磁性高交联聚苯乙烯-纳米Fe_3O_4的制备及其在牛奶中磺胺类药物检测中的应用

Magnetic solid phase extraction based on magnetic hypercrosslinked polystyrene for determination of sulfonamides in milk samples

制备了磁性超高交联聚苯乙烯（HCP）-纳米Fe3O4微球,作为固相萃取材料,对牛奶中的4种磺胺类药物：磺胺甲氧嗪、磺胺甲嘧啶、磺胺甲恶唑、磺胺氯哒嗪进行预富集处理后,经C18反相液相色谱柱分离,以乙腈-0.1%H3PO4溶液（20：80,V/V）为流动相进行洗脱检测。4种磺胺类药物在0.2~10 ng/m L范围内呈良好的线性关系,相关系数均不小于0.98,检出限为0.022~0.068 ng/m L,平均回收率为94%~105%,相对标准偏差为2.1%~4.3%。方法已用于实际样品中磺胺类药物的定量分析。

In this study,a novel magnetic solid-phase extraction（MSPE） sorbent,magnetic hypercrosslinked polystyrene（HCP-Fe3O4）, was prepared and used for preconcentration of four sulfonamides ：sulfamethoxypyridazine（SMP）,sulfamethazine（SMZ）,sulfamethoxazole（SMX） and sulfachloropyridazine（SCP） from milk samples. The milk samples were concentrated with magnetic polystyrene,then separated on a C18 analytical column using acetonitrile- 0. 1% H3PO4（20： 80,V/V） as mobile phase. The results showed that,under the optimal condition,good linearities for the sulfonamides were obtained between 0. 2 ~ 10 ng/m L with correlation coefficients not less than 0. 98. The limits of detection was 0. 022 ~ 0. 068 ng/m L. The spiked recoveries were between 94% ~ 105% with relative standard deviations of 2. 1 ~ 4. 3%. The developed method could be applied in the real samples.