A High‑Throughput, Non‐Derivatization Method for Determination of Glyphosate, Glufosinate, and Their Metabolites in Water and Sediments Using Pass‐Through Cleanup and UHPLC–MS/MS

ABSTRACT

Glyphosate (GLYP) and glufosinate (GLUF) are widely used herbicides that can persist in aquatic environments. Rapid, sensitive, and matrix‐versatile analytical methods for the simultaneous monitoring of these herbicides, along with their major metabolites (aminomethylphosphonic acid: AMPA, and 3‐(methyl‐phosphinico)‐propionic acid: MPPA), remain limited. Most existing liquid chromatography‐tandem mass spectrometry (LC–MS/MS) methods require derivatization or target only food matrices, with little attention to environmental water and sediment. In this study, we developed a high‐throughput, non‐derivatization ultra‐high‐performance LC (UHPLC)–MS/MS method incorporating solid‐phase extraction using Oasis PRiME HLB cartridges to directly determine all four analytes in both water and sediment samples. The PRiME HLB cartridge effectively reduces interfering substances (such as salts, organic matter, and phospholipids) without conditioning or elution steps, thereby simplifying sample preparation and enabling high‐throughput analysis. The method was validated across six distinct environmental matrices (pond, lake, river water, and corresponding sediments). Excellent linearity ( R ² > 0.996), satisfactory recoveries (78.3%–104.7%), precision (RSD < 15%), and sensitivity (limits of detection [LODs]: 0.3–0.5 µg L ^{− 1} for water and 2–3 µg kg ^{− 1} for sediment) were achieved, with negligible matrix effects (<20%). Applied to 60 real environmental samples, the method detected GLYP and AMPA residues in sediments (up to 15.6 and 45.4 µg kg ^{− 1} , respectively), while GLUF and MPPA were below LODs. This simple, robust, and high‐throughput workflow is well suited for routine monitoring of herbicide residues in aquatic systems.