全氟和多氟化合物(Per and Polyfluoroalkyl Substances, 简称PFAS),指含有至少一个完全氟化碳原子的全氟烷基和多氟烷基物质,是一种新型持久性有机污染物。
全氟化合物提前步骤:
(1)液体样品前处理方法:
乙腈提取:摇匀水样,量取250 mL水样于500 mL分液漏斗种,加入100ml乙腈,上下振摇5min,加人20 g氯化钠,振摇5 min,静置分层,取上清液,于40 ℃下旋蒸近干,用10ml 50%的甲醇水复溶,依次用6 mL氨水甲醇混合溶液、6 mL甲醇和6 mL水活化WAX 固相萃取柱,将提取的上清液以4 mL/min的流速 通过固相萃取柱后,依次用6 mL水和8 mL乙酸铵缓冲液淋洗固相萃取柱。最后用8mL甲醇以2mL/min的流速洗脱固相萃取柱,再用1mL氨水甲醇混合溶液洗脱固相萃取柱,收集洗脱液于离心管中。氮吹干后,用25ul甲醇-水(体积比为9∶1)复溶,过0.22 μm聚丙烯滤膜到100ul的玻璃内衬管中上机测定。
(2)固体样品前处理方法:
称取2.0 g左右样品放入50 mL离心管中, 50%甲醇水混合溶液10 mL,涡旋混合1 min,以 300 r/min常温振荡30 min后离心。上清液加水 40 mL后转移于另1支离心管中。依次用6 mL氨 水甲醇混合溶液、6 mL甲醇和6 mL水活化WAX 固相萃取柱,将提取的上清液以4 mL/min的流速 通过固相萃取柱后,依次用6 mL水和8 mL乙酸铵 缓冲液淋洗固相萃取柱。最后洗脱分2步,先用8mL甲醇以2mL/min的流速洗脱固相萃取柱,再 用1mL氨水甲醇混合溶液洗脱固相萃取柱,收集 洗脱液于离心管中。 将洗脱液浓缩至近干,用 50%甲醇水定容至1.0mL,混匀后经0.22 μm 针 头式过滤器过滤至进样瓶中。
仪器条件:
仪器条件:Agilent Eclipse Plus C18柱(100 mm×2.1 mm,1.8 μm,美国安捷伦科技有限公司);流动相:A相为水,B相为含0.01%甲酸的甲醇溶液;流量:0.3mL/min;洗脱方式:梯度洗脱,
洗脱程序见表1;
柱温:35 ℃;
进样体积:5 μL
离子源:电喷雾离子源(AJS-ESI);扫描方式:负离子扫描;毛细管电压:-2.5 kV;脱溶剂气温度:350 ℃;鞘气流量:40 L/min;离子源温度:350 ℃;扫描模式:多反应监测(MRM)模式.
|
时间 |
A(水) |
B(甲醇+0.01甲酸%) |
|
0 |
95 |
5 |
|
2 |
70 |
30 |
|
3 |
40 |
60 |
|
5 |
5 |
95 |
|
6 |
5 |
95 |
|
6.2 |
95 |
5 |
|
7 |
95 |
5 |
离子对信息:
|
英文缩写 |
母离子 |
子离子 |
毛细管电压 |
碰撞能量 |
极性 |
检出限ng/L |
|
PFHxDA |
813 |
768.9 |
70 |
20 |
Negative |
0.01 |
|
PFHxDA |
813 |
168.9 |
70 |
35 |
Negative |
|
|
PFTeDA |
712.9 |
668.9 |
15 |
12 |
Negative |
0.05 |
|
PFTeDA |
712.9 |
168.9 |
15 |
28 |
Negative |
|
|
PFTrDA |
662.9 |
618.9 |
15 |
12 |
Negative |
0.1 |
|
PFTrDA |
662.9 |
168.8 |
15 |
28 |
Negative |
|
|
11Cl-PF3OUdS |
630.9 |
450.8 |
15 |
30 |
Negative |
0.1 |
|
11Cl-PF3OUdS |
630.9 |
82.9 |
15 |
36 |
Negative |
|
|
PFDoA |
612.9 |
568.9 |
15 |
10 |
Negative |
0.1 |
|
PFDoA |
612.9 |
168.8 |
15 |
26 |
Negative |
|
|
PFDS |
598.9 |
98.8 |
10 |
45 |
Negative |
0.1 |
|
PFDS |
598.9 |
79.9 |
10 |
52 |
Negative |
|
|
N-EtPFOSAA |
583.9 |
525.8 |
15 |
18 |
Negative |
0.1 |
|
N-EtPFOSAA |
583.9 |
418.8 |
15 |
18 |
Negative |
|
|
NMeFOSAA |
570.1 |
482.8 |
15 |
14 |
Negative |
0.1 |
|
NMeFOSAA |
570.1 |
418.8 |
15 |
18 |
Negative |
|
|
PFUnA |
562.9 |
518.8 |
15 |
10 |
Negative |
0.1 |
|
PFUnA |
562.9 |
268.9 |
15 |
18 |
Negative |
|
|
9Cl-PF3ONS |
530.9 |
350.8 |
15 |
26 |
Negative |
0.1 |
|
9Cl-PF3ONS |
530.9 |
82.9 |
15 |
30 |
Negative |
|
|
M6PFDA |
512.9 |
