- Single cartridge with both WAX and carbon beds simplifies workflows.
- Factory-packed filter aid saves time and prevents clogs.
- Ultra-clean sorbents ensure MDLs are met.
Streamline PFAS Sample Preparation with Dual-Bed Resprep PFAS Cartridges
Effective sample preparation is essential for accurate trace-level PFAS analysis in complex sample matrices, such as non-potable waters, solids, biosolids, and tissues. Solid phase extraction (SPE) is typically used, but good results are difficult to achieve if background PFAS are present or if sample components clog the SPE cartridges. EPA Method 1633, which has been validated in multiple laboratories, uses a wool-packed weak anion exchange (WAX) cartridge for matrix extraction, followed by a dispersive graphitized carbon black (dGCB) cleanup step, with many labs adopting a carbon cartridge instead of using dGCB. While effective, this two-cartridge approach with manually packed wool adds extra time, complexity, and risk of introducing contaminants to the sample preparation process.
Resprep PFAS Cartridges Are a Simpler Solution
PFAS SPE sample preparation can be streamlined significantly with dual-bed Resprep PFAS cartridges, which combine SPE extraction and carbon cleanup into a single cartridge. In this fast, simple workflow, the ultra-clean WAX and CarboPrep Plus sorbents used in Resprep PFAS cartridges ensure that method performance requirements will be met. In addition, an optional, factory-packed filter aid eliminates the time and variability associated with manually packing glass wool. This ready-to-use solution prevents clogging so that even dirty matrices can be processed quickly with a single extraction.
Meet Performance Requirements Quickly and Consistently
Developed specifically to help labs meet PFAS performance requirements, dual-bed Resprep PFAS cartridges contain ultra-clean, high-quality WAX and carbon sorbent layers that provide effective extraction and cleanup. Every lot of our WAX sorbent is tested against Method 1633 PFAS analytes to demonstrate cleanliness and to ensure it does not contribute background PFAS. In addition, our high-performance CarboPrep Plus sorbent provides more effective and consistent cleanup than other carbon materials. The combination of both sorbents in a single cartridge makes sample preparation much faster and results in clean extracts and excellent analytical performance (Figure 1 and Table I).
LC_EV0599
Peaks
| Peaks | tR (min) | Conc. (ng/L) | Precursor 1 | Product 1 | Product 2 | Precursor 2 | Product 1 | |
|---|---|---|---|---|---|---|---|---|
| 1. | Perfluoro-n-[1,2,3,4- 13C3]butanoic acid (13C3-PFBA) | 1.485 | 5 | 216 | 172 | – | – | – |
| 2. | Perfluoro-n-[1,2,3,4- 13C4]butanoic acid (13C4-PFBA) | 1.487 | 10 | 217 | 172 | – | – | – |
| 3. | Perfluorobutanoic acid (PFBA) | 1.489 | 10 | 213 | 169 | – | – | – |
| 4. | Perfluoro-3-methoxypropanoic acid (PFMPA) | 2.007 | 5 | 229 | 85 | – | – | – |
| 5. | 3-Perfluoropropyl propanoic acid (3:3FTCA) | 2.7 | 12.5 | 241 | 177 | 117 | – | – |
| 6. | Perfluoro-n-[1,2,3,4,5- 13C5]pentanoic acid (13C5-PFPeA) | 2.765 | 5 | 268 | 223 | – | – | – |
| 7. | Perfluoropentanoic acid (PFPeA) | 2.768 | 5 | 263 | 219 | 69 | – | – |
