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Determination of benzimidazole anthelmintics in milk and honey by monolithic fiber-based solid-phase microextraction combined with high-performance liquid chromatography-diode array detection

机译:整体纤维基固相微萃取-高效液相色谱-二极管阵列检测法测定牛奶和蜂蜜中的苯并咪唑驱虫药

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摘要

A porous poly(methacrylic acid-co-ethylene dimethacrylate) monolithic fiber (MEMF) for solid-phase microextraction (SPME) of five benzimidazole anthelmintics was prepared by in-situ polymerization. The effect of polymerization conditions on SPME of the target analytes was studied thoroughly. The physicochemical properties of the monolith were characterized by infrared spectroscopy, elemental analysis, scanning electron microscopy, and mercury intrusion porosimetry. Several conditions affecting the extraction efficiency were investigated and, under the optimized conditions, a simple and sensitive method for the determination of trace benzimidazoles residues in milk and honey was established by coupling MEMF-SPME with high-performance liquid chromatography-diode array detection (MEMF-SPME-HPLC-DAD). Under the optimum experimental conditions, the limits of detection (S/N = 3) of the method were 0.11-0.30 mu g L-1 for milk and 0.086-0.28 mu g L-1 for honey. Evaluation of intra-day and inter-day precision showed reproducibility was satisfactory-relative standard deviations (RSD) for both were < 10 %. Finally, the method was successfully used for determination of benzimidazole residues in milk and honey. Recoveries obtained for determination of benzimidazole anthelmintics in spiked samples ranged from 72.3 to 121 %, with RSD always < 11 %.
机译:通过原位聚合制备了五种苯并咪唑类驱虫药的固相微萃取(SPME)用多孔聚(甲基丙烯酸-乙二甲基丙烯酸乙酯)共聚物单片纤维(MEMF)。深入研究了聚合条件对目标分析物SPME的影响。通过红外光谱,元素分析,扫描电子显微镜和压汞法测定了整料的理化性质。研究了几种影响萃取效率的条件,并在优化条件下,通过将MEMF-SPME与高效液相色谱-二极管阵列检测(MEMF)结合,建立了测定牛奶和蜂蜜中痕量苯并咪唑残留量的简单而灵敏的方法。 -SPME-HPLC-DAD)。在最佳实验条件下,该方法的检出限(S / N = 3)对于牛奶为0.11-0.30μg L-1,对于蜂蜜为0.086-0.28μgL-1。日内和日间精度的评估表明,两者的重现性均令人满意,相对标准偏差(RSD)均<10%。最终,该方法成功用于牛奶和蜂蜜中苯并咪唑的残留量测定。测定加标样品中苯并咪唑驱虫药的回收率范围为72.3%至121%,RSD总是<11%。

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