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肉类样品中磺胺类药物的测定:一种磁性介孔金属有机框架作为用于磁性固相萃取结合高效液相色谱的高效吸附剂

Towards the determination of sulfonamides in meat samples: A magnetic and mesoporous metal-organic framework as an efficient sorbent for magnetic solid phase extraction combined with high-performance liquid chromatography.

作者信息

Xia Lian, Liu Lijie, Lv Xiaoxia, Qu Fei, Li Guoliang, You Jinmao

机构信息

Key Laboratory of Life-Organic Analysis of Shandong Province, Qufu Normal University, Qufu, PR China.

Key Laboratory of Life-Organic Analysis of Shandong Province, Qufu Normal University, Qufu, PR China.

出版信息

J Chromatogr A. 2017 Jun 2;1500:24-31. doi: 10.1016/j.chroma.2017.04.004. Epub 2017 Apr 4.

Abstract

A magnetic, mesoporous core/shell structured FeO@JUC-48 nanocomposite was synthesized and employed as a magnetic solid phase extraction (MSPE) sorbent for the determination of trace sulfonamides (SAs) in meat samples. The synthesized nanocomposite was characterized by X-ray diffraction, Fourier transform infrared spectra, transmission electron microscopy, scanning electron microscopy, Brunner-Emmet-Teller, and vibrating sample magnetometry; the FeO@JUC-48 nanocomposite exhibited a distinctive morphology, large surface area, high magnetism, open adsorption sites, and high chemical stability. By combining the optimized MSPE conditions with high performance liquid chromatography diode array detection, an accurate and sensitive method for the determination of 5 SAs, including sulfadiazine (SDZ), sulfathiazole (STZ), sulfamerazine (SMR), sulfamethazine (SMZ), and sulfamethoxypyridazine (SMP), was developed. The method exhibited good linearity in the range of 3.97-1000ng/g with R ranging from 0.9991 to 0.9994, high sensitivity with LODs ranging from 1.73 to 5.23ng/g, adequate recoveries between 76.1 and 102.6% with low relative standard deviations ranging from 2.1 to 6.4%, and high precision with RSD<4.5%. The FeO@JUC-48 magnetic nanocomposite is a promising sorbent for the rapid and efficient extraction of SAs from complex biological samples such as chicken, pork, and shrimp.

摘要

合成了一种磁性介孔核壳结构的FeO@JUC-48纳米复合材料,并将其用作磁性固相萃取(MSPE)吸附剂,用于测定肉类样品中的痕量磺胺类药物(SAs)。通过X射线衍射、傅里叶变换红外光谱、透射电子显微镜、扫描电子显微镜、Brunner-Emmet-Teller和振动样品磁强计对合成的纳米复合材料进行了表征;FeO@JUC-48纳米复合材料具有独特的形态、大表面积、高磁性、开放的吸附位点和高化学稳定性。将优化的MSPE条件与高效液相色谱二极管阵列检测相结合,建立了一种准确、灵敏的方法,用于测定5种SAs,包括磺胺嘧啶(SDZ)、磺胺噻唑(STZ)、磺胺甲嘧啶(SMR)、磺胺二甲嘧啶(SMZ)和磺胺甲氧嗪(SMP)。该方法在3.97-1000ng/g范围内具有良好的线性,相关系数R在0.9991至0.9994之间,具有高灵敏度,检测限在1.73至5.23ng/g之间,回收率在76.1%至102.6%之间,相对标准偏差较低,在2.1%至6.4%之间,精密度高,相对标准偏差<4.5%。FeO@JUC-48磁性纳米复合材料是一种有前景的吸附剂,可用于从鸡肉、猪肉和虾等复杂生物样品中快速高效地提取SAs。

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