Chinese Journal of Chromatography ›› 2021, Vol. 39 ›› Issue (11): 1239-1246.DOI: 10.3724/SP.J.1123.2021.01043
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WANG Chunlan1,*(), ZHANG Haixuan1, ZHU Li2, HU Wangxia1, LIN Ziwei1
Received:
2021-01-27
Online:
2021-11-08
Published:
2021-06-17
Contact:
WANG Chunlan
CLC Number:
WANG Chunlan, ZHANG Haixuan, ZHU Li, HU Wangxia, LIN Ziwei. Simultaneous determination of 11 volatile perfluorinated compound precursors in textiles using gas chromatography-triple quadrupole mass spectrometry[J]. Chinese Journal of Chromatography, 2021, 39(11): 1239-1246.
Fig. 1 Chemical structures of the 11 perfluorinated compound precursors 4:2FTOH: 1H,1H,2H,2H-perfluoro-1-hexanol; 6:2FTOH: 1H,1H,2H,2H-perfluoro-1-octanol; 6:2FTA: 1H,1H,2H,2H-perfluorooctyl acrylate; 8:2FTOH: 1H,1H,2H,2H-perfluoro-1-decanol; 8:2FTA: 1H,1H,2H,2H-perfluorodecyl acrylate; 10:2FTOH: 1H,1H,2H,2H-perfluoro-1-dodecanol; 10:2FTA: 1H,1H,2H,2H-perfluorododecyl acrylate; N-Me-FOSA: N-methyl-perfluorooctane sulfonamide; N-Me-FOSE: N-methyl-perfluorooctane sulfonamide ethanol; N-Et-FOSA: N-ethyl-perfluorooctane sulfonamide; N-Et-FOSE: N-ethyl-perfluorooctane sulfonamide ethanol.
Compound | CAS No. | t/ min | MRM ion pairs (m/z) | CEs/ eV | |
---|---|---|---|---|---|
6:2FTA | 17527-29-6 | 7.31 | 55.0>27.0*; | 418.1>99.0 | 25;42 |
4:2FTOH | 2043-47-2 | 8.05 | 95.0>69.0*; | 196.1>127.0 | 25;18 |
8:2FTA | 27905-45-9 | 8.87 | 55.0>27.0*; | 518.1>99.0 | 18;48 |
6:2FTOH | 647-42-7 | 9.01 | 95.0>69.0*; | 296.1>127.0 | 25;35 |
8:2FTOH | 678-39-7 | 10.18 | 95.0>69.0*; | 131.0>68.9 | 28;46 |
10:2FTA | 17741-60-5 | 10.76 | 55.0>27.0*; | 618.0>99.1 | 20;58 |
10:2FTOH | 865-86-1 | 11.35 | 95.0>69.0*; | 131.0>68.9 | 30;42 |
N-Et-FOSA | 4151-50-2 | 15.75 | 108.0>80.0*; | 131.0>68.9 | 10;44 |
N-Me-FOSA | 31506-32-8 | 16.23 | 94.0>30.0*; | 131.0>68.9 | 22;48 |
N-Me-FOSE | 24448-09-7 | 17.30 | 526.0>462.0*; | 131.0>68.9 | 52;39 |
N-Et-FOSE | 1691-99-2 | 17.36 | 540.0>169.0*; | 131.0>68.9 | 41;39 |
Table 1 Retention times, monitoring ion pairs, and collision energies of the 11 perfluorinated compound precursors
Compound | CAS No. | t/ min | MRM ion pairs (m/z) | CEs/ eV | |
---|---|---|---|---|---|
6:2FTA | 17527-29-6 | 7.31 | 55.0>27.0*; | 418.1>99.0 | 25;42 |
4:2FTOH | 2043-47-2 | 8.05 | 95.0>69.0*; | 196.1>127.0 | 25;18 |
8:2FTA | 27905-45-9 | 8.87 | 55.0>27.0*; | 518.1>99.0 | 18;48 |
6:2FTOH | 647-42-7 | 9.01 | 95.0>69.0*; | 296.1>127.0 | 25;35 |
8:2FTOH | 678-39-7 | 10.18 | 95.0>69.0*; | 131.0>68.9 | 28;46 |
10:2FTA | 17741-60-5 | 10.76 | 55.0>27.0*; | 618.0>99.1 | 20;58 |
10:2FTOH | 865-86-1 | 11.35 | 95.0>69.0*; | 131.0>68.9 | 30;42 |