468.9 |
10 |
8 |
Negative |
0.1 |
|
M6PFDA |
512.9 |
218.9 |
10 |
16 |
Negative |
|
|
PFOS |
498.9 |
98.8 |
15 |
40 |
Negative |
0.01 |
|
PFOS |
498.9 |
79.9 |
15 |
43 |
Negative |
|
|
PFOSA |
497.9 |
168.9 |
10 |
28 |
Negative |
0.01 |
|
PFOSA |
497.9 |
77.9 |
10 |
34 |
Negative |
|
|
PFNA |
462.9 |
418.9 |
15 |
8 |
Negative |
0.01 |
|
PFNA |
462.9 |
218.9 |
15 |
14 |
Negative |
|
|
6:2 FTS |
426.9 |
406.9 |
15 |
24 |
Negative |
0.01 |
|
6:2 FTS |
426.9 |
81 |
15 |
35 |
Negative |
|
|
PFOA |
412.9 |
368.9 |
15 |
8 |
Negative |
0.01 |
|
PFOA |
412.9 |
168.9 |
15 |
16 |
Negative |
|
|
PFHxS |
398.9 |
98.8 |
15 |
35 |
Negative |
0.02 |
|
PFHxS |
398.9 |
79.9 |
15 |
35 |
Negative |
|
|
6:2 FTCA |
376.9 |
312.9 |
10 |
4 |
Negative |
0.005 |
|
6:2 FTCA |
376.9 |
292.9 |
10 |
12 |
Negative |
|
|
PFHpA |
362.8 |
318.9 |
15 |
8 |
Negative |
0.005 |
|
PFHpA |
362.8 |
168.9 |
15 |
16 |
Negative |
|
|
GenX |
328.9 |
168.9 |
20 |
20 |
Negative |
0.01 |
|
GenX |
328.9 |
84.9 |
20 |
30 |
Negative |
|
|
PFHxA |
312.9 |
268.9 |
12 |
10 |
Negative |
0.01 |
|
PFHxA |
312.9 |
118.9 |
12 |
18 |
Negative |
|
|
PFBS |
298.9 |
98.8 |
4 |
25 |
Negative |
0.01 |
|
PFBS |
298.9 |
79.9 |
4 |
30 |
Negative |
|
|
FBSA |
297.8 |
119 |
10 |
18 |
Negative |
0.01 |
|
FBSA |
297.8 |
77.9 |
10 |
22 |
Negative |
|
|
HFPODA |
284.9 |
184.8 |
10 |
16 |
Negative |
0.01 |
|
HFPODA |
284.9 |
168.8 |
10 |
6 |
Negative |
|
|
PFPeA |
262.9 |
218.9 |
15 |
6 |
Negative |
0.003 |
|
PFPeA |
262.9 |
68.9 |
15 |
40 |
Negative |
|
|
PFBA |
212.9 |
171.9 |
20 |
8 |
Negative |
2 |
|
PFBA |
212.9 |
168.9 |
20 |
8 |
Negative |
全氟化合物检测指标:
| 名称 | 缩写 | 分子量 | 分子式 | CAS 号 |
| Perfluorobutanoic acid | PFBA | 214.04 | C4HF7O2 | 375-22-4 |
| Perfluoropentanoic acid | PFPeA | 264.05 | C5HF9O2 | 2706-90-3 |
| Perfluorohexanoic acid | PFHxA | 314.05 | C6HF11O2 | 307-24-4 |
| Perfluoroheptanoic acid | PFHpA | 364.06 | C7HF13O2 | 375-85-9 |
| Perfluorooctanoic acid | PFOA | 414.07 | C8HF15O2 | 335-67-1 |
| Perfluorononanoic acid | PFNA | 464.08 | C9HF17O2 | 375-95-1 |
| Perfluorodecanoic acid | PFDA | 514.08 | C10HF19O2 | 335-76-2 |
| Perfluoroundecanoic acid | PFUnDA | 564.09 | C11HF21O2 | 2058-94-8 |
| Perfluorododecanoic acid | PFDoDA | 614.10 | C12HF23O2 | 307-55-1 |
| Perfluorotridecanoic acid | PFTrDA | 664.10 | C13HF25O2 | 72629-94-8 |
