Technical Information
Poly- and perfluoroalkyl substances (PFAS) have been widely used because they have various properties such as water repellency, heat resistance etc. However, they have been researched and regulated worldwide in recent years due to concern over their adverse health effects.
Recently, the highly sensitive and high-throughput method for the analysis of 28 PFAS in human serum was reported by Nakayama et al1). An automated solid phase extraction (SPE) coupled with the on-line SPE column-switching LC-MS/MS method using YMC-Triart C18 as analytical column was employed.
1. Perfluorobutanoic acid (PFBA)
2. Perfluoropentanoic acid (PFPA)
3. Perfluorohexanoic acid (PFHxA)
4. Perfluoroheptanoic acid (PFHpA)
5. Perfluorooctanoic acid (PFOA)
6. Perfluorononanoic acid (PFNA)
7. Perfluorodecanoic acid (PFDA)
8. Perfluoroundecanoic acid (PFUnA)
9. Perfluorododecanoic acid (PFDoA)
10. Perfluorotridecanoic acid (PFTrDA)
11. Perfluorotetradecanoic acid (PFTeDA)
12. Perfluorohexadecanoic acid (PFHxDA)
13. Perfluorooctadecanoic acid (PFODA)
14. Perfluorobutane sulphonic acid (PFBS)
15. Perfluorohexane sulphonic acid (PFHxS)
16. Perfluoroheptane sulphonic acid (PFHpS)
17. Perfluorooctane sulphonic acid (PFOS)
18. Perfluorodecane sulphonic acid (PFDS)
19. N -Methyl perfluorooctane sulphonamide (MeFOSA-M)
20. N -Ethyl perfluorooctane sulphonamide (EtFOSA-M)
21. N -Methyl perfluorooctane sulphonamido acetic acid (MeFOSA-A)
22. N -Ethyl perfluorooctane sulphonamido acetic acid (EtFOSA-A)
23. 4:2 Fluorotelomer sulphonic acid (4:2 FTS)
24. 6:2 Fluorotelomer sulphonic acid (6:2 FTS)
25. 8:2 Fluorotelomer sulphonic acid (8:2 FTS)
26. 6:2 Polyfluoroalkyl phosphoric acid diester (6:2 diPAP)
27. 8:2 Polyfluoroalkyl phosphoric acid diester (8:2 diPAP)
28. Perfluorooctane sulphonamido ethanol-based phosphate ester (diSAmPAP)
Neutral matrices (#19, 20) were analyzed using eluent with near neutral pH, and ionization matrices were analyzed by switching to alkaline eluent. YMC-Triart C18 have great durability and enable stable analysis even under alkaline condition.
| Column | YMC-Triart C18 (3 µm, 12 nm) [Guard column] 10 X 2.1 mmI.D. [Analytical column] 100 X 2.1 mmI.D. |
|---|---|
| Eluent | |
| LC Pump A | 2.5 mM ammonium acetate |
| LC Pump B1 | methanol |
| LC Pump B2 | 2.5 mM ammonium acetate in 95% methanol |
| LC Pump C | 0.1% ammonia in methanol |
| Temperature | 40°C |
|---|---|
| Detection | negative ESI |
| Injection | 400 µL |
| Sample | standard solution (4 ng/mL) |
| Sample load | |
| LC pump D1 | water |
| On-line SPE column wash | |
| LC pump D2 | 0.5% ammonia in 90% methanol |
| System | LCMS-8060 (Shimadzu Corporation) |
| Time (min) |
Ternary gradient | Flow rate | Binary gradient | Flow rate | Valve position | |||||||||
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
| Pump A
(%) |
Pump B1
(%) |
Pump B2
(%) |
Pump C
(%) |
Pump A+B+C (ml/min) |
Pump D1 (%) |
Pump D2 (%) |
Pump D (ml/min) |
Valve L | Valve R | |||||
| 0.00 | 12.5 | 87.5 | 0.0 | 0.0 | 0.3 | 100 |
0.0 | 1.0 | 1 | 0 | ||||
| 2.00 | 12.5 | 87.5 | 0.0 | 0.0 | 0.3 | 100 | 0.0 | 1.0 | 0 | 1 | ||||
| 2.01 | 12.5 | 87.5 | 0.0 | 0.0 | 0.3 | 0.0 | 0.0 | 0.0 | 0 | 1 | ||||
| 4.00 | 12.5 | 87.5 | 0.0 | 0.0 | 0.3 | 0.0 | 0.0 | 0.0 | 0 | 1 | ||||
| 5.50 | 12.5 | 87.5 | 0.0 | 0.0 | 0.3 | 0.0 | 0.0 | 0.0 | 1 | 0 | ||||
| 5.51 | 12.5 | 0.0 | 87.5 | 0.0 | 0.3 | 0.0 | 0.0 | 0.0 | 1 | 0 | ||||
| 7.00 | 12.5 | 0.0 | 87.5 | 0.0 | 0.3 | 0.0 | 0.0 | 0.0 | 1 | 0 | ||||
| 7.01 | 92.5 | 0.0 | 0.0 | 7.5 | 0.5 | 0.0 | 0.0 | 0.0 | 1 | 0 | ||||
| 7.50 | 92.5 | 0.0 | 0.0 | 7.5 | 0.5 | 0.0 | 0.0 | 0.0 | 0 | 1 | ||||
| 10.00 | 92.5 | 0.0 | 0.0 | 7.5 | 0.5 | 0.0 | 0.0 | 0.0 | 0 | 1 | ||||
| 10.01 | 92.5 | 0.0 | 0.0 | 7.5 | 0.3 | 0.0 | 0.0 | 0.0 | 0 | 1 | ||||
| 18.00 | 45 | 0.0 | 47.5 | 7.5 | 0.3 | 0.0 | 0.0 | 0.0 | 0 | 1 | ||||
| 20.00 | 27.5 | 0.0 | 65 | 7.5 | 0.3 | 0.0 | 0.0 | 0.0 | 1 | 0 | ||||
| 20.01 | *a | 0.0 | *a | 12.5 | 0.3 | 0.0 | 100 | 1.0 | 1 | 0 | ||||
| 24.00 | *a | 0.0 | *a | 12.5 | 0.3 | 0.0 | 100 | 1.0 | 1 | 0 | ||||
| 24.01 | *a | 0.0 | *a | 12.5 | 0.3 | 100 | 0.0 | 1.0 | 1 | 0 | ||||
| 25.00 | 0.0 | 0.0 | 87.5 | 12.5 | 0.3 | 100 | 0.0 | 1.0 | 1 | 0 | ||||
| 25.01 | 12.5 | 87.5 | 0.0 | 0.0 | 0.3 | 100 | 0.0 | 1.0 | 1 | 0 | ||||
| 27.00 | 12.5 | 87.5 | 0.0 | 0.0 | 0.3 | 100 | 0.0 | 1.0 | 1 | 0 | ||||
*a 20.00–25.00 min linear gradient (Pump A + Pump B2)
Courtesy of Dr. Shoji F. Nakayama, National Institute for Environmental Studies
Shoji F. Nakayama et al. Poly- and perfluoroalkyl substances in maternal serum: Method development and application in Pilot Study of the Japan Environment and Children’s Study, Journal of Chromatography A 1618 (2020) 460933
