全自动在线检测尿液中的全氟及多氟化合物
表1. PFASs的检测参数(加粗代表定量离子)
化合物 | 母离子 (m/z) | 子离子(m/z) | 碰撞能(V) | RF Lens (V) | 内标物 |
FTSAs | |||||
4:2 FTSA | 327 | 81,307 | 29 | 82 | 13C2-4:2 FTSA |
6:2 FTSA | 427 | 81,407 | 24 | 91 | 13C2-6:2 FTSA |
8:2 FTSA | 527 | 81,507 | 26 | 113 | 13C2-8:2 FTSA |
10:2 FTSA | 627 | 81,607 | 30 | 141 | 13C2-8:2 FTSA |
monoPAPs | |||||
6:2 monoPAP | 443 | 79,97 | 41 | 61 | 13C2-6:2 monoPAP |
8:2 monoPAP | 543 | 79,97 | 38 | 73 | 13C2-8:2 monoPAP |
diPAPs | |||||
6:2 diPAP | 789 | 97,443 | 39 | 102 | 13C4-6:2 diPAP |
6:2/8:2 diPAP | 889 | 443,543 | 21 | 168 | 13C4-6:2 diPAP |
8:2 diPAP | 989 | 97,543 | 40 | 126 | 13C4-8:2 diPAP |
PFPAs | |||||
PFHxPA | 399 | 79,97 | 32 | 91 | Cl-PFHxPA |
PFOPA | 499 | 79,97 | 36 | 150 | Cl-PFOPA |
PFPiAs | |||||
6:6PFPiA | 701 | 401,501 | 50 | 195 | 13C4-6:2 diPAP |
6:6/8:8 PFPiA | 801 | 401,501 | 55 | 232 | 13C4-6:2 diPAP |
8:8 PFPiA | 901 | 401,501 | 43 | 232 | 13C4-6:2 diPAP |
FOSAs | |||||
FOSA | 498 | 78,169 | 42 | 160 | |
N-MeFOSA | 512 | 169,219 | 24 | 97 | d3- N-MeFOSA |
N-EtFOSA | 526 | 169,269 | 27 | 105 | d-N-EtFOSA |
FOSAAs | |||||
FOSAA | 559 | 419,483 | 30 | 83 | d3-N-MeFOSAA |
N-MeFOSAA | 570 | 419,483 | 25 | 80 | d3-N-MeFOSAA |
N-EtFOSAA | 584 | 419,483 | 27 | 78 | d5-N-EtFOSAA |
Cl-PFESA |
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6:2 Cl-PFESA | 531 | 83,351 | 26 | 112 | 13C2-PFOS |
8:2 Cl-PFESA | 631 | 351,451 | 28 | 164 | 13C2-PFOS |
PFCAs | |||||
PFBA | 213 | 119,169 | 8 | 30 | 13C4-PFBA |
PFPeA | 263 | 119,219 | 10 | 30 | 13C4-PFPeA |
PFHxA | 313 | 219,269 | 5 | 30 | 13C2-PFHxA |
PFHpA | 363 | 269,319 | 10 | 47 | 13C2-PFHpA |
PFOA | 413 | 269,369 | 8 | 39 | 13C4-PFOA |
PFNA | 463 | 369,419 | 18 | 44 | 13C5-PFNA |
PFDA | 513 | 319,469 | 17 | 40 | 13C2-PFDA |
PFUnA | 563 | 469,519 | 16 | 52 | 13C2-PFUnA |
PFDoA | 613 | 519,569 | 10 | 53 | 13C2-PFDoA |
PFTrDA | 663 | 569,619 | 11 | 61 | 13C2-PFDoA |
PFTeDA | 713 | 619,669 | 13 | 71 | 13C2-PFDoA |
PFHxDA | 813 | 719,769 | 13 | 70 | 13C2-PFDoA |
PFODA | 913 | 819,869 | 13 | 67 | 13C2-PFDoA |
PFSAs | |||||
PFBS | 299 | 80,99 | 33 | 113 | 13C2-PFBS |
PFPeS | 349 | 80,99 | 26 | 124 | 13C2-PFBS |
PFHxS | 399 | 80,99,119 | 39 | 141 | 18O2-PFHxS |
PFHpS | 449 | 80,99 | 42 | 156 | 13C2-PFOS |
PFOS | 499 | 80,99,130 | 48 | 169 | 13C2-PFOS |
PFNS | 549 | 80,99 | 42 | 249 | 13C2-PFOS |
PFDS | 599 | 80,99 | 48 | 215 | 13C2-PFOS |
