Simultaneous Determination of Glyphosate and 13 Multiclass Pesticides in Agricultural Soil by Direct-Immersion SPME Followed by Solid–Liquid Extraction
A new method is presented for the simultaneous determination of 13 multiclass pesticides along with glyphosate. The multiclass pesticides were extracted by creating a soil slurry with 2% ethanol in water (<i>v</i>/<i>v</i>), and then, applying direct-immersion solid-phase mic...
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| Main Authors: | , , , , |
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| Format: | Article |
| Language: | English |
| Published: |
MDPI AG
2024-09-01
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| Series: | Applied Sciences |
| Subjects: | |
| Online Access: | https://www.mdpi.com/2076-3417/14/19/8584 |
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| Summary: | A new method is presented for the simultaneous determination of 13 multiclass pesticides along with glyphosate. The multiclass pesticides were extracted by creating a soil slurry with 2% ethanol in water (<i>v</i>/<i>v</i>), and then, applying direct-immersion solid-phase microextraction (DI-SPME) with a new type of semi-disposable SPME fiber configuration called LC-Tips. The fibers were then retroextracted to ethanol, and aqueous ammonia was added to the slurry to extract glyphosate. Derivatization of the glyphosate extract was accomplished with a mixture of trifluoroacetic anhydride and trifluoroethanol, after which the reaction mixture was dried and resuspended with the SPME ethanol extract. To this, a mixture of analyte protectants was added, and it was analyzed by GC-MS/MS in multiple-reaction-monitoring mode. All analytes showed a coefficient of determination greater than 0.95 in the 0.1–100 µg/kg calibrated range, and the limits of detection were between 0.1 and 1 µg/kg, except for glyphosate, which was 0.01 µg/kg. The method shows relatively high replicate relative standard deviation (as much as 37% for five extractions at 20 µg/kg), but the isotopically labeled internal standard was effective at mitigating this effect for some analytes. |
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| ISSN: | 2076-3417 |