Chinese Journal of Chromatography ›› 2020, Vol. 38 ›› Issue (11): 1308-1315.DOI: 10.3724/SP.J.1123.2020.01020
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Jiwei YUAN1, Jincheng WANG2,*(), Weili XU1, Fangxi XU1, Xianbo LU2
Received:
2020-03-02
Online:
2020-11-08
Published:
2020-12-11
Contact:
Jincheng WANG
Supported by:
Jiwei YUAN, Jincheng WANG, Weili XU, Fangxi XU, Xianbo LU. Simultaneous determination of polycyclic aromatic hydrocarbons and phthalate esters in surface water by dispersive liquid-liquid microextraction based on solidification of floating organic drop followed by high performance liquid chromatography[J]. Chinese Journal of Chromatography, 2020, 38(11): 1308-1315.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2020.01020
Time/min | Excitation wavelength/nm | Emission wavelength/nm |
0 | 265 | 340 |
9.50 | 265 | 420 |
11.80 | 270 | 420 |
19.50 | 300 | 430 |
26.60 | 300 | 500 |
Table 1 Excitation and emission wavelengths for fluorescence detection
Time/min | Excitation wavelength/nm | Emission wavelength/nm |
0 | 265 | 340 |
9.50 | 265 | 420 |
11.80 | 270 | 420 |
19.50 | 300 | 430 |
26.60 | 300 | 500 |
Fig. 1 Chromatograms of polycyclic aromatic hydrocarbons (PAHs) and phthalate esters (PAEs) a. fluorescence detection; b. UV detection. 1. dimethyl phthalate (DMP); 2. diethyl phthalate (DEP); 3. naphthalene (NaP); 4 acenaphthylene (AcL); 5. acenaphthene (Ace); 6. fluorine (Flu); 7. butyl benzyl phthalate (BBP); 8. dibutyl phthalate (DBP); 9. phenanthrene (PhA); 10. anthracene (AnT); 11. fluoranthene (FluA); 12. pyrene (pyr); 13. benzo[a ]anthracene (BaA); 14. chrysene (Chr); 15. benzo[b ]fluoranthene (BbF); 16. di(2-ethylhexyl)phthalate (DEHP); 17. benzo[k ]fluoranthene (BkF); 18. dioctyl phthalate (DOP); 19. benzo[a ]pyrene (BaP); 20. dibenzo[a , h ]anthracene (DbA); 21. benzo[g , h , i ]perylene (BghiP); 22. indenol[1, 2, 3-c , d ]pyrene (InP).
Fig. 2 Effect of volumes of extractive solvents on the extraction efficiencies of (a) PAHs and (b) PAEs Dispersive solvent: 400 μL methanol; m (NaCl): 0.2 g; vortex oscillation time: 2 min.
Fig. 3 Effect of volumes of dispersive solvents on the extraction efficiencies of (a) PAHs and (b) PAEs Extractive solvent: 10 μL 1-dodecanol; m (NaCl): 0.2 g; vortex oscillation time: 2 min.
Compound | Linear range/ (μg/L) | Linear equation | r | Added/ (μg/L) | Recovery/ % | RSD (n =3)/% | LOD/ (μg/L) | LOQ/ (μg/L) |
A : peak area; C : mass concentration, μg/L. | ||||||||
DMP | 8-1000 | A =0.0498C +0.1041 | 0.9999 | 16 | 78.0 | 9.5 | 2.2 | 7.4 |