N-Et-FOSA | 4151-50-2 | 15.75 | 108.0>80.0*; | 131.0>68.9 | 10;44 |
N-Me-FOSA | 31506-32-8 | 16.23 | 94.0>30.0*; | 131.0>68.9 | 22;48 |
N-Me-FOSE | 24448-09-7 | 17.30 | 526.0>462.0*; | 131.0>68.9 | 52;39 |
N-Et-FOSE | 1691-99-2 | 17.36 | 540.0>169.0*; | 131.0>68.9 | 41;39 |
Compound | Regression equation | r | LOD/ (mg/kg) | LOQ/ (mg/kg) |
---|---|---|---|---|
6:2FTA | Y=1514X-7845 | 0.9996 | 0.02 | 0.06 |
4:2FTOH | Y=632.5X-3116 | 0.9992 | 0.01 | 0.04 |
8:2FTA | Y=1062X-3652 | 0.9991 | 0.03 | 0.01 |
6:2FTOH | Y=812.3X-4550 | 0.9991 | 0.01 | 0.03 |
8:2FTOH | Y=740.1X-1409 | 0.9987 | 0.002 | 0.006 |
10:2FTA | Y=833.2X-5348 | 0.9989 | 0.04 | 0.1 |
10:2FTOH | Y=642X-3177 | 0.9987 | 0.002 | 0.006 |
N-Et-FOSA | Y=1923X-12060 | 0.9986 | 0.004 | 0.01 |
N-Me-FOSA | Y=1179X-6168 | 0.9990 | 0.002 | 0.006 |
N-Me-FOSE | Y=2493X-17390 | 0.9987 | 0.003 | 0.01 |
N-Et-FOSE | Y=1557X-12250 | 0.9984 | 0.005 | 0.02 |
Table 2 Regression equations, correlation coefficients (r), limits of detection (LODs), and limits of quantification (LOQs) of the 11 perfluorinated compound precursors
Compound | Regression equation | r | LOD/ (mg/kg) | LOQ/ (mg/kg) |
---|---|---|---|---|
6:2FTA | Y=1514X-7845 | 0.9996 | 0.02 | 0.06 |
4:2FTOH | Y=632.5X-3116 | 0.9992 | 0.01 | 0.04 |
8:2FTA | Y=1062X-3652 | 0.9991 | 0.03 | 0.01 |
6:2FTOH | Y=812.3X-4550 | 0.9991 | 0.01 | 0.03 |
8:2FTOH | Y=740.1X-1409 | 0.9987 | 0.002 | 0.006 |
10:2FTA | Y=833.2X-5348 | 0.9989 | 0.04 | 0.1 |
10:2FTOH | Y=642X-3177 | 0.9987 | 0.002 | 0.006 |
N-Et-FOSA | Y=1923X-12060 | 0.9986 | 0.004 | 0.01 |
N-Me-FOSA | Y=1179X-6168 | 0.9990 | 0.002 | 0.006 |
N-Me-FOSE | Y=2493X-17390 | 0.9987 | 0.003 | 0.01 |
N-Et-FOSE | Y=1557X-12250 | 0.9984 | 0.005 | 0.02 |
Compound | Recoveries/% (RSDs/%) | |||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|
Cotton fabric | Synthetic fabric | Synthetic leather | ||||||||||
0.2 μg | 1 μg | 8 μg | 0.2 μg | 1 μg | 8 μg | 0.2 μg | 1 μg | 8 μg | ||||
6:2FTA | 85.2 (8.3) | 78.4 (6.3) | 77.3 (5.4) | 99.6 (6.2) | 80.7 (6.4) | 75.5 (6.2) | 81.7 (4.5) | 75.8 (6.7) | 87.3 (9.3) | |||
4:2FTOH | 99.8 (5.2) | 99.8 (3.8) | 112.6 (8.4) | 98.1 (5.6) | 96.0 (1.3) | 95.2 (2.0) | 93.7 (7.4) | 90.7 (1.6) | 94.4 (6.0) | |||
8:2FTA | 114.0 (3.5) | 115.2 (1.2) | 114.6 (6.4) | 108.3 (7.0) | 115.3 (9.1) | 105.9 (3.2) | 73.2 (5.4) | 81.5 (1.7) | 76.0 (5.2) | |||
6:2FTOH | 105.2 (3.5) | 99.6 (2.5) | 103.3 (1.5) | 100.7 (1.4) | 95.7 (2.4) | 93.2 (1.3) | 100.6 (1.7) | 117.2 (9.2) | 101.0 (2.0) | |||
8:2FTOH | 106.5 (2.1) | 94.4 (5.8) | 105.4 (3.6) | 111.7 (4.3) | 90.6 (4.6) | 93.5 (2.1) | 92.5 (4.4) | 95.4 (4.2) | 101.3 (5.0) | |||
