Development of Simultaneous Determination Method of Pesticide High Toxic Metabolite 3,4-Dichloroaniline and 3,5 Dichloroaniline in Chives Using HPLC-MS/MS
Abstract
:1. Introduction
2. Materials and Methods
2.1. Chemical and Reagents
2.2. Stock and Standard Solutions
2.3. Instruments and Analytical Conditions
2.4. Sample Preparation
2.5. Validation of the Method
2.6. Statistical Analysis
3. Results and Discussion
3.1. Optimization of Mass Spectrum Conditions
3.2. Optimization of Chromatographic Conditions
3.3. Optimization of Extractants in Chive Samples
3.4. Evaluation of the Purification Effects on Chive Samples
3.5. Method Validation
3.5.1. Linearity, LOD, and LOQ
3.5.2. Accuracy and Precision
3.6. Application of Method for the Analysis of Real Samples
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Data Availability Statement
Conflicts of Interest
Abbreviations
AA | ammonia water |
ACE | acetone |
ACN | acetonitrile |
BEN | benzene |
3,4-DCA | 3,4-Dichloroaniline |
3,5-DCA | 3,5 Dichloroaniline |
DCM | dichloromethane |
EA | ethyl acetate |
FA | formic acid |
GCB | graphite carbon black |
GC | gas chromatography |
GC-MS | gas chromatography-mass spectrometry |
HPLC | liquid chromatography |
UPLC-MS/MS | ultra-high performance liquid chromatography-tandem mass spectrometry |
HPLC-MS/MS | high-performance liquid chromatography-tandem mass spectrometry |
LOD | limit of detection |
LOQ | limit of quantitation) |
ME | matrix effect |
MEOH | methanol |
MB | toluene |
MRL | maximum residue limit |
PSA | primary secondary amine |
Appendix A
References
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Retention Time/min | Flow Rate/(mL/min) | Mobile Phase A/% | Mobile Phase B/% |
---|---|---|---|
0 | 0.5 | 30 | 70 |
1 | 0.5 | 30 | 70 |
3 | 0.5 | 10 | 90 |
5 | 0.5 | 30 | 70 |
6 | 0.5 | 30 | 70 |
Type of Elution | Compound | Peak Area 1 | Peak Area 2 | Peak Area 3 | Mean Peak Area | Response Improvement Rate (%) |
---|---|---|---|---|---|---|
Isocratic elution | 3,4-DCA | 605.95 | 666.08 | 585.39 | 619.14 | — |
3,5-DCA | 298.19 | 286.52 | 307.86 | 297.52 | — | |
Gradient elute | 3,4-DCA | 742.75 | 744.61 | 779.67 | 755.68 | 22.05 |
3,5-DCA | 458.88 | 465.01 | 461.95 | 461.95 | 55.26 |
Compound | Matrix | Linear Equation | R2 | LOD (μg/kg) | LOQ (μg/kg) | ME (%) |
---|---|---|---|---|---|---|
3,4-DCA | Aboveground tissue | 0.9972 | 0.6 | 2.0 | −9.0 | |
Underground tissue | 0.9999 | −2.6 | ||||
Solvent | 0.9999 * | — | — | — | ||
3,5-DCA | Aboveground tissue | 0.9969 | 1.0 | 3.0 | −4.4 | |
Underground tissue | 0.9999 | 2.3 | ||||
Solvent | 0.9999 * | — | — | — |
Compound | Matrix | Addition Level (mg/kg) | Average Recovery (%) | RSD (%) |
---|---|---|---|---|
3,4-DCA | Aboveground tissue | 0.001 | 75.3 | 8.5 |
0.010 | 85.4 | 4.3 | ||
0.100 | 80.1 | 2.6 | ||
1.000 | 84.4 | 2.1 | ||
Underground tissue | 0.001 | 78.5 | 6.7 | |
0.010 | 77.3 | 3.8 | ||
0.100 | 81.2 | 3.2 | ||
1.000 | 86.0 | 2.7 | ||
3,5-DCA | Aboveground tissue | 0.001 | 78.2 | 9.4 |
0.010 | 98.1 | 7.5 | ||
0.100 | 87.1 | 5.1 | ||
1.000 | 94.3 | 2.1 | ||
Underground tissue | 0.001 | 79.6 | 10.6 | |
0.010 | 82.0 | 11.9 | ||
0.100 | 87.2 | 2.9 | ||
1.000 | 93.4 | 1.4 |
Compound | Parent Compounds | Vegetable | Average (mg/kg) | Median (mg/kg) | Range (mg/kg) |
---|---|---|---|---|---|
3,4-DCA | Diuron | Chive | 0.076 | 0.082 | 0.01–0.176 |
Carrot | 0.016 | 0.024 | 0.002–0.053 | ||
Onions | — | — | — | ||
Leek | — | — | — | ||
Parsley | — | — | — | ||
Propanil | Spinach | — | — | — | |
Tomato | — | — | — | ||
Cucumber | — | — | — | ||
Potato | — | — | — | ||
Pepper | — | — | — | ||
3,5-DCA | Iprodione | Chive | 0.083 | 0.067 | 0.01–0.2 |
Leek | 0.273 | 0.312 | 0.02–1.07 | ||
Tomato | 0.084 | 0.067 | 0.01–0.154 | ||
Onion | — | — | — | ||
Cucumber | — | — | — | ||
Procymidone | Potato | — | — | — | |
Pepper | — | — | — | ||
Parsley | — | — | — | ||
Spinach | — | — | — | ||
Carrot | — | — | — |
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Dong, Y.; Yao, X.; Zhang, W.; Wu, X. Development of Simultaneous Determination Method of Pesticide High Toxic Metabolite 3,4-Dichloroaniline and 3,5 Dichloroaniline in Chives Using HPLC-MS/MS. Foods 2023, 12, 2875. https://doi.org/10.3390/foods12152875
Dong Y, Yao X, Zhang W, Wu X. Development of Simultaneous Determination Method of Pesticide High Toxic Metabolite 3,4-Dichloroaniline and 3,5 Dichloroaniline in Chives Using HPLC-MS/MS. Foods. 2023; 12(15):2875. https://doi.org/10.3390/foods12152875
Chicago/Turabian StyleDong, Yibo, Xiaolong Yao, Wanping Zhang, and Xiaomao Wu. 2023. "Development of Simultaneous Determination Method of Pesticide High Toxic Metabolite 3,4-Dichloroaniline and 3,5 Dichloroaniline in Chives Using HPLC-MS/MS" Foods 12, no. 15: 2875. https://doi.org/10.3390/foods12152875