Investigation of Residue Dissipation of Fluxapyroxad and Its Metabolites in Chinese Cabbage and Spring Scallion Using Different Application Methods
Abstract
:1. Introduction
2. Results and Discussion
2.1. Method Validation for the Quantitative Analysis of Fluxapyroxad and Its Metabolites
2.2. Effect of Systemic Application on Fluxapyroxad Residue in Chinese Cabbage
2.3. Effect of Systemic Application on Fluxapyroxad Residue in Spring Scallion
2.4. Crop Dilution and Degradation Effect on Fluxapyroxad Residue
3. Materials and Methods
3.1. Standards and Reagents
3.2. Field Experiment and Fungicide Application
3.3. Sample Preparation for Residue Analysis of Fluxapyroxad
3.4. Validation of Analytical Method
3.5. Total Fluxapyroxad
3.6. Crop Growth Dilution Effect
3.7. Statistical Analysis
4. Conclusions
Author Contributions
Funding
Data Availability Statement
Conflicts of Interest
References
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Matrix | Compound | R2 | LOQ (mg kg−1) | Mean Recoveries ± SD(%, n = 3) | |||
---|---|---|---|---|---|---|---|
0.01 mg kg−1 | CV(%) | 0.1 mg kg−1 | CV(%) | ||||
Chinese cabbage | Fluxapyroxad | 0.9995 | 0.01 | 99.2 ± 3.9 | 2.6 | 109.6 ± 0.9 | 1.0 |
M700F048 | 0.9992 | 0.01 | 90.2 ±4.1 | 6.4 | 112.7 ± 1.8 | 1.7 | |
M700F002 | 0.9993 | 0.02 | 104.0 ± 2.5 | 1.1 | 97.8 ± 4.6 | 1.5 | |
Scallion | Fluxapyroxad | 0.9998 | 0.01 | 84.7 ± 2.0 | 2.7 | 104.3 ± 1.7 | 2.3 |
M700F048 | 0.9998 | 0.01 | 95.7 ± 3.7 | 3.3 | 99.8 ± 1.2 | 1.6 | |
M700F002 | 0.9998 | 0.02 | 84.0 ± 8.1 | 11.2 | 96.1 ± 3.2 | 0.3 |
Compounds | DAT a (days) | Detected Residue (mg kg−1) (CV) | |||||
---|---|---|---|---|---|---|---|
Chinese Cabbage | Spring Scallion | ||||||
Soil | Foliar | Systemic | Soil | Foliar | Systemic | ||
Fluxapyroxad | 0 | <0.01 | 4.46 (6.5) | 3.11 (4.7) | 0.09 (4.7) | 0.20 (15.3) | 0.22 (6.8) |
3 | <0.01 | 1.89 (15.9) | 1.03 (8.2) | 0.07 (8.2) | 0.17 (18.5) | 0.16 (6.7) | |
7 | <0.01 | 0.89 (4.9) | 0.51 (11.8) | 0.05 (8.2) | 0.16 (5.4) | 0.13 (7.6) | |
10 | <0.01 | 0.41 (6.5) | 0.46 (9.1) | 0.04 (16.7) | 0.14 (18.5) | 0.14 (4.6) | |
14 | <0.01 | 0.21 (9.8) | 0.18 (3.5) | 0.01 (9.1) | 0.06 (5.6) | 0.09 (13.4) | |
M700F048 | 0 | 0.02 (16.8) | 0.11 (4.3) | 0.15 (2.2) | <0.01 | <0.01 | <0.01 |
3 | <0.01 | 0.10 (3.3) | 0.11 (9.1) | <0.01 | <0.01 | <0.01 | |
7 | <0.01 | 0.10 (4.4) | 0.10 (5.3) | <0.01 | <0.01 | <0.01 | |
10 | <0.01 | 0.06 (3.6) | 0.08 (8.0) | <0.01 | <0.01 | <0.01 | |
14 | <0.01 | 0.03 (7.0) | 0.04 (4.1) | <0.01 | <0.01 | <0.01 | |
M700F002 | 0 | <0.02 | <0.02 | <0.02 | <0.02 | <0.02 | <0.02 |
3 | <0.02 | <0.02 | <0.02 | <0.02 | <0.02 | <0.02 | |
7 | <0.02 | <0.02 | <0.02 | <0.02 | <0.02 | <0.02 | |
10 | <0.02 | <0.02 | <0.02 | <0.02 | <0.02 | <0.02 | |
14 | <0.02 | <0.02 | <0.02 | <0.02 | <0.02 | <0.02 | |
Total Fluxapyroxad | 0 | 0.01 (17.3) | 4.54 (6.4) | 3.22 (4.6) | 0.09 (4.7) | 0.20 (15.3) | 0.22 (6.8) |
3 | <0.01 | 1.96 (15.3) | 1.12 (8.2) | 0.07 (8.2) | 0.17 (18.5) | 0.16 (6.7) | |
7 | <0.01 | 0.96 (4.6) | 0.58 (10.9) | 0.05 (8.2) | 0.16 (5.4) | 0.13 (7.6) | |
