Abstract
Solid-phase extraction in combination with large-volume sample stacking-capillary electrophoresis (SPE-LVSS-CE) was applied to measure chlortetracycline, doxycycline, oxytetracycline, and tetracycline in milk samples. Under optimal conditions, the proposed method had a linear range of 29 to 200 µg·L−1, with limits of detection ranging from 18.6 to 23.8 µg·L−1 with inter- and intraday repeatabilities < 10% (as a relative standard deviation) in all cases. The enrichment factors obtained were from 50.33 to 70.85 for all the TCs compared with a conventional capillary zone electrophoresis (CZE). This method is adequate to analyze tetracyclines below the most restrictive established maximum residue limits. The proposed method was employed in the analysis of 15 milk samples from different brands. Two of the tested samples were positive for the presence of oxytetracycline with concentrations of 95 and 126 µg·L−1. SPE-LVSS-CE is a robust, easy, and efficient strategy for online preconcentration of tetracycline residues in complex matrices.
Highlights
Preconcentration methods are an important tool for sample preparation because they enrich analytes in a liquid or solid sample. is improves analytical sensitivity, with the additional advantage of removing interferences [1]
The proposed method had a linear range of 29 to 200 μg·L−1, with limits of detection ranging from 18.6 to 23.8 μg·L−1 with inter- and intraday repeatabilities < 10% in all cases. e enrichment factors obtained were from 50.33 to 70.85 for all the TCs compared with a conventional capillary zone electrophoresis (CZE). is method is adequate to analyze tetracyclines below the most restrictive established maximum residue limits. e proposed method was employed in the analysis of 15 milk samples from different brands
Samples treated by solid-phase extraction (SPE) were introduced by hydrodynamic injection at 5 psi for 180 s. e capillary was set in background electrolyte (BGE) vials, and a potential of 12 kV was applied for 120 s to preconcentrate TCs at the inlet, while water and other ions were removed from the capillary
Summary
Solid-phase extraction in combination with large-volume sample stacking-capillary electrophoresis (SPE-LVSS-CE) was applied to measure chlortetracycline, doxycycline, oxytetracycline, and tetracycline in milk samples. The proposed method had a linear range of 29 to 200 μg·L−1, with limits of detection ranging from 18.6 to 23.8 μg·L−1 with inter- and intraday repeatabilities < 10% (as a relative standard deviation) in all cases. Is method is adequate to analyze tetracyclines below the most restrictive established maximum residue limits. E proposed method was employed in the analysis of 15 milk samples from different brands. Two of the tested samples were positive for the presence of oxytetracycline with concentrations of 95 and 126 μg·L−1. SPE-LVSS-CE is a robust, easy, and efficient strategy for online preconcentration of tetracycline residues in complex matrices
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