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Determination of trace macrolide antibiotics in milk with online solid-phase extraction with an ionic-liquid-based monolithic column

机译:离子液体基整体柱在线固相萃取法测定牛奶中的痕量大环内酯类抗生素

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An ionic liquid (IL)-based monolithic poly(ionic liquid glycidylmethacrylate-co-ethylene glycol dimethacrylate) column was prepared via in situ free-radical polymerization with 1-vinyl-3-butylimidazolium chlorine as one of the comonomers. The obtained monolithic column was used as the sorbent of solid-phase extraction (SPE) and coupled with high-performance liquid chromatography for the simultaneous determination of the macrolide antibiotics roxithromycin (ROX) and acetylspiramycin (ACE) in processed pure milk. The monolithic column was characterized by Fourier transform infrared spectrometry, scanning electron microscopy, nitrogen absorption-desorption, mercury intrusion porosimetry, and thermogravimetric analysis. The results reveal that the monolithic column exhibited a high selectivity and good permeability to the macrolide antibiotics in milk. The optimized method offered excellent linearity with a linear regression coefficient greater than 0.998. The precisions for interday and intraday were both less than 7.7%. The accuracies expressed by the recoveries for ROX and ACE were in the ranges 92.5-103.8 and 93.0-107.6%, respectively. Compared to the previous methods, this method had a low limit of detection and a good accuracy. As a result, the polymer IL based monolithic column could feasibly be used as a high-selectivity online SPE sorbent for determining trace macrolide antibiotics in milk. (c) 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016, 133, 43943.
机译:通过以1-乙烯基-3-丁基咪唑鎓氯作为共聚单体之一通过原位自由基聚合制备基于离子液体(IL)的整体式聚(甲基丙烯酸缩水甘油酯-甲基丙烯酸乙二醇酯-共聚乙二醇)柱。所得整体柱用作固相萃取(SPE)的吸附剂,并与高效液相色谱法结合使用,可同时测定纯牛奶中大环内酯类抗生素罗红霉素(ROX)和乙酰螺旋霉素(ACE)。通过傅立叶变换红外光谱法,扫描电子显微镜,氮吸收-解吸,压汞法和热重分析法对整体柱进行了表征。结果表明,整体柱对牛奶中的大环内酯类抗生素表现出高选择性和良好的渗透性。优化的方法具有出色的线性度,线性回归系数大于0.998。盘中和盘中的精度均低于7.7%。 ROX和ACE的回收率所表示的准确度分别在92.5-103.8和93.0-107.6%之间。与以前的方法相比,该方法检测限低,准确度高。结果,基于聚合物IL的整体式色谱柱可以用作确定牛奶中痕量大环内酯类抗生素的高选择性在线SPE吸附剂。 (c)2016 Wiley Periodicals,Inc. J. Appl。 Polym。科学2016,133,43943。

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