80 | 91.4 | 3.8 | ||||||
800 | 84.9 | 1.9 | ||||||
DEP | 8-1000 | A =0.3001C +0.3957 | 0.9999 | 16 | 85.0 | 7.6 | 1.5 | 5.2 |
80 | 107.2 | 3.4 | ||||||
800 | 97.6 | 2.3 | ||||||
BBP | 1.6-1000 | A =1.4545C -8.3765 | 0.9997 | 16 | 87.0 | 5.6 | 0.3 | 0.9 |
80 | 96.4 | 2.6 | ||||||
800 | 92.0 | 2.4 | ||||||
DBP | 1.6-1000 | A =1.3246C -4.2022 | 0.9996 | 16 | 82.0 | 6.4 | 0.2 | 0.8 |
80 | 100.0 | 3.6 | ||||||
800 | 92.1 | 2.4 | ||||||
DEHP | 8-1000 | A =0.9831C -6.8964 | 0.9998 | 16 | 85.6 | 4.5 | 0.36 | 1.2 |
80 | 86.3 | 3.2 | ||||||
800 | 89.6 | 3.0 | ||||||
DOP | 8-1000 | A =0.9772C -7.5297 | 0.9997 | 16 | 87.2 | 4.6 | 0.96 | 3.2 |
80 | 100.7 | 2.1 | ||||||
800 | 89.2 | 2.9 | ||||||
NaP | 0.032-20 | A =33.5929C -6.2300 | 0.9988 | 0.1 | 100.8 | 9.8 | 0.009 | 0.03 |
1.0 | 88.3 | 11.0 | ||||||
10 | 101.3 | 9.4 | ||||||
AcL | 0.8-20 | A =8.2097C -0.9605 | 0.9997 | 1.0 | 92.1 | 5.7 | 0.07 | 0.23 |
10 | 90.4 | 3.2 | ||||||
Ace | 0.032-20 | A =93.7444C -10.8165 | 0.9992 | 0.1 | 73.5 | 7.4 | 0.009 | 0.03 |
1.0 | 86.5 | 5.0 | ||||||
10 | 93.5 | 3.6 | ||||||
Flu | 0.0064-20 | A =286.7528C -20.0540 | 0.9994 | 0.1 | 88.9 | 2.3 | 0.002 | 0.007 |
1.0 | 94.1 | 3.0 | ||||||
10 | 93.1 | 2.0 | ||||||
PhA | 0.032-20 | A =59.9951C +2.3175 | 0.9998 | 0.1 | 72.0 | 6.2 | 0.006 | 0.02 |
1.0 | 85.0 | 4.4 | ||||||
10 | 91.5 | 2.7 | ||||||
AnT | 0.032-20 | A =204.3444C +3.9495 | 0.9999 | 0.1 | 67.7 | 11.7 | 0.004 | 0.02 |
1.0 | 96.8 | 3.5 | ||||||
10 | 86.2 | 2.8 | ||||||
FluA | 0.16-20 | A =32.6151C -1.9232 | 0.9996 | 0.1 | 66.9 | 12.3 | 0.02 | 0.08 |
1.0 | 92.5 | 2.2 | ||||||
10 | 91.0 | 2.8 | ||||||
Pyr | 0.0064-20 | A =112.7728C -5.1630 | 0.9997 | 0.1 | 96.9 | 8.4 | 0.008 | 0.027 |
1.0 | 101.0 | 4.5 | ||||||
10 | 98.9 | 4.7 | ||||||
BaA | 0.032-20 | A =137.4110C -17.3321 | 0.9996 | 0.1 | 73.1 | 14.3 | 0.002 | 0.007 |
1.0 | 93.5 | 3.3 | ||||||
10 | 93.2 | 2.0 | ||||||
Chr | 0.032-20 | A =9.4625C +0.0728 | 1.000 | 0.1 | 113.5 | 14.4 | 0.009 | 0.03 |
1.0 | 103.0 | 4.4 | ||||||
10 | 101.8 | 2.5 | ||||||
BbF | 0.032-20 | A =163.1200C -17.9893 | 0.9996 | 0.1 | 66.6 | 11.7 | 0.008 | 0.027 |
1.0 | 89.1 | 2.4 | ||||||
10 | 93.9 | 9.1 | ||||||
BkF | 0.0064-4 | A =807.0140C +0.0658 | 0.9999 | 0.1 | 92.0 | 8.1 | 0.002 | 0.006 |
1.0 | 106.9 | 2.1 | ||||||
10 | 80.3 | 7.6 | ||||||
BaP | 0.032-20 | A =350.6990C +2.6530 | 0.9995 | 0.1 | 60.7 | 13.6 | 0.005 | 0.016 |
1.0 | 66.0 | 2.6 | ||||||
10 | 96.2 | 1.5 | ||||||
DbA | 0.032-20 | A =222.8170C -30.6302 | 0.9996 | 0.1 | 70.2 | 14.3 | 0.004 | 0.014 |
1.0 | 90.7 | 2.9 | ||||||
10 | 88.5 | 2.0 | ||||||
