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有機フッ素化合物のポリおよびパーフルオロアルキル化合物（PFAS）は、撥水性や耐熱性など多様な特性を持つため、幅広い分野で使用されています。しかし、健康への悪影響が懸念され、近年世界的に調査・研究が行われ、規制も導入されています。
ここでは、Nakayamaらにより報告1)されているヒト血清中の28種類のPFASの高感度ハイスループット分析例を紹介します。自動固相抽出（SPE）カラムを組み込んだカラムスイッチングLC-MS/MSを用いたメソッドで、分析カラムとしてYMC-Triart C18が使用されています。
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)
中性付近のpHの移動相で中性化合物（ピーク19, 20）を分析したのち、アルカリ性の移動相に切り替えてイオン性の化合物を分析しています。Triart C18は耐久性に優れており、アルカリ性条件下でも安定した分析が可能です。
| 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
