Chinese Journal of Chromatography ›› 2023, Vol. 41 ›› Issue (3): 265-273.DOI: 10.3724/SP.J.1123.2022.05021
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XUE Kunpeng1,2,*(), YU Lingyu2, REN Xingfa2, TU Bingfang2, CHEN Chao2, XU Ting2, HE Huan1, HU Shuai3
Received:
2022-05-18
Online:
2023-03-08
Published:
2023-03-02
Contact:
XUE Kunpeng, Tel:(0791)89107801,E-mail:kunpengxue@126.com.
Supported by:
CLC Number:
XUE Kunpeng, YU Lingyu, REN Xingfa, TU Bingfang, CHEN Chao, XU Ting, HE Huan, HU Shuai. Determination of 15 carbonyl compounds in soil using improved solid phase extraction-high performance liquid chromatography[J]. Chinese Journal of Chromatography, 2023, 41(3): 265-273.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2022.05021
Fig. 1 Chromatograms of the 15 carbonyl compound- dinitrophenylhydrazine (DNPH) derivatives in the national standard HJ 997-2018[23] Peak identifications: 1. formaldehyde (FOR); 2. acetaldehyde (ACETA); 3. acrolein (ACR); 4. acetone (ACETO); 5. propionaldehyde (PRO); 6. crotonaldehyde (CRO); 7. butanal (BUT); 8. benzaldehyde (BEN); 9. isovaleraldehyde (ISO); 10. valeraldehyde (VAL); 11. o-tolualdehyde (o-TOL); 12. m-tolualdehyde (m-TOL); 13. p-tolualdehyde (p-TOL); 14. hexanal (HEX); 15. 2,5-dimethylbenzaldehyde (DIM).
Fig. 2 Chromatograms of 15 carbonyl compound-DNPH derivatives in the standard solution Experimental conditions: mixed standard solution of the 15 carbonyl compounds at 0.1 mg/L; separation column, Ultimate? XB-C18 (250 mm×4.6 mm, 5 μm); mobile phase: acetonitrile-water; flow rate: 1.0 mL/min; column temperature: 30 ℃; injection volume: 20 μL; detection wavelength: 360 nm.
Fig. 3 Derivative effects of different solvents on the 15 carbonyl compounds The sample solution was prepared from a 10.0 g sample spiked with a mixed standard solution of the 15 carbonyl compounds at 0.1 mg/L.Conditions: a. 100 mL of sample solution, extracted with 0.065 mol/L acetic acid sodium-acetate buffer solution, added with 4 mL pH 3.0 citric acid-sodium citrate buffer solution and 6 mL 2,4-DNPH acetonitrile solution, derivatized at 40 ℃ for 1 h; b. 100 mL of sample solution, extracted with 0.065 mol/L acetic acid-sodium acetate buffer, added with 4 mL acetonitrile and 6 mL 2,4-DNPH acetonitrile solution, derivatized at 40 ℃ for 1 h; c. 100 mL of sample solution, extracted with acetonitrile, added with 6 mL 2,4-DNPH acetonitrile solution and 1.0 mL 20% phosphoric acid solution, derivatized at 4 ℃ for 6 h.
Fig. 6 Effect of extraction time on the recoveries of the 15 carbonyl compounds The extracted solution was prepared from a 10.0 g sample spiked with a mixed standard solution of the 15 carbonyl compounds at 0.1 mg/L.