BghiP | 0.032-20 | A =174.2370C -23.7386 | 0.9996 | 0.1 | 70.5 | 13.7 | 0.008 | 0.027 |
1.0 | 95.9 | 3.4 | ||||||
10 | 99.3 | 7.4 | ||||||
InP | 0.032-20 | A =83.2597C -12.9146 | 0.9995 | 0.1 | 60.2 | 9.4 | 0.006 | 0.02 |
1.0 | 79.5 | 1.9 | ||||||
10 | 88.2 | 6.8 |
Table 2 Linear ranges, linear equations, correlation coefficients (r ), spiked recoveries, precisions, limits of detection (LODs) and limits of quantification (LOQs) of the target compounds
Compound | Linear range/ (μg/L) | Linear equation | r | Added/ (μg/L) | Recovery/ % | RSD (n =3)/% | LOD/ (μg/L) | LOQ/ (μg/L) |
A : peak area; C : mass concentration, μg/L. | ||||||||
DMP | 8-1000 | A =0.0498C +0.1041 | 0.9999 | 16 | 78.0 | 9.5 | 2.2 | 7.4 |
80 | 91.4 | 3.8 | ||||||
800 | 84.9 | 1.9 | ||||||
DEP | 8-1000 | A =0.3001C +0.3957 | 0.9999 | 16 | 85.0 | 7.6 | 1.5 | 5.2 |
80 | 107.2 | 3.4 | ||||||
800 | 97.6 | 2.3 | ||||||
BBP | 1.6-1000 | A =1.4545C -8.3765 | 0.9997 | 16 | 87.0 | 5.6 | 0.3 | 0.9 |
80 | 96.4 | 2.6 | ||||||
800 | 92.0 | 2.4 | ||||||
DBP | 1.6-1000 | A =1.3246C -4.2022 | 0.9996 | 16 | 82.0 | 6.4 | 0.2 | 0.8 |
80 | 100.0 | 3.6 | ||||||
800 | 92.1 | 2.4 | ||||||
DEHP | 8-1000 | A =0.9831C -6.8964 | 0.9998 | 16 | 85.6 | 4.5 | 0.36 | 1.2 |
80 | 86.3 | 3.2 | ||||||
800 | 89.6 | 3.0 | ||||||
DOP | 8-1000 | A =0.9772C -7.5297 | 0.9997 | 16 | 87.2 | 4.6 | 0.96 | 3.2 |
80 | 100.7 | 2.1 | ||||||
800 | 89.2 | 2.9 | ||||||
NaP | 0.032-20 | A =33.5929C -6.2300 | 0.9988 | 0.1 | 100.8 | 9.8 | 0.009 | 0.03 |
1.0 | 88.3 | 11.0 | ||||||
10 | 101.3 | 9.4 | ||||||
AcL | 0.8-20 | A =8.2097C -0.9605 | 0.9997 | 1.0 | 92.1 | 5.7 | 0.07 | 0.23 |
10 | 90.4 | 3.2 | ||||||
Ace | 0.032-20 | A =93.7444C -10.8165 | 0.9992 | 0.1 | 73.5 | 7.4 | 0.009 | 0.03 |
1.0 | 86.5 | 5.0 | ||||||
10 | 93.5 | 3.6 | ||||||
Flu | 0.0064-20 | A =286.7528C -20.0540 | 0.9994 | 0.1 | 88.9 | 2.3 | 0.002 | 0.007 |
1.0 | 94.1 | 3.0 | ||||||
10 | 93.1 | 2.0 | ||||||
PhA | 0.032-20 | A =59.9951C +2.3175 | 0.9998 | 0.1 | 72.0 | 6.2 | 0.006 | 0.02 |
1.0 | 85.0 | 4.4 | ||||||
10 | 91.5 | 2.7 | ||||||
AnT | 0.032-20 | A =204.3444C +3.9495 | 0.9999 | 0.1 | 67.7 | 11.7 | 0.004 | 0.02 |
1.0 | 96.8 | 3.5 | ||||||
10 | 86.2 | 2.8 | ||||||
FluA | 0.16-20 | A =32.6151C -1.9232 | 0.9996 | 0.1 | 66.9 | 12.3 | 0.02 | 0.08 |
1.0 | 92.5 | 2.2 | ||||||
10 | 91.0 | 2.8 | ||||||
Pyr | 0.0064-20 | A =112.7728C -5.1630 | 0.9997 | 0.1 | 96.9 | 8.4 | 0.008 | 0.027 |
1.0 | 101.0 | 4.5 | ||||||
10 | 98.9 | 4.7 | ||||||
BaA | 0.032-20 | A =137.4110C -17.3321 | 0.9996 | 0.1 | 73.1 | 14.3 | 0.002 | 0.007 |
