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使用磁性Co/NCHP/LDH纳米复合材料从牛奶样品中磁分散微固相萃取黄曲霉毒素M1

Magnetic dispersive µ-solid phase extraction of aflatoxin M1 from milk samples using magnetic Co/NCHP/LDH nanocomposite.

作者信息

Shirani Mahboube, Salamat Qamar, Payam Mahtab Rezaei, Sepahi Soheila, Soylak Mustafa

机构信息

Department of Chemistry, Faculty of Science, University of Jiroft, Jiroft, P.O. Box 7867161167, Iran.

Department of Chemistry, Faculty of Sciences, Erciyes University, Kayseri, Turkey.

出版信息

J Chromatogr A. 2025 Aug 30;1757:466139. doi: 10.1016/j.chroma.2025.466139. Epub 2025 Jun 17.

Abstract

A novel magnetic adsorbent composed of cobalt/nitrogen-doped carbon nanohybrid particles/ZIF-8/ZIF-67 nanoparticles/layered double hydroxides was synthesized and applied for preconcentration and determination of aflatoxin M1 in different milk samples using a magnetic dispersive µSPE approach followed by high-performance liquid chromatography-florescence detection (HPLC-FLD). The synthesized adsorbent was then characterized using Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDX) techniques. The affective parameters, including pH, the adsorbent dosage, ionic strength, sample volume, and desorption conditions, were studied using a matrix-matched method. The linearity of 0.5-2000 ng Kg, the detection limit of 0.14 ng Kg, and the quantification limit of 0.45 ng Kg were obtained. The intra-day (n = 6) and inter-day (5 days, n = 3) precisions were acquired at ≤3.3 % and ≤3.3 %, respectively, in which the results confirmed satisfactory reproducibility and repeatability. The relative recoveries (%) of 91.0- 99.0 were obtained with RSDs (%) ≤3.1 (n = 3).

摘要

合成了一种由钴/氮掺杂碳纳米杂化颗粒/沸石咪唑酯骨架材料-8/沸石咪唑酯骨架材料-67纳米颗粒/层状双氢氧化物组成的新型磁性吸附剂,并采用磁分散微固相萃取方法结合高效液相色谱-荧光检测(HPLC-FLD),将其应用于不同牛奶样品中黄曲霉毒素M1的预富集和测定。然后,使用傅里叶变换红外光谱(FTIR)、X射线衍射(XRD)、扫描电子显微镜(SEM)和能量色散X射线光谱(EDX)技术对合成的吸附剂进行表征。采用基质匹配法研究了包括pH值、吸附剂用量、离子强度、样品体积和解吸条件在内的影响参数。获得了0.5-2000 ng Kg的线性范围、0.14 ng Kg的检出限和0.45 ng Kg的定量限。日内(n = 6)和日间(5天,n = 3)精密度分别≤3.3%和≤3.3%,结果证实具有令人满意的重现性和重复性。相对回收率(%)为91.0-99.0,相对标准偏差(%)≤3.1(n = 3)。

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