SPE column type | Stationary phase group | Morphology | Specific surface area/(m2/g) | Particle size/μm | Pore size/nm |
---|---|---|---|---|---|
C18 | octadecyl | amorphous | 500 | 40-63 | 4 |
PS-DVB | polystyrene-divinyl polymer | spherical | 700 | 50-70 | 20 |
BRP | N-vinylpyrrolidone-divinyl polymer | spherical | 700 | 50-70 | 20 |
Table 1 Physicochemical properties of the packing materials of the three reversed-phase SPE cartridges
SPE column type | Stationary phase group | Morphology | Specific surface area/(m2/g) | Particle size/μm | Pore size/nm |
---|---|---|---|---|---|
C18 | octadecyl | amorphous | 500 | 40-63 | 4 |
PS-DVB | polystyrene-divinyl polymer | spherical | 700 | 50-70 | 20 |
BRP | N-vinylpyrrolidone-divinyl polymer | spherical | 700 | 50-70 | 20 |
Compound | C18 | PS-DVB | BRP | |||||
---|---|---|---|---|---|---|---|---|
ME/% | RSD/% | ME/% | RSD/% | ME/% | RSD/% | |||
FOR | 110.4 | 1.8 | 108.7 | 1.2 | 90.5 | 1.3 | ||
ACETA | 125.6 | 3.4 | 129.0 | 3.6 | 115.9 | 3.1 | ||
ACR | 113.9 | 2.8 | 110.2 | 2.1 | 102.7 | 4.6 | ||
ACETO | 129.0 | 2.7 | 118.0 | 3.5 | 98.4 | 1.3 | ||
PRO | 112.8 | 2.4 | 116.1 | 2.4 | 105.2 | 2.3 | ||
CRO | 127.2 | 4.6 | 125.4 | 3.6 | 107.8 | 1.0 | ||
BUT | 145.4 | 5.6 | 132.1 | 5.3 | 109.7 | 2.2 | ||
BEN | 128.0 | 3.7 | 127.1 | 2.0 | 104.4 | 1.3 | ||
ISO | 120.9 | 4.1 | 123.7 | 4.7 | 108.3. | 2.8 | ||
VAL | 130.5 | 4.3 | 124.3 | 4.4 | 109.1 | 3.0 | ||
o-TOL | 115.7 | 3.2 | 118.6 | 3.5 | 92.0 | 1.7 | ||
m-TOL | 113.3 | 4.0 | 113.7 | 3.0 | 101.7 | 2.5 | ||
p-TOL | 117.3 | 4.2 | 118.5 | 3.7 | 103.6 | 1.3 | ||
HEX | 111.2 | 1.6 | 116.4 | 1.9 | 103.8 | 1.3 | ||
DIM | 115.6 | 1.8 | 118.9 | 2.3 | 107.6 | 1.6 |
Table 2 Matrix effects of the SPE packing materials on the 15 carbonyl compounds (n=6)
Compound | C18 | PS-DVB | BRP | |||||
---|---|---|---|---|---|---|---|---|
ME/% | RSD/% | ME/% | RSD/% | ME/% | RSD/% | |||
FOR | 110.4 | 1.8 | 108.7 | 1.2 | 90.5 | 1.3 | ||
ACETA | 125.6 | 3.4 | 129.0 | 3.6 | 115.9 | 3.1 | ||
ACR | 113.9 | 2.8 | 110.2 | 2.1 | 102.7 | 4.6 | ||
ACETO | 129.0 | 2.7 | 118.0 | 3.5 | 98.4 | 1.3 | ||
PRO | 112.8 | 2.4 | 116.1 | 2.4 | 105.2 | 2.3 | ||
CRO | 127.2 | 4.6 | 125.4 | 3.6 | 107.8 | 1.0 | ||
BUT | 145.4 | 5.6 | 132.1 | 5.3 | 109.7 | 2.2 | ||
BEN | 128.0 | 3.7 | 127.1 | 2.0 | 104.4 | 1.3 | ||
ISO | 120.9 | 4.1 | 123.7 | 4.7 | 108.3. | 2.8 | ||
VAL | 130.5 | 4.3 | 124.3 | 4.4 | 109.1 | 3.0 | ||
o-TOL | 115.7 | 3.2 | 118.6 | 3.5 | 92.0 | 1.7 | ||