1.0 | 93.5 | 3.3 | ||||||
10 | 93.2 | 2.0 | ||||||
Chr | 0.032-20 | A =9.4625C +0.0728 | 1.000 | 0.1 | 113.5 | 14.4 | 0.009 | 0.03 |
1.0 | 103.0 | 4.4 | ||||||
10 | 101.8 | 2.5 | ||||||
BbF | 0.032-20 | A =163.1200C -17.9893 | 0.9996 | 0.1 | 66.6 | 11.7 | 0.008 | 0.027 |
1.0 | 89.1 | 2.4 | ||||||
10 | 93.9 | 9.1 | ||||||
BkF | 0.0064-4 | A =807.0140C +0.0658 | 0.9999 | 0.1 | 92.0 | 8.1 | 0.002 | 0.006 |
1.0 | 106.9 | 2.1 | ||||||
10 | 80.3 | 7.6 | ||||||
BaP | 0.032-20 | A =350.6990C +2.6530 | 0.9995 | 0.1 | 60.7 | 13.6 | 0.005 | 0.016 |
1.0 | 66.0 | 2.6 | ||||||
10 | 96.2 | 1.5 | ||||||
DbA | 0.032-20 | A =222.8170C -30.6302 | 0.9996 | 0.1 | 70.2 | 14.3 | 0.004 | 0.014 |
1.0 | 90.7 | 2.9 | ||||||
10 | 88.5 | 2.0 | ||||||
BghiP | 0.032-20 | A =174.2370C -23.7386 | 0.9996 | 0.1 | 70.5 | 13.7 | 0.008 | 0.027 |
1.0 | 95.9 | 3.4 | ||||||
10 | 99.3 | 7.4 | ||||||
InP | 0.032-20 | A =83.2597C -12.9146 | 0.9995 | 0.1 | 60.2 | 9.4 | 0.006 | 0.02 |
1.0 | 79.5 | 1.9 | ||||||
10 | 88.2 | 6.8 |
Compound | Tap water | Yingkou park | |||
Content/ (μg/L) | RSD/ % | Content/ (μg/L) | RSD/ % | ||
nd:<LOD. | |||||
DMP | nd | nd | |||
DEP | nd | nd | |||
BBP | nd | 7.6 | 5.5 | ||
DBP | 5.7 | 4.7 | 7.9 | 12.1 | |
DEHP | 15.3 | 4.6 | 11.7 | 11.8 | |
DOP | nd | 9.8 | 5.6 | ||
NaP | 0.19 | 0.8 | 0.22 | 3.0 | |
AcL | nd | nd | |||
Ace | 0.12 | 1.7 | 0.14 | 7.3 | |
Flu | 0.09 | 0.6 | 0.11 | 13.1 | |
PhA | 0.12 | 4.7 | 1.23 | 7.9 | |
AnT | nd | nd | |||
FluA | nd | 0.10 | 7.5 | ||
Pyr | nd | 0.08 | 23.4 | ||
BaA | nd | 0.14 | 4.8 | ||
Chr | nd | nd | |||
BbF | nd | 0.14 | 10.1 | ||
BkF | nd | nd | |||
BaP | nd | nd | |||
DbA | nd | 4.0 | 0.17 | 9.7 | |
BghiP | nd | 4.0 | 0.17 | 9.5 | |
InP | nd | 3.5 | 0.18 | 6.2 |
Table 3 Test results of the real water samples (n =3)
Compound | Tap water | Yingkou park | |||
Content/ (μg/L) | RSD/ % | Content/ (μg/L) | RSD/ % | ||
nd:<LOD. | |||||
DMP | nd | nd | |||
DEP | nd | nd | |||
BBP | nd | 7.6 | 5.5 | ||
DBP | 5.7 | 4.7 | 7.9 | 12.1 | |
DEHP | 15.3 | 4.6 | 11.7 | 11.8 | |
DOP | nd | 9.8 | 5.6 | ||
NaP | 0.19 | 0.8 | 0.22 | 3.0 | |
AcL | nd | nd | |||
Ace | 0.12 | 1.7 | 0.14 | 7.3 | |
Flu | 0.09 | 0.6 | 0.11 | 13.1 | |
PhA | 0.12 | 4.7 | 1.23 | 7.9 | |
AnT | nd | nd | |||
FluA | nd | 0.10 | 7.5 | ||
Pyr | nd | 0.08 | 23.4 | ||
BaA | nd | 0.14 | 4.8 | ||
Chr | nd | nd | |||
BbF | nd | 0.14 | 10.1 | ||
BkF | nd | nd | |||
BaP | nd | nd | |||
DbA | nd | 4.0 | 0.17 | 9.7 | |
BghiP | nd | 4.0 | 0.17 | 9.5 | |
InP | nd | 3.5 | 0.18 | 6.2 |
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