Department of Analytical Chemistry and Pollutants, Shahid Beheshti University, Evin, Tehran, Iran.
Department of Analytical Chemistry and Pollutants, Shahid Beheshti University, Evin, Tehran, Iran.
J Chromatogr A. 2023 Sep 13;1706:464220. doi: 10.1016/j.chroma.2023.464220. Epub 2023 Jul 17.
In this work, for the first time, magnetic-phthalated maltodextrin nanosponges (M-PAMDNSs) were synthetized and introduced as efficient and green sorbents. The integration of phthaloyl groups as hydrophobic moieties into networks of maltodextrin nanosponges provided good enrichment for hypothalamic-related peptides (HRPs). The synthesized materials were characterized by H nuclear magnetic resonance spectroscopy, water contact angle, attenuated total reflection-Fourier transform infrared spectroscopy, dynamic light scattering, zeta potential, pH point of zero charge, acid-base titration, field-emission scanning electron microscopy, Brunauer-Emmett-Teller, and vibrating sample magnetometer. Under the optimized conditions (sorbent amount: 5.0 mg, desorption solvent volume and type: 300 µL of methanol: HO: trifluoroacetic acid, extraction time: 15 min, and desorption time: 10 min), the developed magnetic solid-phase extraction (MSPE) method in combination with HPLC-UV was used as a novel and sensitive analytical method for the determination of HRPs in plasma samples. The proposed MSPE-HPLC-UV method provided good linearity (1.5-500 ng mL R ≥ 0.9988), low limits of detection (0.1-0.2 ng mL) and quantification (0.4-0.8 ng mL), desirable precision (RSD ≤ 8.8%, n ₌ 5), satisfactory enrichment factor (EFs ≥ 66.0), and well relative recoveries (92.8-108.8%). Overall, the established method effectively expanded the analytical potential of MSPE approach for the quantification of HRPs in biological samples.
在这项工作中，首次合成了磁性酞化麦芽糊精纳米海绵（M-PAMDNSs），并将其作为高效、绿色的吸附剂进行了介绍。将疏水性的邻苯二甲酰基基团整合到麦芽糊精纳米海绵的网络中，为下丘脑相关肽（HRPs）提供了良好的富集效果。合成材料的特征通过氢核磁共振波谱、水接触角、衰减全反射傅里叶变换红外光谱、动态光散射、Zeta 电位、pH 值零点电荷、酸碱滴定、场发射扫描电子显微镜、Brunauer-Emmett-Teller 和振动样品磁强计进行了表征。在优化条件下（吸附剂用量：5.0mg，解吸溶剂体积和类型：300µL 甲醇：H₂O：三氟乙酸，萃取时间：15min，解吸时间：10min），开发的磁性固相萃取（MSPE）与 HPLC-UV 结合，作为一种新的、灵敏的分析方法，用于测定血浆样品中的 HRPs。所提出的 MSPE-HPLC-UV 方法提供了良好的线性（1.5-500ng mL R ≥ 0.9988）、低检测限（0.1-0.2ng mL）和定量限（0.4-0.8ng mL）、令人满意的精密度（RSD ≤ 8.8%，n = 5）、良好的富集因子（EFs ≥ 66.0）和相对回收率（92.8-108.8%）。总的来说，该方法有效地扩展了 MSPE 方法在生物样品中 HRPs 定量分析的分析潜力。