| 8. | Perfluorobutane sulfonate (PFBS) | 3.006 | 2.5 | 299 | 80 | 99 | – | – |
| 9. | Sodium perfluoro-1-[2,3,4- 13C3]butanesulfonate (13C3-PFBS) | 3.007 | 2.5 | 302 | 80 | 99 | – | – |
| 10. | Perfluoro-4-methoxybutanoic acid (PFMBA) | 3.071 | 5 | 279 | 85 | – | – | – |
| 11. | Perfluoro(2-ethoxyethane)sulfonic acid (PFEESA) | 3.333 | 5 | 315 | 135 | 83 | – | – |
| 12. | Nonafluoro-3,6-dioxaheptanoic acid (NFDHA) | 3.493 | 5 | 295 | 201 | 85 | – | – |
| 13. | 1H,1H,2H,2H-perfluorohexane sulfonate (4:2 FTS) | 3.545 | 10 | 327 | 307 | 81 | – | – |
| 14. | Sodium 1H,1H,2H,2H-perfluoro-1-[1,2- 13C2]hexane sulfonate (13C2-4:2FTS) | 3.55 | 5 | 329 | 81 | 309 | – | – |
| 15. | Perfluorohexanoic acid (PFHxA) | 3.608 | 2.5 | 313 | 269 | 119 | – | – |
| 16. | Perfluoro-n-[1,2,3,4,6- 13C2]hexanoic acid (13C2-PFHxA) | 3.609 | 2.5 | 315 | 270 | 119 | – | – |
| 17. | Perfluoro-n-[1,2,3,4,6- 13C5]hexanoic acid (13C5-PFHxA) | 3.61 | 2.5 | 318 | 273 | 120 | – | – |
| 18. | Perfluoropentane sulfonate (PFPeS) | 3.718 | 2.5 | 349 | 80 | 99 | – | – |
| 19. | 2,3,3,3-Tetrafluoro-2-(1,1,2,2,3,3,3-heptafluoropropoxy13C3-propanoic acid (13C3-HFPO-DA) | 3.79 | 10 | 287 | 169 | 185 | – | – |
| 20. | Hexafluoropropylene oxide (HFPO-DA) | 3.795 | 10 | 285 | 169 | 185 | – | – |
| 21. | Perfluoroheptanoic acid (PFHpA) | 4.174 | 2.5 | 363 | 319 | 169 | – | – |
| 22. | Perfluoro-n-[1,2,3,4- 13C4]heptanoic acid (13C4-PFHpA) | 4.174 | 2.5 | 367 | 322 | – | – | – |
| 23. | Perfluoro-1-hexane[18O2]sulfonic acid (18O2-PFHxS) | 4.218 | 2.5 | 403 | 84 | – | – | – |
| 24. | Sodium perfluoro-1-[1,2,3- 13C3]hexanesulfonate (13C3-PFHxS) | 4.218 | 2.5 | 402 | 80 | 99 | – | – |
| 25. | Perfluorohexane sulfonate (PFHxS) | 4.22 | 2.5 | 399 | 80 | 99 | – | – |
| 26. | <a class="cmpd_link" title="View compound information for 4,8-Dioxa-3H-perfluorononanoic acid (ADONA)” title=”View compound information for 4,8-Dioxa-3H-perfluorononanoic acid (ADONA)” href=”https://ez.restek.com/compound/view/en/919005-14-4/4,8-Dioxa-3H-perfluorononanoic acid”>4,8-Dioxa-3H-perfluorononanoic acid (ADONA) | 4.232 | 10 | 377 | 251 | 85 | – | – |
| 27. | 2H,2H,3H,3H-Perfluorooctanoic acid (5:3FTCA) | 4.247 | 62.5 | 341 | 237 | 217 | – | – |
| 28. | 1H,1H,2H,2H-perfluorooctane sulfonate (6:2 FTS) | 4.58 | 10 | 427 | 407 | 81 | – | – |
| 29. | Sodium 1H,1H,2H,2H-perfluoro-1-[1,2-13C2]-octane sulfonate (13C2-6:2FTS) | 4.581 | 5 | 429 | 81 | 409 | – | – |
| 30. | Perfluoro-n-[ 13C8]octanoic acid (13C8-PFOA) | 4.598 | 2.5 | 421 | 376 | – | – | – |
| 31. | Perfluorooctanoic acid (PFOA) | 4.601 | 2.5 | 413 | 369 | 169 | – | – |
| 32. | Perfluoro-n-[ 13C4]octanoic acid (13C4-PFOA) | 4.601 | 2.5 | 417 | 172 | – | – | – |
| 33. | Perfluoroheptane sulfonate (PFHpS) | 4.621 | 2.5 | 449 | 80 | 99 | – | – |
| 34. | Perfluorononanoic acid (PFNA) | 4.944 | 2.5 | 463 | 419 | 219 | – | – |
| 35. | Perfluoro-n-[ 13C5]nonanoic acid (13C5-PFNA) | 4.944 | 1.25 | 468 | 423 | – | – | – |
| 36. | Perfluoro-n-[ 13C9]nonanoic acid (13C9-PFNA) | 4.944 | 1.25 | 472 | 427 | – | – | – |
| 37. | Perfluorooctane sulfonate (PFOS) | 4.949 | 2.5 | 499 | 80 | 99 | – | – |
