Determination of glyphosate and glufosinate in corn using multi-walled carbon nanotubes followed by ultra high performance liquid chromatography coupled with tandem mass spectrometry.

Glyphosate (Glyp) and glufosinate (Gluf) are widely used herbicides around the world, and their effects on human health and detection of levels have drawn increasing attention. The present study was to establish a method to determine the contents of Glyp and Gluf from corn using multi-walled carbon nanotubes (MWCNTs) followed by ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). The corn samples were purified by MWCNTs, then the analytes reacted with 9-fluorenylmethylchloroformate (FMOCCl) of acetonitrile solution (20.0 g/L) at 50 °C water bath in a borate buffer solution (50.0 g/L, pH=9) to generate FMOC derivative products. After the derivatization, HSS T3 was used as the separation column, with acetonitrile and 0.05% ammonia as the mobile phase, and multiple reaction monitoring (MRM) mode with negative electrospray ionization (ESI-) was adopted. The validation parameters showed good verification results, with both of their quantitative limits (LOQ) as 0.005 mg/kg, recoveries between 90.3% and 95.4%, intra-day relative standard deviations (RSDs) in the ranges of 1.24% and 3.35%, and inter-day RSDs between 3.56% and 6.06%. The analytical method, developed in this study, has high accuracy and sensitivity, and is suitable for the simultaneous detection of Glyp and Gluf in corn.