State Key Laboratory for Managing Biotic and Chemical Threats to the Quality and Safety of Agro-products, State Key Laboratory Base of Novel Functional Materials and Preparation Science, School of Materials Science & Chemical Engineering, Ningbo University, Ningbo, Zhejiang 315211, China.
State Key Laboratory for Managing Biotic and Chemical Threats to the Quality and Safety of Agro-products, State Key Laboratory Base of Novel Functional Materials and Preparation Science, School of Materials Science & Chemical Engineering, Ningbo University, Ningbo, Zhejiang 315211, China.
J Chromatogr A. 2022 Jul 19;1675:463184. doi: 10.1016/j.chroma.2022.463184. Epub 2022 May 31.
Magnetic polyimide nanosheet microspheres (PI-NMs) were used for magnetic solid-phase extraction (MSPE) for the first time. The PI-NMs were modified with magnetic FeO nanoparticles by chemical coprecipitation to produce the PI-NM/FeO composite. The prepared composite possessed a nanosheet structure, large specific surface area (71.5 m/g), high saturation magnetization (19.1 emu/g), large adsorption capacity (≥ 676 ng/mg for selected estrogens), and good extraction stability (> 10 times). Trace estrogens in environmental water and urine samples were extracted by the PI-NM/FeO composite, desorbed, derivatized, and analyzed by gas chromatography-mass spectrometry (GC-MS). The derivatization, extraction, and desorption conditions were optimized. Extraction equilibrium was achieved within 1 min due to the good dispersibility and large specific surface area of the PI-NM/FeO composite. Under the optimized conditions, the MSPE/GC-MS method validation results showed wide linearity (0.02-50 µg/L or 0.05-50 µg/L), high determination coefficients (R ≥ 0.9983), good intraday and interday precisions (expressed as relative standard deviation, RSDs ≤ 8.2%), and low limits of detection (LODs, 0.001-0.015 µg/L). For the real environmental water and urine samples, the recoveries and RSDs were 77.0-112.5% and 0.1-10.7%, respectively. The performance of the MSPE/GC-MS method proved that the PI-NM/FeO composite was a good alternative material for the extraction of organic pollutants in aqueous samples.
磁性聚酰亚胺纳米片微球（PI-NMs）首次被用于磁性固相萃取（MSPE）。通过化学共沉淀法将 PI-NMs 修饰上磁性 FeO 纳米颗粒，得到 PI-NM/FeO 复合材料。所制备的复合材料具有纳米片结构、大比表面积（71.5 m/g）、高饱和磁化强度（19.1 emu/g）、大吸附容量（≥676ng/mg 用于选择的雌激素）和良好的萃取稳定性（>10 次）。采用 PI-NM/FeO 复合材料萃取环境水样和尿样中的痕量雌激素，然后解吸、衍生化，并用气相色谱-质谱联用仪（GC-MS）进行分析。对衍生化、萃取和洗脱条件进行了优化。由于 PI-NM/FeO 复合材料良好的分散性和大的比表面积，萃取平衡在 1 分钟内达到。在优化条件下，MSPE/GC-MS 方法验证结果表明具有较宽的线性范围（0.02-50 µg/L 或 0.05-50 µg/L）、高测定系数（R≥0.9983）、良好的日内和日间精密度（表示为相对标准偏差，RSDs≤8.2%）和低检出限（LODs，0.001-0.015 µg/L）。对于实际环境水样和尿样，回收率和 RSDs 分别为 77.0-112.5%和 0.1-10.7%。MSPE/GC-MS 方法的性能证明，PI-NM/FeO 复合材料是萃取水样中有机污染物的一种良好替代材料。