| 38. | Sodium perfluoro-[ 13C4]octanesulfonate (13C4-PFOS) | 4.95 | 2.5 | 503 | 80 | 99 | – | – |
| 39. | Sodium perfluoro-[ 13C8]octanesulfonate (13C8-PFOS) | 4.95 | 2.5 | 507 | 80 | 99 | – | – |
| 40. | 3-Perfluoroheptyl propanoic acid (7:3FTCA) | 5.046 | 62.5 | 441 | 317 | 337 | – | – |
| 41. | 9-Chlorohexadecafluoro-3-oxanonane-1-sulfonic acid (9Cl-PF3ONS) | 5.114 | 10 | 531 | 351 | – | 533 | 353 |
| 42. | Perfluorodecanoic acid (PFDA) | 5.237 | 2.5 | 513 | 469 | 219 | – | – |
| 43. | Perfluoro-n-[1,2,3,4,5,6- 13C2]decanoic acid (13C2-PFDA) | 5.237 | 1.25 | 515 | 470 | – | – | – |
| 44. | Perfluoro-n-[1,2,3,4,5,6- 13C6]decanoic acid (13C6-PFDA) | 5.237 | 1.25 | 519 | 474 | – | – | – |
| 45. | 1H,1H,2H,2H-perfluorodecane sulfonate (8:2 FTS) | 5.238 | 10 | 527 | 507 | 81 | – | – |
| 46. | Sodium 1H,1H,2H,2H-perfluoro-1-[1,2- 13C2]-decane sulfonate (13C2-8:2FTS) | 5.238 | 5 | 529 | 81 | 509 | – | – |
| 47. | Perfluorononanesulfonic acid (PFNS) | 5.239 | 2.5 | 549 | 80 | 99 | – | – |
| 48. | N-methyl-d 3-perfluoro-1-octanesulfonamidoacetic acid (D3-NMeFOSAA) | 5.361 | 5 | 573 | 419 | – | – | – |
| 49. | N-methyl perfluorooctanesulfonamidoacetic acid (NMeFOSAA) | 5.366 | 2.5 | 570 | 419 | 483 | – | – |
| 50. | Perfluorodecanesulfonic acid (PFDS) | 5.475 | 2.5 | 599 | 80 | 99 | – | – |
| 51. | Perfluoroundecanoic acid (PFUnA) | 5.486 | 2.5 | 563 | 519 | 269 | – | – |
| 52. | Perfluoro-n-[1,2,3,4,5,6,7- 13C7]undecanoic acid (13C7-PFUnA) | 5.486 | 1.25 | 570 | 525 | – | – | – |
| 53. | N-ethyl-d 5-perfluoro-1-octanesulfonamidoacetic acid (D5-NEtFOSAA) | 5.487 | 5 | 589 | 419 | – | – | – |
| 54. | N-ethyl perfluorooctanesulfonamidoacetic acid (NEtFOSAA) | 5.487 | 2.5 | 584 | 419 | 526 | – | – |
| 55. | 11-Chloroeicosafluoro-3-oxaundecane-1-sulfonic acid (11Cl-PF3OUdS) | 5.59 | 10 | 631 | 451 | – | 633 | 453 |
| 56. | Perfluorooctanesulfonamide (PFOSA) | 5.669 | 2.5 | 498 | 78 | 478 | – | – |
| 57. | Perfluoro-1-[ 13C8]octanesulfonamide (13C8-PFOSA) | 5.669 | 2.5 | 506 | 78 | – | – | – |
| 58. | Perfluorododecanoic acid (PFDoA) | 5.691 | 2.5 | 613 | 569 | 319 | – | – |
| 59. | Perfluoro-n-[1,2- 13C2]dodecanoic acid (13C2-PFDoA) | 5.692 | 1.25 | 615 | 570 | – | – | – |
| 60. | Perfluorododecanesulfonic acid (PFDoS) | 5.861 | 2.5 | 699 | 80 | 99 | – | – |
| 61. | Perfluorotridecanoic acid (PFTrDA) | 5.876 | 2.5 | 663 | 619 | 169 | – | – |
| 62. | Perfluorotetradecanoic acid (PFTeDA) | 6.031 | 2.5 | 713 | 669 | 169 | – | – |
| 63. | Perfluoro-n-[1,2- 13C2]tetradecanoic acid (13C2-PFTeDA) | 6.031 | 1.25 | 715 | 670 | – | – | – |
| 64. | N-methyl perfluorooctanesulfonamide (NMeFOSA) | 6.158 | 2.5 | 512 | 219 | 169 | – | – |
| 65. | N-methyl-D 3-perfluoro-1-octanesulfonamide (D3-NMeFOSA) | 6.159 | 2.5 | 515 | 219 | – | – | – |
| 66. | N-methyl perfluorooctanesulfonamidoethanol (NMeFOSE) | 6.166 | 25 | 616 | 59 | – | – | – |
| 67. | N-methyl-D 7-perfluorooctanesulfonamidoethanol (D7-NMeFOSE) | 6.167 | 25 | 623 | 59 | – | – | – |
| 68. | N-ethyl-D 5-perfluoro-1-octanesulfonamide (D5-NEtFOSA) | 6.295 | 2.5 | 531 | 219 | – | – | – |
| 69. | N-ethyl perfluorooctanesulfonamide (NEtFOSA) | 6.296 | 2.5 | 526 | 219 | 169 | – | – |