10:2FTA | 99.7 (3.8) | 97.3 (3.7) | 102.6 (5.9) | 101.8 (3.8) | 100.9 (4.1) | 101.3 (3.3) | 95.6 (2.5) | 98.6 (3.0) | 98.0 (5.2) | |||
10:2FTOH | 116.2 (4.0) | 96.3 (6.5) | 100.1 (4.0) | 99.1 (0.1) | 90.8 (5.4) | 90.4 (3.5) | 78.8 (4.1) | 86.5 (3.7) | 99.3 (5.4) | |||
N-Et-FOSA | 92.8 (7.8) | 84.7 (6.3) | 91.0 (8.7) | 95.3 (7.0) | 81.3 (5.6) | 90.2 (3.4) | 105.9 (8.2) | 92.5 (7.3) | 98.5 (1.0) | |||
N-Me-FOSA | 94.5 (7.4) | 80.5 (6.3) | 87.4 (6.2) | 86.6 (9.0) | 79.4 (5.9) | 91.7 (4.8) | 96.4 (7.0) | 90.3 (4.7) | 101.9 (2.6) | |||
N-Me-FOSE | 114.6 (3.3) | 102.5 (7.7) | 104.8 (7.9) | 95.1 (8.5) | 93.0 (7.6) | 99.6 (8.9) | 110.1 (6.3) | 94.5 (9.2) | 100.5 (9.4) | |||
N-Et-FOSE | 103.6 (6.5) | 102.3 (8.3) | 105.9 (9.1) | 100.5 (5.5) | 97.4 (9.2) | 98.7 (8.9) | 107.4 (8.7) | 97.8 (4.2) | 101.8 (5.8) |
Table 3 Recoveries and relative standard deviations of the 11 perfluorinated compound precursors spiked in the three textile samples (n=6)
Compound | Recoveries/% (RSDs/%) | |||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|
Cotton fabric | Synthetic fabric | Synthetic leather | ||||||||||
0.2 μg | 1 μg | 8 μg | 0.2 μg | 1 μg | 8 μg | 0.2 μg | 1 μg | 8 μg | ||||
6:2FTA | 85.2 (8.3) | 78.4 (6.3) | 77.3 (5.4) | 99.6 (6.2) | 80.7 (6.4) | 75.5 (6.2) | 81.7 (4.5) | 75.8 (6.7) | 87.3 (9.3) | |||
4:2FTOH | 99.8 (5.2) | 99.8 (3.8) | 112.6 (8.4) | 98.1 (5.6) | 96.0 (1.3) | 95.2 (2.0) | 93.7 (7.4) | 90.7 (1.6) | 94.4 (6.0) | |||
8:2FTA | 114.0 (3.5) | 115.2 (1.2) | 114.6 (6.4) | 108.3 (7.0) | 115.3 (9.1) | 105.9 (3.2) | 73.2 (5.4) | 81.5 (1.7) | 76.0 (5.2) | |||
6:2FTOH | 105.2 (3.5) | 99.6 (2.5) | 103.3 (1.5) | 100.7 (1.4) | 95.7 (2.4) | 93.2 (1.3) | 100.6 (1.7) | 117.2 (9.2) | 101.0 (2.0) | |||
8:2FTOH | 106.5 (2.1) | 94.4 (5.8) | 105.4 (3.6) | 111.7 (4.3) | 90.6 (4.6) | 93.5 (2.1) | 92.5 (4.4) | 95.4 (4.2) | 101.3 (5.0) | |||
10:2FTA | 99.7 (3.8) | 97.3 (3.7) | 102.6 (5.9) | 101.8 (3.8) | 100.9 (4.1) | 101.3 (3.3) | 95.6 (2.5) | 98.6 (3.0) | 98.0 (5.2) | |||
10:2FTOH | 116.2 (4.0) | 96.3 (6.5) | 100.1 (4.0) | 99.1 (0.1) | 90.8 (5.4) | 90.4 (3.5) | 78.8 (4.1) | 86.5 (3.7) | 99.3 (5.4) | |||
N-Et-FOSA | 92.8 (7.8) | 84.7 (6.3) | 91.0 (8.7) | 95.3 (7.0) | 81.3 (5.6) | 90.2 (3.4) | 105.9 (8.2) | 92.5 (7.3) | 98.5 (1.0) | |||
N-Me-FOSA | 94.5 (7.4) | 80.5 (6.3) | 87.4 (6.2) | 86.6 (9.0) | 79.4 (5.9) | 91.7 (4.8) | 96.4 (7.0) | 90.3 (4.7) | 101.9 (2.6) | |||
N-Me-FOSE | 114.6 (3.3) | 102.5 (7.7) | 104.8 (7.9) | 95.1 (8.5) | 93.0 (7.6) | 99.6 (8.9) | 110.1 (6.3) | 94.5 (9.2) | 100.5 (9.4) | |||
N-Et-FOSE | 103.6 (6.5) | 102.3 (8.3) | 105.9 (9.1) | 100.5 (5.5) | 97.4 (9.2) | 98.7 (8.9) | 107.4 (8.7) | 97.8 (4.2) | 101.8 (5.8) |
