (ppt)

Methanol Samples LOQ (ppt)

Acetonitrile Samples LOQ (ppt)

9Cl-PF3ONS

8

16

16

11Cl-PF3OUdS

PFEESA

4

8

8

Native PFAS compounds

Water Samples LOQ (ppt)

Methanol Samples LOQ (ppt)

Acetonitrile Samples LOQ (ppt)

3:3FTCA

8

16

16

5:3FTCA

7:3FTCA

4

8

8

EIS compoundsRecovery in %
 Water Water Acceptance criteria of EPA method 1633A (aqueous matrices)
(Supelco®)(Sigma-Aldrich®)
 UHPLC gradeLC-MS gradeHPLC gradeGradient gradeUHPLC grade 
13C4-PFBA98100.499.1101.2925 ─ 130
13C5-PFPeA97.2103.6102.1104.2102.140 ─ 130
13C5-PFHxA94.499.998.9100.299.440 ─ 130
13C4-PFHpA94.9102.699.2102.799.240 ─ 130
13C8-PFOA95.910096.898.897.240 ─ 130
13C9-PFNA96102.5100.899.998.940 ─ 130
13C6-PFDA95.810197.799.895.640 ─ 130
13C7-PFUnA98.7101.1100.499.797.130 ─ 130
13C2-PFDoA92.195.895.198.192.310 ─ 130
13C2-PFTeDA89.293.392.592.588.410 ─ 130
13C3-PFBS102.3109.8106.7105.8104.940 ─ 135
13C3-PFHxS95.6105.698.8103.4100.440 ─ 130
13C8-PFOS97.4106.4100.1102.1100.640 ─ 130
13C2-4:2FTS95.5104.298.893.797.240 ─ 200
13C2-6:2FTS92.3101.494.698.793.340 ─ 200
13C2-8:2FTS88.297.195.291.491.440 ─ 300
13C8-PFOSA88.797.997.196.990.740 ─ 130
D3-NMeFOSA75.583.395.291.780.310 ─ 130
D5-NEtFOSA7685.796.293.379.510 ─ 130
D3-NMeFOSAA92.8103.1102.3101.395.640 ─ 170
D5-NEtFOSAA87.5100.794.795.791.625 ─ 135
D7-NMeFOSE8593.492.691.790.410 ─ 130
D9-NEtFOSE83.391.889.789.387.410 ─ 130
13C3-HFPO-DA99.3105.7105.7105.3105.540 ─ 130
EIS compoundsRecovery in %
 Acetonitrile Acetonitrile Acceptance criteria of EPA method 1633A (aqueous matrices)
(Supelco®)(Sigma-Aldrich®)
 HPLC gradeGradient gradeUHPLC gradeLC-MS gradeGradient gradeUHPLC grade 
13C4-PFBA99100.9100.399.499.3101.15 ─ 130
13C5-PFPeA102103.6103.3102.2102.5104.140 ─ 130
13C5-PFHxA99.4100.898.697.696.899.140 ─ 130
13C4-PFHpA99.399.7101.3100.498.499.640 ─ 130
13C8-PFOA96.497.597.797.29799.240 ─ 130
13C9-PFNA99101.1100.9101.399.6103.140 ─ 130
13C6-PFDA95.8101.4103.197.296.397.340 ─ 130
13C7-PFUnA99.4104.9102.8100.398.510230 ─ 130
13C2-PFDoA94.297.998.695.997.698.510 ─ 130
13C2-PFTeDA96.399100.197.998.398.610 ─ 130
13C3-PFBS101.4101.2106.2101.7100.8104.940 ─ 135
13C3-PFHxS96.496.996.794.693.293.640 ─ 130
13C8-PFOS95.6100.496.696.19899.640 ─ 130
13C2-4:2FTS100.799.8101.197.796.9100.440 ─ 200
13C2-6:2FTS95.494.695.494.192.897.440 ─ 200
13C2-8:2FTS85.394.394.59290.79440 ─ 300
13C8-PFOSA76.882.773.476.777.677.940 ─ 130
D3-NMeFOSA96.2105.299.296.296.899.210 ─ 130
D5-NEtFOSA95.5105.798.598.299.598.210 ─ 130
D3-NMeFOSAA99.4104.699.6101.7103.2105.440 ─ 170
D5-NEtFOSAA96.5100.896.396.599.6101.125 ─ 135
D7-NMeFOSE21.523.524.920.724.52210 ─ 130
D9-NEtFOSE33.636.63932.138.234.510 ─ 130
13C3-HFPO-DA104.2105.4105.4104.2103.6106.440 ─ 130

EIS compounds

Recovery in %

 

Methanol

(Supelco®)

Methanol

(Sigma-Aldrich®)

Acceptance criteria of EPA method 1633A (aqueous matrices)

 

HPLC      grade

Gradient grade

UHPLC grade

LC-MS grade

HPLC    grade

HPLC grade plus

Gradient grade

UHPLC    grade

 

