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基于整体纤维的固相微萃取结合高效液相色谱 - 二极管阵列检测法测定牛奶和蜂蜜中的苯并咪唑类驱虫药

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

作者信息

Zhang Yong, Huang Xiaojia, Yuan Dongxing

机构信息

State Key Laboratory of Marine Environmental Science, Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystem, College of the Environment and Ecology, Xiamen University, Xiamen, 361005, China.

出版信息

Anal Bioanal Chem. 2015 Jan;407(2):557-67. doi: 10.1007/s00216-014-8284-8. Epub 2014 Nov 19.

Abstract

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 μg L(-1) for milk and 0.086-0.28 μg 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 %.

摘要

通过原位聚合法制备了一种用于固相微萃取(SPME)5种苯并咪唑驱虫药的多孔聚(甲基丙烯酸 - 二甲基丙烯酸乙烯酯)整体纤维(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对整体材料的物理化学性质进行了表征。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 - SPME - HPLC - DAD)联用,建立了一种简单灵敏的测定牛奶和蜂蜜中痕量苯并咪唑残留量的方法。在最佳实验条件下,该方法对牛奶的检测限(S/N = 3)为0.11 - 0.30 μg L⁻¹,对蜂蜜为0.086 - 0.28 μg L⁻¹。日内和日间精密度评估表明重现性良好,两者的相对标准偏差(RSD)均<10%。最后,该方法成功用于牛奶和蜂蜜中苯并咪唑残留量的测定。加标样品中苯并咪唑驱虫药测定的回收率为72.3%至121%,RSD始终<11%。

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