Compound | Contents/(mg/kg) | ||||||||||||||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Uncoated textile samples | Coated textile samples | Synthetic leather samples | |||||||||||||||||||||||
1# | 2# | 3# | 4# | 5# | 6# | 7# | 8# | 9# | 10# | 11# | 12# | 13# | |||||||||||||
6:2FTA | - | - | - | - | - | - | - | - | - | - | - | - | - | ||||||||||||
4:2FTOH | - | - | - | - | - | - | - | - | - | - | - | - | - | ||||||||||||
8:2FTA | - | - | - | - | - | - | - | - | - | - | - | - | - | ||||||||||||
6:2FTOH | - | - | 26.3 | 0.38 | - | - | - | 3.63 | 6.72 | 3.68 | 3.81 | 3.34 | 2.94 | ||||||||||||
8:2FTOH | 0.24 | - | - | 0.72 | 0.61 | 26.2 | 196 | 1058 | 1745 | 1398 | 1269 | 1421 | 347 | ||||||||||||
10:2FTA | - | - | - | - | - | - | - | - | - | - | - | - | - | ||||||||||||
10:2FTOH | - | - | - | 0.34 | 2.83 | 100 | 41.1 | 327 | 572 | 497 | 405 | 1837 | 386 | ||||||||||||
N-Et-FOSA | - | - | - | - | - | - | - | - | - | - | - | - | - | ||||||||||||
N-Me-FOSA | - | - | - | - | - | - | - | - | - | - | - | - | - | ||||||||||||
N-Me-FOSE | - | 0.02 | - | - | - | - | - | - | - | - | - | - | - | ||||||||||||
N-Et-FOSE | - | - | - | - | - | - | - | - | - | - | - | - | - |
Table 4 Analytical results of the 11 perfluorinated compound precursors in textile samples (only samples with at least one target compound detected are listed)
Compound | Contents/(mg/kg) | ||||||||||||||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Uncoated textile samples | Coated textile samples | Synthetic leather samples | |||||||||||||||||||||||
1# | 2# | 3# | 4# | 5# | 6# | 7# | 8# | 9# | 10# | 11# | 12# | 13# | |||||||||||||
6:2FTA | - | - | - | - | - | - | - | - | - | - | - | - | - | ||||||||||||
4:2FTOH | - | - | - | - | - | - | - | - | - | - | - | - | - | ||||||||||||
8:2FTA | - | - | - | - | - | - | - | - | - | - | - | - | - | ||||||||||||
6:2FTOH | - | - | 26.3 | 0.38 | - | - | - | 3.63 | 6.72 | 3.68 | 3.81 | 3.34 | 2.94 | ||||||||||||
8:2FTOH | 0.24 | - | - | 0.72 | 0.61 | 26.2 | 196 | 1058 | 1745 | 1398 | 1269 | 1421 | 347 | ||||||||||||
10:2FTA | - | - | - | - | - | - | - | - | - | - | - | - | - | ||||||||||||
10:2FTOH | - | - | - | 0.34 | 2.83 | 100 | 41.1 | 327 | 572 | 497 | 405 | 1837 | 386 | ||||||||||||
N-Et-FOSA | - | - | - | - | - | - | - | - | - | - | - | - | - | ||||||||||||
N-Me-FOSA | - | - | - | - | - | - | - | - | - | - | - | - | - | ||||||||||||
N-Me-FOSE | - | 0.02 | - | - | - | - | - | - | - | - | - | - | - | ||||||||||||
N-Et-FOSE | - | - | - | - | - | - | - | - | - | - | - | - | - |
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