PFDoS | 699 | 80,99 | 55 | 256 | 13C2-PFOS |
内标物 |
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13C4-PFBA | 217 | 172 | 8 | 30 |
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13C4-PFPeA | 266 | 222 | 5 | 30 |
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13C2-PFHxA | 315 | 270 | 10 | 30 |
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13C2-PFHpA | 367 | 322 | 24 | 47 |
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13C4-PFOA | 417 | 372 | 7 | 39 |
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13C5-PFNA | 468 | 219 | 16 | 45 |
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13C2-PFDA | 515 | 470 | 17 | 40 |
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13C2-PFUnA | 565 | 520 | 10 | 53 | |
13C2-PFDoA | 615 | 570 | 10 | 53 | |
13C2-PFBS | 302 | 80,99 | 31 | 113 | |
18O2-PFHxS | 403 | 103 | 36 | 111 | |
13C2-PFOS | 503 | 80,99 | 49 | 188 | |
13C8-PFOS | 503 | 80,99 | 49 | 188 | |
13C2-4:2FTSA | 329 | 81,309 | 29 | 76 | |
13C2-6:2FTSA | 429 | 81,409 | 23 | 109 | |
13C2-8:2FTSA | 529 | 81,509 | 26 | 102 | |
13C8-FOSA | 506 | 78 | 42 | 160 |
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d-N-MeFOSA | 515 | 219 | 25 | 110 |
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d-N-EtFOSA | 531 | 419 | 20 | 104 |
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d3-N-MeFOSAA | 573 | 419 | 19 | 101 |
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d5-N-EtFOSAA | 589 | 419 | 20 | 78 |
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13C2-6:2 monoPAP | 445 | 97 | 16 | 70 | |
13C2-8:2 monoPAP | 545 | 97 | 18 | 73 | |
13C4-6:2 diPAP | 793 | 445 | 30 | 114 | |
13C4-8:2 diPAP | 993 | 545 | 21 | 134 | |
Cl-PFHxPA | 415 | 79 | 32 | 103 | |
Cl-PFOPA | 515 | 79 | 35 | 101 |
图1在线湍流固相萃取-液相色谱-质谱联用系统示意图
时间 (min) | 左泵 | 时间(min) | 右泵 | 阀位置 | ||||||
流速 | %A | %B | %C | 流速 | %A | %B | %C | |||
(mL min-1) | (mL min-1) | |||||||||
0 | 2 | 100 | 0 | 0 | 0 | 0.4 | 90 | 10 | 1-2 a | |
3 | 2 | 100 | 0 | 0 | 1 | 0.4 | 90 | 10 | 6-1b | |
3.5 | 1 | 0 | 0 | 100 | 2 | 0.4 | 90 | 10 | 6-1 | |
6 | 1 | 0 | 0 | 100 | 3 | 0.4 | 55 | 45 | 6-1 | |
9 | 1 | 0 | 0 | 100 | 6 | 0.4 | 23 | 77 | 1-2 c | |
9.5 | 1 | 0 | 100 | 0 | 12 | 0.4 | 0 | 95 | 5 | 1-2 |
15 | 1 | 0 | 100 | 0 | 15 | 0.4 | 0 | 95 | 5 | 1-2 |
15.5 | 2 | 100 | 0 | 0 | 15.2 | 0.4 | 90 | 10 | 1-2 | |
19 | 2 | 100 | 0 | 0 | 19 | 0.4 | 90 | 10 | 1-2 |
图2在线检测43种PFASs的色谱图