Screening and Evaluation of Variables for Determination of Sulfonylurea Herbicides in Water Samples by Capillary Zone Electrophoresis
Abstract
:1. Introduction
2. Materials and Methods
2.1. Chemicals and Reagents
2.2. Instrumentation and Software
2.3. CE Analysis
2.4. Water Samples
3. Results and Discussion
3.1. Preliminary Studies
3.2. Method Optimization
3.3. Screening Process
3.4. Analytical Performance
3.5. Analysis of Real Samples
4. Conclusions
Acknowledgments
Author Contributions
Conflicts of Interest
References
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Factors | ||||
---|---|---|---|---|
Exp. | pH | Methanol %(v/v) | Voltage (kV) | Resolution (Rs) |
1 | 8.5 | 3 | 15 | 2.29 |
2 | 9.5 | 3 | 15 | 1.73 |
3 | 8.5 | 8 | 15 | 1.99 |
4 | 9.5 | 8 | 15 | 1.45 |
5 | 8.5 | 3 | 25 | 2.07 |
6 | 9.5 | 3 | 25 | 1.12 |
7 | 8.5 | 8 | 25 | 2.11 |
8 | 9.5 | 8 | 25 | 2.08 |
9 | 9.0 | 5.5 | 20 | 1.60 |
10 | 9.0 | 5.5 | 20 | 1.79 |
11 | 9.0 | 5.5 | 20 | 1.78 |
Analytes | Method | Detection Time (min) | Separation Medium | LODs | Ref. |
---|---|---|---|---|---|
12 sulfonylurea compounds including Metsulfuron-methyl and Nicosulfuron | CZE-UV (λ: 239 nm) | NS (25) | 50 mM acetate buffer, pH 4.76 | 1.0 µg·kg−1 soil (SPE included through C18 column) | [19] |
MSM (29) | |||||
12 sulfonylurea compounds including Metsulfuron-methyl and Nicosulfuron | LC-UV (λ: 226 nm) | NS (13) | mobile phase: acetonitrile–0.01M H3PO4 (gradient elution program) | 1.0 µg·kg−1 soil (SPE included through C18 column) | [19] |
MSM (21) | |||||
17 sulfonylurea compounds including Metsulfuron-methyl Nicosulfuron and degradation products | CZE-UV (λ: 239 nm) | NS (12.9) | 25 mM acetic acid and 25 mM sodium acetate, pH 4.76, and 1.86 M acetonitrile in water | 0.1 µg·mL−1 (NS and MSM) | [20] |
MSM (14.8) | |||||
8 sulfonylurea compounds including Metsulfuron-methyl and Nicosulfuron | CZE-UV (λ: 254 nm) | NS (6) | 5 mM ammonium acetate-acetonitrile (75:25), pH 5 | - | [21] |
MSM (8) | |||||
10 sulfonylurea compounds including Metsulfuron-methyl and Nicosulfuron | LC-ESI-MS | NS (10.7) | mobile phase: acetonitrile/methanol–0.2% (v/v) acetic acid in water (gradient elution program) | 3.5 µg·mL−1 (NS), 1.5 µg·mL−1 (MSM) | [22] |
MSM (11.5) | |||||
30 sulfonylurea compounds including Metsulfuron-methyl and Nicosulfuron | LC-MS2 | NS (14.2) | Mobile phase: acetonitrile–0.1% formic acid (gradient elution program) | 6.10−7µg·mL−1 (NS) 3.10−7µg·mL−1 (MSM) (SPE included through Oasis HLB cartridges) | [23] |
MSM (15.5) | |||||
Nicosulfuron and metsulfuron-methyl | CZE-UV (λ: 231 nm) | NS (9.1) | 25 mM sodium borate, 3% v/v methanol, pH 8.5 | 0.044 µg·mL−1 (NS) 0.034 µg·mL−1 (MSM) | This work |
MSM (9.8) |
Sample Added (µg·mL−1) | Found (µg·mL−1) * ± SD | RSD (%) | Recovery (%) | |
---|---|---|---|---|
Groundwater | ||||
NS | 0.1 | 0.092 ± 0.002 | 2.2 | 92.0 |
0.5 | 0.455 ± 0.007 | 1.5 | 92.0 | |
MSM | 0.1 | 0.082 ± 0.002 | 2.4 | 82.0 |
0.5 | 0.499 ± 0.004 | 0.8 | 99.8 | |
Surface | ||||
NS | 0.1 | 0.102 ± 0.006 | 5.8 | 102 |
0.5 | 0.471 ± 0.003 | 0.6 | 94.2 | |
MSM | 0.1 | 0.097 ± 0.003 | 3.1 | 97.0 |
0.5 | 0.500 ± 0.009 | 1.8 | 100 |
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Springer, V.; Di Anibal, C.V.; Lista, A.G. Screening and Evaluation of Variables for Determination of Sulfonylurea Herbicides in Water Samples by Capillary Zone Electrophoresis. Separations 2016, 3, 22. https://doi.org/10.3390/separations3030022
Springer V, Di Anibal CV, Lista AG. Screening and Evaluation of Variables for Determination of Sulfonylurea Herbicides in Water Samples by Capillary Zone Electrophoresis. Separations. 2016; 3(3):22. https://doi.org/10.3390/separations3030022
Chicago/Turabian StyleSpringer, Valeria, Carolina V. Di Anibal, and Adriana G. Lista. 2016. "Screening and Evaluation of Variables for Determination of Sulfonylurea Herbicides in Water Samples by Capillary Zone Electrophoresis" Separations 3, no. 3: 22. https://doi.org/10.3390/separations3030022