Influence of different hydrophilic interaction liquid chromatography stationary phases on method performance for the determination of highly polar anionic pesticides in complex feed matrices

Abstract

Hydrophilic interaction liquid chromatography is an alternative liquid chromatography mode for separation of polar compounds. In the recent years, this liquid chromatography mode has been recognized as an important solution for the analysis of compounds not amenable to reverse phase chromatography. In this work, we evaluated three different hydrophilic liquid chromatography stationary phases for the determination of 14 highly polar anionic molecules including pesticides such as glyphosate, glufosinate, ethephon and fosetyl, their main metabolites, and bromide, chlorate, and perchlorate. Several mobile phase compositions were evaluated combined with different gradients for the chromatographic run. The two columns that presented the best results were used to assess the performance for the determination of the 14 compounds in challenging highly complex feed materials. Very different matrix effects were observed for most of the compounds in each column, suggesting that different interactions can occur. Using isotopically labeled internal standards, acceptable quantitative performance and identification could be achieved down to 0.02 mg kg−1 (the lowest level tested) for most compounds. While one column was found to be favorable in terms of scope (suited for all 14 compounds), the other one was more suited for quantification and identification at lower levels, however, not for all analytes tested.

Capillary electrophoresis applied for the determination of acidity constants and limiting electrophoretic mobilities of ionizable herbicides including glyphosate and its metabolites and for their simultaneous separation

“…In comparison, when analyzing water samples, a non‐derivatization normal phase LC‐MS method with SPE pretreatment achieved LOQs in the range of 20 ng/L for glyphosate, glufosinate, and AMPA [38]. HILIC‐LC‐MS methods showed LOQs of 20 μg/kg for glyphosate and some of its degradation products in peas and soya cake [39].…”

Characterization of a highly stable zwitterionic hydrophilic interaction chromatography stationary phase based on hybrid organic–inorganic particles

“…The combination of high retentivity and a net-zero surface charge has made sulfobetaine columns a popular choice for a wide range of applications, including metabolomics [18], cell culture media analysis [19], pharmaceutical bioanalysis and impurity profiling [20,21], determination of the concentrations of toxins in food [22][23][24], and analyses of biopolymers including peptides [25,26], glycoproteins [26], and oligonucleotides [27]. Most of the commercially available sulfobetaine stationary phases are based on silica particles.…”

“…Sulfobetaine stationary phases have been shown to accumulate a relatively thick layer of adsorbed water [14–17], which makes them strongly retentive for polar neutrals in HILIC. The combination of high retentivity and a net‐zero surface charge has made sulfobetaine columns a popular choice for a wide range of applications, including metabolomics [18], cell culture media analysis [19], pharmaceutical bioanalysis and impurity profiling [20,21], determination of the concentrations of toxins in food [22–24], and analyses of biopolymers including peptides [25,26], glycoproteins [26], and oligonucleotides [27].…”

Development of a Quantitative Method for Detection of Multiclass Veterinary Drugs in Feed Using Modified QuPPe Extraction and LC–MS/MS

“…In the last few years, analysis methods for residual polar compounds, including veterinary drugs in food and feed, have been continuously studied. For example, the liquid chromatography–electrospray ionization–tandem mass spectrometry (LC–ESI–MS/MS), or a combination of hydrophilic interaction liquid chromatography (HILIC) with MS, can be used in the analysis and identification of compounds even at low concentration levels [ 4 , 11 , 12 , 13 , 14 , 15 ]. In addition, methods for extracting polar compounds, including veterinary drugs, continue to be studied [ 7 , 13 ].…”