m-TOL | 113.3 | 4.0 | 113.7 | 3.0 | 101.7 | 2.5 | ||
p-TOL | 117.3 | 4.2 | 118.5 | 3.7 | 103.6 | 1.3 | ||
HEX | 111.2 | 1.6 | 116.4 | 1.9 | 103.8 | 1.3 | ||
DIM | 115.6 | 1.8 | 118.9 | 2.3 | 107.6 | 1.6 |
Compound | Linear range/ (μg/mL) | Linear equation | r2 | LODs/(mg/L) | LOQs/(mg/L) | |||
---|---|---|---|---|---|---|---|---|
This method | HJ 997-2018 | This method | HJ 997-2018 | |||||
FOR | 0.1-20.0 | y=13.613x+0.052 | 0.997 | 0.02 | 0.02 | 0.05 | 0.08 | |
ACETA | 0.2-20.0 | y=10.242x+0.045 | 0.996 | 0.03 | 0.04 | 0.10 | 0.16 | |
ACR | 0.2-20.0 | y=9.355x+0.038 | 0.996 | 0.03 | 0.04 | 0.10 | 0.16 | |
ACETO | 0.2-20.0 | y=7.977x+0.040 | 0.997 | 0.03 | 0.04 | 0.10 | 0.16 | |
PRO | 0.2-20.0 | y=7.419x+0.017 | 0.996 | 0.03 | 0.04 | 0.10 | 0.16 | |
CRO | 0.2-20.0 | y=6.648x+0.017 | 0.997 | 0.04 | 0.04 | 0.14 | 0.16 | |
BUT | 0.5-20.0 | y=4.789x+0.005 | 0.998 | 0.04 | 0.04 | 0.13 | 0.16 | |
BEN | 0.2-20.0 | y=4.633x+0.024 | 0.996 | 0.04 | 0.06 | 0.13 | 0.24 | |
ISO | 0.5-20.0 | y=4.037x+0.015 | 0.996 | 0.05 | 0.06 | 0.18 | 0.24 | |
VAL | 0.5-20.0 | y=3.558x+0.067 | 0.997 | 0.05 | 0.06 | 0.18 | 0.24 | |
o-TOL | 0.5-20.0 | y=3.865x+0.012 | 0.996 | 0.05 | 0.05 | 0.10 | 0.20 | |
m-TOL | 0.5-20.0 | y=4.113x+0.014 | 0.999 | 0.05 | 0.06 | 0.18 | 0.24 | |
p-TOL | 0.5-20.0 | y=3.588x+0.025 | 0.999 | 0.05 | 0.06 | 0.18 | 0.24 | |
HEX | 0.5-20.0 | y=3.931x-0.047 | 0.998 | 0.06 | 0.06 | 0.20 | 0.24 | |
DIM | 0.5-20.0 | y=3.294x-0.003 | 0.999 | 0.06 | 0.06 | 0.20 | 0.24 |
Table 3 Linear relationships, limits of detection (LODs) and limits of quantification (LOQs) of the 15 carbonyl compounds
Compound | Linear range/ (μg/mL) | Linear equation | r2 | LODs/(mg/L) | LOQs/(mg/L) | |||
---|---|---|---|---|---|---|---|---|
This method | HJ 997-2018 | This method | HJ 997-2018 | |||||
FOR | 0.1-20.0 | y=13.613x+0.052 | 0.997 | 0.02 | 0.02 | 0.05 | 0.08 | |
ACETA | 0.2-20.0 | y=10.242x+0.045 | 0.996 | 0.03 | 0.04 | 0.10 | 0.16 | |
ACR | 0.2-20.0 | y=9.355x+0.038 | 0.996 | 0.03 | 0.04 | 0.10 | 0.16 | |
ACETO | 0.2-20.0 | y=7.977x+0.040 | 0.997 | 0.03 | 0.04 | 0.10 | 0.16 | |
PRO | 0.2-20.0 | y=7.419x+0.017 | 0.996 | 0.03 | 0.04 | 0.10 | 0.16 | |
CRO | 0.2-20.0 | y=6.648x+0.017 | 0.997 | 0.04 | 0.04 | 0.14 | 0.16 | |
BUT | 0.5-20.0 | y=4.789x+0.005 | 0.998 | 0.04 | 0.04 | 0.13 | 0.16 | |
BEN | 0.2-20.0 | y=4.633x+0.024 | 0.996 | 0.04 | 0.06 | 0.13 | 0.24 | |
ISO | 0.5-20.0 | y=4.037x+0.015 | 0.996 | 0.05 | 0.06 | 0.18 | 0.24 | |
