Abstract

Using MIL-101(Fe) as the source of carbon and Fe, a magnetic porous carbon (MPC) material with Fe₃C nanoparticles encapsulated in porous carbon was prepared through one-pot pyrolysis under N₂ atmosphere. With MPC as adsorption material, a stir bar sorptive-dispersive microextraction (SBSDME) method was proposed to extract and preconcentrate sulfonamides (SAs) prior to HPLC-DAD determination. To investigate their extraction ability, different MPC materials were prepared under different carbonization temperatures (600, 700, 800, 900, and 1000 °C). The material prepared under 900 °C (MPC-900) exhibited the highest extraction ability for SAs. The as-prepared MPC materials were also characterized by Raman spectroscopy, scanning electron microscopy, X-ray photoelectron spectroscopy, zeta potential, and other techniques. The main parameters that affect extraction were systematically studied. Under optimal conditions, favorable linearity (R² ≥ 0.9938) and detection limits (0.02–0.04 ng mL⁻¹) of sulfonamides were obtained. The average recoveries for spiked milk and lake water samples ranged from 76.9 to 109% and from 75.4 to 118% with RSDs of 3.10–9.63% and 1.71–11.3%, respectively. Sulfameter and sulfisoxazole were detected in milk sample. Sulfisoxazole was detected in the lake water sample. The MPC-900 material demonstrated excellent reusability. It can be reused 24 times with peak areas having no obvious decline. The method can be applied to extract ultra-trace compounds in complex sample matrices.

Graphical abstract

中文翻译：

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MIL-101(Fe)衍生的磁性多孔碳作为吸附剂，用于磺胺类的搅拌棒吸附分散微萃取

摘要

以MIL-101(Fe)为碳源和Fe源，在N ₂下通过一锅热解制备了Fe ₃ C纳米颗粒包裹在多孔碳中的磁性多孔碳(MPC)材料。大气层。以 MPC 作为吸附材料，提出了一种搅拌棒吸附分散微萃取 (SBSDME) 方法在 HPLC-DAD 测定之前提取和预浓缩磺胺 (SA)。为了研究它们的提取能力，在不同的碳化温度（600、700、800、900 和 1000 °C）下制备了不同的 MPC 材料。在 900 °C 下制备的材料 (MPC-900) 对 SA 表现出最高的提取能力。所制备的 MPC 材料还通过拉曼光谱、扫描电子显微镜、X 射线光电子能谱、zeta 电位和其他技术进行了表征。系统地研究了影响提取的主要参数。在最佳条件下，良好的线性 ( R ²  ≥ 0.9938) 和检测限 (0.02–0.04 ng mL^获得-1 )的磺胺。加标牛奶和湖水样品的平均回收率为 76.9% 至 109% 和 75.4% 至 118%，RSD 分别为 3.10-9.63% 和 1.71-11.3%。牛奶样品中检出磺胺计和磺胺异恶唑。在湖水样品中检测到磺胺异恶唑。MPC-900 材料表现出出色的可重用性。可重复使用24次，峰面积无明显下降。该方法可用于提取复杂样品基质中的超痕量化合物。

图形概要