- 单支柱管同时装填 WAX 和GCB填料，简化工作流程
- 出厂预装的助滤剂节省时间并防止堵塞
- 超纯净吸附剂确保达到方法检测限（Method Detection Limit, MDL），并保证分析结果的一致性
- 单支柱管同时装填 WAX 和GCB填料，简化工作流程
- 出厂预装的助滤剂节省时间并防止堵塞
- 超纯净吸附剂确保达到方法检测限（Method Detection Limit, MDL），并保证分析结果的一致性
使用双层 Resprep PFAS 小柱精简 PFAS 样品前处理
对于非饮用水、固体、生物固体和组织等复杂样品基质中的痕量全氟及多氟烷基物质（Per- and Polyfluoroalkyl Substances, PFAS）分析，有效的样品前处理至关重要。
通常采用固相萃取（Solid Phase Extraction, SPE），但如果存在背景 PFAS，或样品成分堵塞 SPE 柱管，则难以获得良好结果。
EPA 1633方法先采用填有玻璃毛的WAX小柱进行基质提取，随后通过GCB小柱进行净化。许多实验室正采用碳萃取柱替代 dGCB。
尽管该方法可行，但需要两支SPE小柱且需手动填装玻璃毛，两步操作不仅增加了额外的时间和操作复杂性，还增加了样品采集和前处理过程中含PFAS材料引起交叉污染的风险。
使用带助滤剂的 Resprep PFAS 小柱，简化您的样品前处理流程
Resprep PFAS 双层小柱是更简单的解决方案
采用双层填料的Resprep PFAS萃取小柱，可显著简化PFAS样品前处理流程。该萃取柱将WAX萃取和GCB净化合二为一，有助于降低污染风险。在此快速简便的工作流程中，小柱内装填的超洁净的WAX吸附剂和GCB吸附剂，可确保满足饮用水及其他样品中PFAS分析的方法性能要求。
此外，可选配的工厂预装助滤剂，省去了水样处理过程中手动填装玻璃毛的步骤，从而节省了时间并消除了操作差异性。这种即用型解决方案可有效防止堵塞，即使面对基质较脏的样品，也可通过单次萃取快速完成处理。
快速且一致地满足性能要求
Resprep PFAS双层小柱专为帮助实验室满足 PFAS 性能要求而开发，内含超纯净、高品质的 WAX 和GCB填料，可实现有效的萃取与净化。每一批 WAX 吸附剂均检测了EPA 1633方法中待测PFAS的空白值，以证明其洁净度并确保不引入背景 PFAS。此外，高性能的 GCB吸附剂较其他碳材料能提供更有效、更一致的净化。两种填料集成于单支SPE小柱，使样品前处理更为快速，并获得洁净的萃取液和优异的分析性能。
两种吸附剂合并在同一萃取柱中，可使 PFAS 样品制备速度大大加快。当与 LC-MS 或高分辨质谱联用进行数据分析时，可快速获得洁净的提取物和出色的分析结果（图 1 和表 I）。
图 1：Resprep PFAS 小柱可实现有效的 SPE 样品前处理，较分立的萃取与净化流程更快速、更易用
图 1：Resprep PFAS 小柱可实现有效的 SPE 样品前处理，较分立的萃取与净化流程更快速、更易用
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. |
表 I：使用 Resprep PFAS小柱制备的试剂水样品，所有 PFAS 均达到目标回收率（70-135%）
| 化合物 | 缩写 | MDL (ng/L) | 空白 (ng/L)* | 回收率 (%) | 精密度(%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 = 未检出（低于 MDL）。
出厂预装助滤剂选项确保样品前处理更快速、更有效
Resprep PFAS 小柱还提供 Restek 独有的出厂预装助滤剂版本，可防止堵塞，处理样品时比手动填装玻璃毛流动得更顺畅。
当技术人员按EPA 1633 的说明（第 12.1.1 节）将玻璃棉填装至柱管管身一半高度以适配所有样品基质时，玻璃棉的用量和填装密度可能存在显著差异，这意味着样品流速和堵塞情况也会随之受到影响。Resprep PFAS 小柱所用的助滤剂均匀一致，可提供有效且稳定的过滤与防护。
在一项比较稀释后的 ASTM 废水基质分别通过 Resprep PFAS带助滤剂小柱、手动填装玻璃棉的 WAX 小柱以及单纯 WAX 柱管的流动性实验中，只有出厂预装助滤剂的 Resprep PFAS 小柱未发生堵塞并能萃取全部样品体积（图 2）。
表 II：按EPA 1633 基于高度的说明手动填装柱管时，玻璃棉用量和填装密度在不同技术人员之间可能存在显著差异
| 技术人员 1 | 技术人员 2 | 技术人员 3 | 技术人员 4 | |
|---|---|---|---|---|
| 平均玻璃棉质量 mg（n = 3） | 39 | 150 | 51 | 116 |
| 标准偏差 (SD) | 2 | 13 | 7 | 49 |
| 相对标准偏差 (%RSD) | 5% | 8% | 14% | 42% |
图 2：只有出厂预装助滤剂的 Resprep PFAS 小柱成功萃取了全部 500 mL 经 2.5 倍稀释的 ASTM 废水基质（总悬浮固体 = 100 mg/L）
综上所述，采用带出厂预装助滤剂的 Resprep PFAS小柱，可显著简化样品前处理流程，节省操作时间、降低变异性并确保分析性能。
相关产品
Resprep PFAS SPE Cartridge with Filter Aid, 6 mL, Filter Aid 2000 mg/WAX 150 mg/GCB 50 mg, 30-pk.
您的PFAS分析需要帮助吗？
从方法选择到产品推荐，Restek PFAS 专家助您应对复杂分析流程，获得准确、可靠的分析结果。