10 | <0.01 | 0.46 (6.0) | 0.52 (9.0) | 0.04 (16.7) | 0.14 (18.5) | 0.14 (4.6) | |
14 | <0.01 | 0.23 (9.5) | 0.21 (3.2) | 0.01 (9.1) | 0.06 (5.6) | 0.09 (13.4) |
Crop | DAT a | Crop Weight (gfw plant−1) b | Detected Residue (mg kg−1, CV) | TDR (mg kg−1) | Residue Amount (μg plant−1) | Dissipation Ratio c |
---|---|---|---|---|---|---|
Chinese cabbage | 0 | 37.3a | 3.22, 4.6% | 3.22 | 120.1 | - |
3 | 64.1b | 1.12, 8.2% | 1.87 | 71.8 | 40.2% | |
7 | 72.4bc | 0.58, 10.9% | 1.66 | 42.0 | 65.0% | |
10 | 91.4c | 0.52, 9.0% | 1.31 | 47.5 | 60.4% | |
14 | 156.2d | 0.21, 3.2% | 0.77 | 32.8 | 72.7% | |
Spring scallion | 0 | 10.8a | 0.22, 6.8% | 0.22 | 2.38 | |
3 | 11.2a | 0.16, 6.7% | 0.21 | 1.79 | 24.6% | |
7 | 13.7a | 0.13, 7.6% | 0.17 | 1.78 | 25.0% | |
10 | 13.2a | 0.14, 4.6% | 0.18 | 1.69 | 28.9% | |
14 | 13.1a | 0.09, 13.4% | 0.18 | 1.23 | 48.2% |
Instrument | Shimadzu Triple Quadrupole LCMS-8050 | |||||||
---|---|---|---|---|---|---|---|---|
Analytes | Fluxapyroxad, M700F048 | M700F002 | ||||||
Column | Kinetex phenyl-hexyl (100 × 2.1 mm, 2.6 µm) | Hypercarb (100 × 2.1 mm, 3 µm) | ||||||
Mobile phase A | 0.1% formic acid in dH2O with 5 mM ammonium formate | 0.1% formic acid in dH2O with 5 mM ammonium formate | ||||||
Mobile phase B | 0.1% formic acid in ACN with 5 mM ammonium formate | 0.1% formic acid in ACN | ||||||
Gradient | Time (min) | A (%) | B(%) | Time (min) | A (%) | B(%) | ||
0 | 85 | 15 | 0 | 70 | 30 | |||
1.5 | 40 | 60 | 5 | 70 | 30 | |||
8 | 10 | 90 | 5.5 | 0 | 100 | |||
8.1 | 0 | 100 | 14 | 0 | 100 | |||
15 | 0 | 100 | 14.5 | 70 | 30 | |||
Flow rate | 0.2 mL/min | 0.3 mL/min | ||||||
Injection volume | 1 µL | 5 µL | ||||||
ColumnTemp. | 35 °C | 35 °C | ||||||
Ionization mode | ESI positive | |||||||
Scan type | MRM mode | |||||||
Detection ion (m/z) | Analyte | Precursor | Quantitative (CE) | Qualitative (CE) | Analyte | Precursor | Quantitative (CE) | Qualitative (CE) |
Fluxapyroxad | 381.7 | 362.1 (−17) | 342.0 (−23) | M700F002 | 161.0 | 141.0 (−14) | 116.9 (−14) | |
M700F048 | 529.8 | 347.7 (−23) | 367.8 (−23) |
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Lee, J.W.; Kim, J.-S.; Park, J.H.; Noh, H.H.; Oh, M.S.; Kim, J.-H.; Son, K.-A. Investigation of Residue Dissipation of Fluxapyroxad and Its Metabolites in Chinese Cabbage and Spring Scallion Using Different Application Methods. Plants 2024, 13, 2448. https://doi.org/10.3390/plants13172448
Lee JW, Kim J-S, Park JH, Noh HH, Oh MS, Kim J-H, Son K-A. Investigation of Residue Dissipation of Fluxapyroxad and Its Metabolites in Chinese Cabbage and Spring Scallion Using Different Application Methods. Plants. 2024; 13(17):2448. https://doi.org/10.3390/plants13172448
Chicago/Turabian StyleLee, Ji Won, Jin-Seong Kim, Ji Hyun Park, Hyun Ho Noh, Min Seok Oh, Jin-Hyo Kim, and Kyeong-Ae Son. 2024. "Investigation of Residue Dissipation of Fluxapyroxad and Its Metabolites in Chinese Cabbage and Spring Scallion Using Different Application Methods" Plants 13, no. 17: 2448. https://doi.org/10.3390/plants13172448