| Perfluorotetradecanoic acid | PFTeDA | 714.11 | C14HF27O2 | 376-06-7 |
| Perfluorohexadecanoic acid | PFHxDA | 814.13 | C16HF31O2 | 67905-19-5 |
| Perfluorooctadecanoic acid | PFODA | 914.10 | C18HF35O2 | 16517-11-6 |
| Perfluorobutane sulfonic acid | PFBS | 300.1 | C4HF9O3S | 375-73-5 |
| Perfluoropentane sulfonic acid | PFPeS | 350.11 | C5HF11O3S | 2706-91-4 |
| Perfluorohexane sulfonic acid | PFHxS | 400.12 | C6HF13O3S | 355-46-4 |
| Perfluoroheptane sulfonic acid | PFHpS | 450.12 | C7HF15O3S | 375-92-8 |
| Perfluorooctanesulfonic acid | PFOS | 500.13 | C8HF17O3S | 1763-23-1 |
| Perfluorononane sulfonic acid | PFNS | 550.14 | C9HF19O3S | 68259-12-1 |
| Perfluorodecane sulfonic acid | PFDS | 600.15 | C10HF21O3S | 335-77-3 |
| Perfluorododecane sulfonic acid | PFDoS | 700.16 | C12HF25O3S | 79780-39-5 |
| 6:2 Fluorotelomer carboxylic acid | FHEA | 378.09 | C8H3F13O2 | 53826-12-3 |
| 8:2 Fluorotelomer carboxylic acid | FOEA | 478.10 | C10H3F17O2 | 27854-31-5 |
| 10:2 Fluorotelomer carboxylic acid | FDEA | 578.12 | C12H3F21O2 | 53826-13-4 |
| 3:3 Fluorotelomer carboxylic acid | FPrPA | 242.09 | C6H5F7O2 | 356-02-5 |
| 5:3 Fluorotelomer carboxylic acid | FPePA | 342.11 | C8H5F11O2 | 914637-49-3 |
| 7:3 Fluorotelomer carboxylic acid | FHpPA | 442.12 | C10H5F15O2 | 812-70-4 |
| 6:2 Fluorotelomer unsaturatedcarboxylic acid | FHUEA | 358.08 | C8H2F12O2 | 70887-88-6 |
| 8:2 Fluorotelomer unsaturatedcarboxylic acid | FOUEA | 458.1 | C10H2F16O2 | 70887-84-2 |
| 10:2 Fluorotelomer unsaturatedcarboxylic acid | FDUEA | 558.11 | C12H2F20O2 | 70887-94-4 |
| 4:2 Fluorotelomer sulfonic acid | 4:2FTS | 328.15 | C6H5F9O3S | 757124-72-4 |
| 6:2 Fluorotelomer sulfonic acid | 6:2FTS | 428.17 | C8H5F13O3S | 27619-97-2 |
| 8:2 Fluorotelomer sulfonic acid | 8:2FTS | 528.18 | C10H5F17O3S | 39108-34-4 |
| 10:2 Fluorotelomer sulfonic acid | 10:2FTS | 628.2 | C12H5F21O3S | 120226-60-0 |
| Perfluorohexyl phosphonic acid | PFHxPA | 400.03 | C6H2F13O3P | 40143-76-8 |
| Perfluorooctyl phosphonic acid | PFOPA | 500.05 | C8H2F17O3P | 40143-78-0 |
| Perfluorodecyl phosphonic acid | PFDPA | 600.06 | C10H2F21O3P | 52299-26-0 |
| 6:2 Fluorotelomer phosphate diester | 6:2diPAP | 790.17 | C16H9F26O4P | 57677-95-9 |
| 6:2/8:2 Fluorotelomer phosphate diester | 6:2/8:2diPAP | 890.2 | C18H9F30O4P | 943913-15-3 |