VAL | 0.5-20.0 | y=3.558x+0.067 | 0.997 | 0.05 | 0.06 | 0.18 | 0.24 | |
o-TOL | 0.5-20.0 | y=3.865x+0.012 | 0.996 | 0.05 | 0.05 | 0.10 | 0.20 | |
m-TOL | 0.5-20.0 | y=4.113x+0.014 | 0.999 | 0.05 | 0.06 | 0.18 | 0.24 | |
p-TOL | 0.5-20.0 | y=3.588x+0.025 | 0.999 | 0.05 | 0.06 | 0.18 | 0.24 | |
HEX | 0.5-20.0 | y=3.931x-0.047 | 0.998 | 0.06 | 0.06 | 0.20 | 0.24 | |
DIM | 0.5-20.0 | y=3.294x-0.003 | 0.999 | 0.06 | 0.06 | 0.20 | 0.24 |
Compound | 0.2 mg/kg | 0.5 mg/kg | 2.0 mg/kg | ||||||
---|---|---|---|---|---|---|---|---|---|
Recovery/ % | RSD/ % | Recovery/ % | RSD/ % | Recovery/ % | RSD/ % | ||||
FOR | 84.6 | 1.7 | 88.3 | 2.6 | 90.5 | 1.3 | |||
ACETA | 112.7 | 4.1 | 110.2 | 4.1 | 115.9 | 4.1 | |||
ACR | 99.3 | 5.0 | 106.9 | 2.8 | 102.7 | 4.6 | |||
ACETO | 104.4 | 1.2 | 101.1 | 1.7 | 98.4 | 1.3 | |||
PRO | 105.1 | 3.5 | 106.1 | 2.7 | 105.2 | 2.3 | |||
CRO | 107.2 | 1.6 | 108.4 | 2.5 | 107.8 | 1.0 | |||
BUT | 100.2 | 3.5 | 99.8 | 3.6 | 109.7 | 0.2 | |||
BEN | 106.3 | 3.9 | 105.4 | 2.7 | 104.4 | 1.3 | |||
ISO | 107.0 | 4.3 | 110.6 | 3.0 | 108.3 | 2.8 | |||
VAL | 105.2 | 1.9 | 98.6 | 1.6 | 109.1 | 3.0 | |||
o-TOL | 87.5 | 0.6 | 89.7 | 3.6 | 92.0 | 1.7 | |||
m-TOL | 85.4 | 2.8 | 90.2 | 2.7 | 101.7 | 2.5 | |||
p-TOL | 91.2 | 5.1 | 96.6 | 2.9 | 103.6 | 1.3 | |||
HEX | 104.0 | 2.9 | 106.5 | 2.5 | 103.8 | 0.3 | |||
DIM | 97.6 | 2.0 | 96.1 | 1.8 | 107.6 | 0.6 |
Table 4 Spiked recoveries and RSDs of the 15 carbonyl compounds (n=6)
Compound | 0.2 mg/kg | 0.5 mg/kg | 2.0 mg/kg | ||||||
---|---|---|---|---|---|---|---|---|---|
Recovery/ % | RSD/ % | Recovery/ % | RSD/ % | Recovery/ % | RSD/ % | ||||
FOR | 84.6 | 1.7 | 88.3 | 2.6 | 90.5 | 1.3 | |||
ACETA | 112.7 | 4.1 | 110.2 | 4.1 | 115.9 | 4.1 | |||
ACR | 99.3 | 5.0 | 106.9 | 2.8 | 102.7 | 4.6 | |||
ACETO | 104.4 | 1.2 | 101.1 | 1.7 | 98.4 | 1.3 | |||
PRO | 105.1 | 3.5 | 106.1 | 2.7 | 105.2 | 2.3 | |||
CRO | 107.2 | 1.6 | 108.4 | 2.5 | 107.8 | 1.0 | |||
BUT | 100.2 | 3.5 | 99.8 | 3.6 | 109.7 | 0.2 | |||
BEN | 106.3 | 3.9 | 105.4 | 2.7 | 104.4 | 1.3 | |||
ISO | 107.0 | 4.3 | 110.6 | 3.0 | 108.3 | 2.8 | |||
VAL | 105.2 | 1.9 | 98.6 | 1.6 | 109.1 | 3.0 | |||
o-TOL | 87.5 | 0.6 | 89.7 | 3.6 | 92.0 | 1.7 | |||
m-TOL | 85.4 | 2.8 | 90.2 | 2.7 | 101.7 | 2.5 | |||
p-TOL | 91.2 | 5.1 | 96.6 | 2.9 | 103.6 | 1.3 | |||
HEX | 104.0 | 2.9 | 106.5 | 2.5 | 103.8 | 0.3 | |||
DIM | 97.6 | 2.0 | 96.1 | 1.8 | 107.6 | 0.6 |
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