Henan International Joint Laboratory of Medicinal Plants Utilization, College of Chemistry and Chemical Engineering, Henan University, Kaifeng, 475004, Henan, China.
Center for Multi-Omics Research, State Key Laboratory of Cotton Biology, Institute of Plant Stress Biology, Henan University, Kaifeng, 475004, Henan, China.
Mikrochim Acta. 2020 Jun 3;187(6):367. doi: 10.1007/s00604-020-04326-3.
The monodispersed mesoporous SiO@metal-organic framework (MSN@MIL-101(Fe)) composites were prepared by grafting MSN-NH onto MIL-101(Fe) particles with a solvothermal method. The adsorption ability of the composites was greatly improved compared to that of pristine MSNs or MIL-101(Fe) for phytohormones (Phys). The MSN@MIL-101(Fe) composites were characterized by scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, energy dispersive spectrometer, and mapping analysis. Using MSN@MIL-101(Fe) composites as sorbent, a dispersive solid-phase extraction procedure (dSPE) was developed to extract three endogenous Phys (abscisic acid (ABA), indole-3-aceticacid (IAA), and indole-3-butyric acid (IBA)) and two exogenous Phys (1-naphthylacetic acid (1-NAA) and 2-naphthylacetic acid (2-NAA)) prior to HPLC-DAD analysis. The experimental parameters including sample volume, sorbent amount, adsorption time, adsorption pH, desorption time, and desorption solvent on extraction efficiency were optimized and evaluated. Under optimized conditions, the working range of 0.08 to 0.45 ng mL with enrichment factors from 144 to 207 were achieved. The linear range is 0.75-200 ng mL for IAA, 0.20-200 ng mL for ABA, and 1.0-200 ng mL for IBA, 1-NAA, and 2-NAA. With MSN@MIL-101(Fe) as sorbent for extraction of Phys and determination by HPLC-DAD, two endogenous Phys (IAA and ABA) were detected from mung bean sprouts which were made in a laboratory, and the results were further confirmed by high-resolution mass spectrometry. The composites can be applied to extract other small molecules, which have similar chemical structures with Phys in biological, environmental, and food samples. Graphical abstract Schematic presentation of a dispersive solid-phase extraction using monodispersed mesoporous SiO@metal-organic framework composites (MSNs@MIL-101(Fe)) as the sorbent for extraction, clean-up, and preconcentration of phytohormones in mung bean sprouts prior to HPLC-DAD analysis.
介孔硅@金属有机骨架（MSN@MIL-101(Fe)）复合材料通过溶剂热法将 MSN-NH 接枝到 MIL-101(Fe)颗粒上制备而成。与原始 MSNs 或 MIL-101(Fe)相比，该复合材料对植物激素（Phys）的吸附能力有了很大的提高。通过扫描电子显微镜、透射电子显微镜、傅里叶变换红外光谱、X 射线衍射、能谱仪和映射分析对 MSN@MIL-101(Fe)复合材料进行了表征。使用 MSN@MIL-101(Fe)复合材料作为吸附剂，建立了一种分散固相萃取（dSPE）程序，用于提取三种内源性 Phys（脱落酸（ABA）、吲哚-3-乙酸（IAA）和吲哚-3-丁酸（IBA））和两种外源性 Phys（1-萘乙酸（1-NAA）和 2-萘乙酸（2-NAA）），然后进行 HPLC-DAD 分析。对萃取效率的实验参数（样品体积、吸附剂用量、吸附时间、吸附 pH 值、解吸时间和解吸溶剂）进行了优化和评估。在优化条件下，可实现 0.08-0.45ng mL 的工作范围，富集因子为 144-207。IAA 的线性范围为 0.75-200ng mL，ABA 的线性范围为 0.20-200ng mL，IBA、1-NAA 和 2-NAA 的线性范围为 1.0-200ng mL。以 MSN@MIL-101(Fe)为吸附剂，通过 HPLC-DAD 对 Phys 进行提取和测定，从实验室制作的绿豆芽中检测到两种内源性 Phys（IAA 和 ABA），并用高分辨率质谱进一步证实。该复合材料可用于提取生物、环境和食品样品中具有类似化学结构的其他小分子。
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