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Determination of Glyphosate and AMPA in Three Representative Agricultural Austrian Soils with a HPLC-MS/MS Method

, : Determination of Glyphosate and AMPA in Three Representative Agricultural Austrian Soils with a HPLC-MS/MS Method. Soil and Sediment Contamination: An International Journal 22(3): 332-350

We developed a novel method to quantify adsorbed glyphosate and AMPA in soils based on an extraction utilizing Na-tetraborate, an SPE clean-up step, and subsequent LC-MS detection. Reversed phase-based separation of glyphosate and AMPA was realized after FMOC-derivatization. The quantification involved external calibration and 1,2 13C, 15N- labeled glyphosate as well as 13C, 15N labeled AMPA as internal standards. The optimum recovery for extraction was obtained with 40 mM Na-tetraborate. The method was applied in three representative soils (Kirchberg, Phyra, and Pixendorf, Austria) where glyphosate was applied by standard agricultural practices. The recovery for glyphosate extracted with 40 mM Na-tetraborate buffer was 93.5% (RSD <2%) for glyphosate at Kirchberg-cambisol; 95.7% (RSD < 2%) at Pixendorf- chernozem and 79.1% (RSD <7%) at Phyra-stagnosol. The corresponding values for AMPA were 92.4% (RSD <2%) at Kirchberg, 98.1% (RSD <2%) at Pixendorf and 69.9% (RSD <4%) at Phyra. The limits of detection for glyphosate were 6.8 ?g kg?1(RSD <10%) at Kirchberg, 4.3 ?g kg?1 (RSD <10%) at Pixendorf, and 46.5 ?g kg?1 (RSD <7%) at Phyra. The limits of detection for AMPA were 26.7 ?g kg?1 (RSD <10%) at Kirchberg, 25.2 ?g kg?1 (RSD <10%) at Pixendorf, and 120.3 ?g kg?1 (RSD <9%) at Phyra. Accordingly, the limits of quantification were 22.7 ?g kg?1(RSD <5%) for glyphosate, and 88.9 ?g kg?1 (RSD <2%) for AMPA at Kirchberg and respectively 14.4 ?g kg?1 (RSD <6%) and 84 ?g kg?1 (RSD <5%) at Pixendorf and 13.8 ?g kg?1 (RSD <6%) and 87.2 ?g kg?1 (RSD <8%) at Phyra. Both substances in the soils were lower than the LOQ before applying the herbicide Roundup. The influence of higher contents of iron oxides, clay, and acidic pH, resulting in a more pronounced adsorption of glyphosate and AMPA in the soils of Phyra and Kirchberg, is demonstrated.


DOI: 10.1080/15320383.2013.726296

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