| 8:2 Fluorotelomer phosphate diester | 8:2diPAP | 990.2 | C20H9F34O4P | 678-41-1 |
| 6:6 Perfluorophosphinic acid | 6:6PFPiA | 702.07 | C12HF26O2P | 40143-77-9 |
| 8:8 Perfluorophosphinic acid | 8:8PFPiA | 902.1 | C16HF34O2P | 40143-79-1 |
| Perfluorooctane sulfonamido-ethanol-based phosphate diester | diSAmPAP | 1204.5 | C24H19F34N2O8PS2 | 2965-52-8 |
| Perfluorooctansulfonamide | FOSA | 499.15 | C8H2F17NO2S | 754-91-6 |
| N-Methyl perfluorooctane sulfonamide | N-MeFOSA-M | 513.17 | C9H4F17NO2S | 31506-32-8 |
| N-Ethyl perfluorooctane sulfonamide | N-EtFOSA-M | 527.2 | C10H6F17NO2S | 4151-50-2 |
| Perfluorooctane sulfonamido acetic acid | FOSAA | 557.18 | C10H4F17NO4S | 2806-24-8 |
| N-Methyl perfluorooctane sulfonamido acetic acid | N-MeFOSAA | 571.21 | C11H6F17NO4S | 2355-31-9 |
| N-Ethyl perfluorooctane sulfonamidoacetic acid | N-EtFOSAA | 585.24 | C12H8F17NO4S | 2991-50-6 |
| N-Methyl perfluorooctane sulfonamido ethanol | N-MeFOSE-M | 557.23 | C11H8F17NO3S | 24448-09-7 |
| N-Ethyl perfluorooctane sulfonamido ethanol | N-EtFOSE-M | 571.25 | C12H10F17NO3S | 1691-99-2 |
| ADONA | NaDONA | 378.07 | C7H2F12O4 | 919005-14-4 |
| 6:2 Chlorinated perfluoroether sulfonic acid (F-53B)** | 9Cl-PF3ONS | 532.58 | C8HClF16O4S | 756426-58-1 |
| 8:2 Chlorinated perfluoroethersulfonic acid** | 11Cl-PF3OUdS | 632.6 | C10HClF20O4S | 763051-92-9 |
| Perfluoro-4-ethylcyclohexanesulphonic acid potassium salt | PFECHS | 462.13 | C8HF15O3S | 1135682-88-0 |
| HFPO-DA (GenX) | 330.05 | C6HF11O3 | 13252-13-6 | |
| HFPO-TA | 496.07 | C9HF17O4 | 13252-14-7 |

行业分类标准号标准名称
环境ISO 21675-2019 《水质全氟及多氟化合物的测定固相萃取-液相色谱/质谱法》
EPA 533-2019 《饮用水中的全氟和多氟烷基物质的测定同位素稀释阴离子交换固相萃取-液相色谱/串联质谱法》
ASTM D7979-2019 《用液相色谱-串联质谱法测定水、污泥、进水、出水和废水中全氟化合物的标准试验方法》
EPA537.1-2020 《固相萃取-液相色谱/串联质谱法测定饮用水中的多氟烷基物质》
DB32/T 4004-2021 《水质 17种全氟化合物的测定高效液相色谱串联质谱法》
ASTM D7968 《用液相色谱串联质谱法(LC/ MS/MS)测定土壤中多氟化合物的标准试验方法》
DIN 38414-14:2011 德国检验水,废水和污泥的标准方法.污泥和沉淀物(第5组)-第14部分:污泥,堆肥和土壤中选定全氟化合物(PFC)的测定.使用高性能液相色谱法的方法
食品安全GB 5009.253-2016 食品安全国家标准 动物源性食品中全氟辛烷磺酸(PFOS)和全氟辛酸(PFOA)的测定
GB 31604.35-2016 食品安全国家标准 食品接触材料及制品 全氟辛烷磺酸(PFOS)和全氟辛酸(PFOA)的测定
GB 31604.35-2016 生活饮用水标准检验方法:第8部分:有机物指标
工业制造GB/T 31126-2014 纺织品 全氟辛烷磺酰基化合物和全氟羧酸的定
GB/T 37760-2019 电子电气产品中全氟辛酸和全氟辛烷磺酸的测定 超高效液相色谱串联质谱法
SN/T 5352-2021 纸制耐热材料中全氟和多氟化合物的测定