13C4-PFBA

98.3

99.0

99.7

99.9

102.4

99.7

100.7

99.8

5 ─ 130

13C5-PFPeA

100.1

102.9

103.0

103.4

103.2

100.1

103.6

102.8

40 ─ 130

13C5-PFHxA

96.6

98.7

98.7

98.4

103.5

98.2

101.5

100.0

40 ─ 130

13C4-PFHpA

98.7

100.2

100.5

100.1

101.7

100.9

102.3

102.2

40 ─ 130

13C8-PFOA

94.3

95.4

98.4

97.5

99.1

96.1

97.9

97.8

40 ─ 130

13C9-PFNA

99.0

98.8

98.6

100.9

101.9

100.2

100.5

100.5

40 ─ 130

13C6-PFDA

98.4

101.5

99.8

102.6

99.7

99.9

99.9

100.2

40 ─ 130

13C7-PFUnA

98.9

99.9

102.1

103.4

103.3

102.5

100.0

100.8

30 ─ 130

13C2-PFDoA

96.7

97.7

98.9

99.1

99.1

102.0

96.0

99.3

10 ─ 130

13C2-PFTeDA

97.1

99.2

100.7

99.3

98.1

99.8

94.7

97.1

10 ─ 130

13C3-PFBS

101.3

104.4

107.9

101.7

108.3

103.3

106.5

101.4

40 ─ 135

13C3-PFHxS

95.2

97.2

97.9

97.4

103.8

95.5

100.9

99.3

40 ─ 130

13C8-PFOS

94.2

101.1

97.6

99.6

103.0

99.7

106.2

96.1

40 ─ 130

13C2-4:2FTS

96.8

100.7

103.0

98.3

103.4

98.3

100.8

98.1

40 ─ 200

13C2-6:2FTS

92.7

97.2

100.2

95.8

99.8

95.1

98.5

93.7

40 ─ 200

13C2-8:2FTS

92.5

104.7

100.2

92.8

95.4

91.6

98.5

94.6

40 ─ 300

13C8-PFOSA

95.6

98.2

97.2

98.2

102.0

99.4

102.3

94.9

40 ─ 130

D3-NMeFOSA

90.7

96.1

96.8

97.8

101.5

95.4

99.3

94.8

10 ─ 130

D5-NEtFOSA

95.3

98.8

98.8

99.0

101.9

99.6

96.8

96.7

10 ─ 130

D3-NMeFOSAA

102.5

105.5

104.8

104.2

108.6

106.5

109.4

100.3

40 ─ 170

D5-NEtFOSAA

98.6

102.5

101.4

101.1

104.2

100.8

109.1

100.2

25 ─ 135

D7-NMeFOSE

96.7

104.7

100.3

100.0

104.9

101.3

104.0

97.0

10 ─ 130

D9-NEtFOSE

95.4

100.2

99.5

98.7

104.3

98.8

101.4

96.4

10 ─ 130

13C3-HFPO-DA

102.3

105.6

106.1

104.9

106.3

104.1

107.1

105.2

40 ─ 130

Conclusion

An adjusted workflow based on EPA method 1633A was applied for the analysis of 40 PFAS compounds in water, methanol, and acetonitrile of various grades using SPE with a Supelclean™ ENVI-WAX™ cartridg,e followed by LC-MS/MS quantification with Ascentis® Express PFAS analytical and delay columns. Robust method performance was demonstrated by satisfactory recovery values for all 24 EIS surrogates, which fell within the acceptance range of EPA method 1633A. None of the investigated solvents showed PFAS contamination at levels exceeding the respective LOQs defined in EPA Method 1633A, indicating their suitability for trace-level PFAS analysis according to the relevant analytical methods issued by regulatory agencies. Laboratories operating under the EPA 1633 guideline remain responsible for independent verification of each reagent lot to avoid issues with method blanks and other quality control samples. When available, certification of PFAS levels in additives and solvents provided by the supplier is sufficient for meeting this requirement.

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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.. Available from: https://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]. Available from: https://www.epa.gov/cwa-methods/cwa-analytical-methods-and-polyfluorinated-alkyl-substances-pfas
3.
Per- and polyfluoroalkyl substances (PFAS) - ECHA. Europa.eu. [accessed 2024 Oct 2].. Available from: https://echa.europa.eu/hot-topics/perfluoroalkyl-chemicals-pfas
4.
Method C-010.03 Determination of 30 Per and Polyfluoroalkyl Substances (PFAS) in Food and Feed using Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS). United States Food and Drug Administration, April 2024. Available from: https://www.fda.gov/media/131510/download
5.
Method 537.1 Determination of Selected Per- and Polyfluorinated Alkyl Substances in Drinking Water by Solid Phase Extraction and Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS). U.S. Environmental Protection Agency, Washington, DC, 2020. Available from: https://cfpub.epa.gov/si/si_public_record_Report.cfm?dirEntryId=343042&Lab=NERL
6.
Method 533 Determination of Per- and Polyfluoroalkyl Substances in Drinking Water by Isotope Dilution Anion Exchange Solid Phase Extraction and Liquid Chromatography/Tandem Mass Spectrometry. United States Environmental Protection Agency, Office of Water, December 2019. Available from: https://www.epa.gov/dwanalyticalmethods/method-533-determination-and-polyfluoroalkyl-substances-drinking-water-isotope
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