Henan International Joint Laboratory of Medicinal Plants Utilization, College of Chemistry and Chemical Engineering, Henan University, Kaifeng, 475004, Henan, China.
State Key Laboratory of Environmental and Biological Analysis, Department of Chemistry, Hong Kong Baptist University, Hong Kong, SAR, China.
Mikrochim Acta. 2021 Sep 14;188(10):340. doi: 10.1007/s00604-021-04993-w.
Using MIL-101(Fe) as the source of carbon and Fe, a magnetic porous carbon (MPC) material with FeC nanoparticles encapsulated in porous carbon was prepared through one-pot pyrolysis under N 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 (R ≥ 0.9938) and detection limits (0.02-0.04 ng mL) 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. Schematic presentation of a stir bar sorptive-dispersive microextraction (SBSDME) by using magnetic porous carbon (MPC) composites as sorbent combined with high-performance liquid chromatography for sensitive analysis of sulfonamides in milk and lake water samples.
以 MIL-101(Fe) 为碳源和铁源，在氮气气氛下通过一步热解制备了一种磁性多孔碳（MPC）材料，该材料将 FeC 纳米颗粒封装在多孔碳中。以 MPC 为吸附材料，提出了一种搅拌棒吸附分散微萃取（SBSDME）方法，用于在 HPLC-DAD 测定前提取和预浓缩磺胺类药物（SAs）。为了研究它们的萃取能力，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 SAs 表现出最高的萃取能力。还通过拉曼光谱、扫描电子显微镜、X 射线光电子能谱、动电位等技术对所制备的 MPC 材料进行了表征。系统研究了影响萃取的主要参数。在最佳条件下，磺胺类药物获得了良好的线性（R≥0.9938）和检测限（0.02-0.04ng mL）。牛奶和湖水样品中磺胺类药物的平均回收率在 76.9%至 109%之间，相对标准偏差（RSD）在 3.10%至 9.63%之间；在 75.4%至 118%之间，RSD 在 1.71%至 11.3%之间。在牛奶样品中检测到磺胺间甲氧嘧啶和磺胺异噁唑。在湖水样品中检测到磺胺异噁唑。MPC-900 材料表现出优异的可重复使用性。它可以重复使用 24 次，峰面积没有明显下降。该方法可用于提取复杂样品基质中超痕量化合物。在牛奶和湖水样品中，用磁性多孔碳（MPC）复合材料作为吸附剂的搅拌棒吸附分散微萃取（SBSDME）与高效液相色谱法相结合，用于磺胺类药物的灵敏分析示意图。