| 70. | N-ethyl perfluorooctanesulfonamidoethanol (NEtFOSE) | 6.298 | 25 | 630 | 59 | – | – | – |
| 71. | N-ethyl-D 9-perfluorooctanesulfonamidoethanol (D9-NEtFOSE) | 6.298 | 25 | 639 | 59 | – | – | – |
Conditions
| Column | Force C18 (cat.# 9634252) | ||||||||||||||||||||||||
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
| Dimensions: | 50 mm x 2.1 mm ID | ||||||||||||||||||||||||
| Particle Size: | 1.8 µm | ||||||||||||||||||||||||
| Pore Size: | 100 Å | ||||||||||||||||||||||||
| Temp.: | 40 °C | ||||||||||||||||||||||||
| Standard/Sample | |||||||||||||||||||||||||
| Inj. Vol.: | 3 µL | ||||||||||||||||||||||||
| Mobile Phase | |||||||||||||||||||||||||
| A: | Water, 5 mM ammonium acetate | ||||||||||||||||||||||||
| B: | Methanol | ||||||||||||||||||||||||
| |||||||||||||||||||||||||
| Max Pressure: | ~400 bar |
| Detector | Waters Xevo TQ-S |
|---|---|
| Ion Mode: | ESI- |
| Mode: | MRM |
| Instrument | Waters ACQUITY Premier |
| Sample Preparation | Resprep PFAS cartridges (cat.# 28930) and a Thermo AutoTrace PFAS instrument were used for the following sample preparation procedure. 1. Spike 500 mL DI water with 200 µL of Wellington EPA-1633STK and 25 µL of Wellington MPFAC-HIF-ES. 2. Rinse cartridge with 15 mL of 1% ammonium hydroxide in methanol. 3. Rinse with 5 mL of 0.3 M formic acid in water. 4. Load sample onto SPE cartridge dropwise at 5 mL/min. 5. Rinse bottle with 5 mL DI water, load onto SPE cartridge dropwise at 5 mL/min, repeat. 6. Rinse bottle with 5 mL of 1:1 0.1 M formic acid:methanol and load onto SPE cartridge dropwise at 5 mL/min. 7. Flow nitrogen through cartridge for 15 minutes. 8. Rinse bottles with 5 mL of 1% ammonium hydroxide in methanol, elute into collection vessel. 9. Add 25 µL of concentrated acetic acid and 25 µL of Wellington MPFAC-HIF-IS. 10. Transfer aliquot to autosampler vial (cat. # 23243) and cap (cat. # 23244). |
| Notes | A PFAS delay column (cat.# 27854) was installed before the injector. |
Table I: Target recoveries (70-135%) were met for all PFAS in reagent water samples prepared using Resprep PFAS cartridges.
| Compound | Abbreviation | MDL (ng/L) | Blank (ng/L)* | Accuracy (%Recovery) | Precision (%RSD) |
|---|---|---|---|---|---|
| Perfluorobutanoic acid | PFBA | 0.34 | ND | 112 | 5 |
| Perfluoro-3-methoxypropanoic acid | PFMPA | 0.20 | ND | 109 | 6 |
| 3-Perfluoropropyl propanoic acid | 3:3FTCA | 0.31 | ND | 95 | 6 |
| Perfluoropentanoic acid | PFPeA | 0.26 | ND | 111 | 6 |
| Perfluorobutane sulfonate | PFBS | 0.19 | ND | 101 | 5 |
| Perfluoro-4-methoxybutanoic acid | PFMBA | 0.18 | ND | 111 | 6 |
| Perfluoro(2-ethoxyethane)sulfonic acid | PFEESA | 0.15 | ND | 94 | 5 |
| Nonafluoro-3,6-dioxaheptanoic acid | NFDHA | 0.46 | ND | 121 | 5 |
| 1H, 1H,2H,2H-perfluorohexane sulfonate | 4:2 FTS | 0.36 | ND | 104 | 5 |
| 2H,2H,3H,3H-Perfluorooctanoic acid | 5:3FTCA | 1.48 | ND | 102 | 6 |
| Perfluorohexanoic acid | PFHxA | 0.08 | ND | 113 | 5 |
| Perfluoropentane sulfonate | PFPeS | 0.07 | ND | 122 | 4 |
| Hexafluoropropylene oxide dimer acid | HFPO-DA | 0.40 | ND | 114 | 12 |
| Perfluoroheptanoic acid | PFHpA | 0.08 | ND | 109 | 5 |
| Perfluorohexane sulfonate | PFHxS | 0.07 | ND | 104 | 7 |
