Direct Extraction of Triazine Herbicides in Milk Samples by Macroporous Resin-Based Solid-Phase Extraction with High-Performance Liquid Chromatography
摘要
Triazines are widely utilized in agriculture to control weeds and have been found in food frequently, posing a risk to human health. The analysis of trace contaminants in milk samples generally involves the process of protein precipitation. In this work, a lab-made semi-automated solid-phase extraction (SPE) strategy was developed for the rapid extraction of six triazine herbicides in milk samples. Six triazines were directly extracted with macroporous resin-based SPE followed by high-performance liquid chromatography detection. Some parameters affecting the extraction efficiency, including the type and amount of macroporous resin, salt concentration, pH, flow rate, extraction time, type, and volume of elution solvent, were investigated and optimized. The working curves exhibited good linearity in the concentration range of 0.78–100.00 µg L−1 (R2 ≥ 0.9996). LODs and LOQs were in the range of 0.15–0.31 µg L−1 and 0.50–1.05 µg L−1, respectively. The relative standard deviations (RSDs) for intra-day and inter-day were 1.91–3.85% and 0.59–3.78%, respectively. The recoveries and RSDs for five spiked milk samples were 91.5–107.8% and 0.15–6.77%, respectively. The proposed method eliminated the commonly used protein precipitation procedure and could improve the sample throughput, which was a simple, efficient, and economical sample pretreatment with potential applications in complicated matrix pesticide residue analysis.