| 4,8-Dioxa-3H-perfluorononanoic acid | ADONA | 0.39 | ND | 99 | 9 |
| 1H,1H,2H,2H-perfluorooctane sulfonate | 6:2 FTS | 0.37 | ND | 107 | 4 |
| 3-Perfluoroheptyl propanoic acid | 7:3FTCA | 2.32 | ND | 100 | 6 |
| Perfluoroheptane sulfonate | PFHpS | 0.76 | ND | 121 | 8 |
| Perfluorooctanoic acid | PFOA | 0.32 | ND | 104 | 2 |
| Perfluorooctane sulfonate | PFOS | 0.20 | ND | 112 | 7 |
| Perfluorooctanesulfonamide | PFOSA | 0.21 | ND | 81 | 11 |
| Perfluorononanoic acid | PFNA | 0.08 | ND | 114 | 5 |
| N-methyl perfluorooctanesulfonamide | NMeFOSA | 0.07 | ND | 104 | 13 |
| 9-Chlorohexadecafluoro-3-oxanonane-1-sulfonic acid | 9Cl-PF3ONS | 0.61 | ND | 85 | 11 |
| Perfluorononanesulfonic acid | PFNS | 0.25 | ND | 79 | 7 |
| Perfluorodecanoic acid | PFDA | 0.18 | ND | 117 | 8 |
| N-ethyl perfluorooctanesulfonamide | NEtFOSA | 0.14 | ND | 112 | 15 |
| 1H,1H,2H,2H-perfluorodecane sulfonate | 8:2 FTS | 0.91 | ND | 113 | 11 |
| Perfluoroundecanoic acid | PFUnA | 0.26 | ND | 125 | 12 |
| N-methyl perfluorooctanesulfonamidoacetic acid | NMeFOSAA | 0.15 | ND | 95 | 12 |
| N-ethyl perfluorooctanesulfonamidoacetic acid | NEtFOSAA | 0.23 | ND | 93 | 12 |
| Perfluorodecanesulfonic acid | PFDS | 0.25 | ND | 94 | 23 |
| 11-Chloroeicosafluoro-3-oxaundecane-1-sulfonic acid | 11Cl-PF3OUdS | 0.56 | ND | 77 | 25 |
| Perfluorododecanoic acid | PFDoA | 0.27 | ND | 118 | 15 |
| N-methyl perfluorooctanesulfonamidoethanol | NMeFOSE | 1.11 | ND | 106 | 9 |
| N-ethyl perfluorooctanesulfonamidoethanol | NEtFOSE | 1.10 | ND | 111 | 9 |
| Perfluorotridecanoic acid | PFTrDA | 0.33 | ND | 108 | 15 |
| Perfluorododecanesulfonic acid | PFDoS | 0.13 | ND | 89 | 12 |
| Perfluorotetradecanoic acid | PFTeDA | 0.32 | ND | 102 | 23 |
*ND = Not detected above MDL.
Factory-Packed Filter Aid Option Ensures Faster, More Effective Sample Prep
Exclusive to Restek, Resprep PFAS cartridges are also available with a factory-packed filter aid that prevents clogs and keeps samples flowing better than manually packed glass wool. As shown in Table II, when technicians follow Method 1633 instructions to pack glass wool to half the height of the cartridge barrel for all sample matrices (Section 12.1.1), the amount of wool and packing density can vary significantly, which means sample flow and clogging can also be affected. The filter aid used in Resprep PFAS cartridges is uniform and provides effective, consistent filtering and protection. In an experiment comparing the flow of diluted ASTM wastewater matrix through Resprep PFAS cartridges with filter aid, WAX cartridges with manually packed wool, and WAX cartridges alone, only the Resprep PFAS cartridges with the factory-packed filter aid did not clog and were able to extract the full sample volume (Figure 2).
Table II: When cartridges are packed manually following the height-based instructions in Method 1633, the amount of glass wool and packing density can vary significantly between cartridges and technicians, which can affect method performance.
| Technician 1 | Technician 2 | Technician 3 | Technician 4 | |
|---|---|---|---|---|
| Average mg wool (n = 3) | 39 | 150 | 51 | 116 |
| SD | 2 | 13 | 7 | 49 |
| %RSD | 5% | 8% | 14% | 42% |
