Departamento de Química Agrícola, Facultad de Ciencias, Universidad Autónoma de Madrid, 28049 Madrid, Spain.
J Agric Food Chem. 2011 Dec 28;59(24):13110-6. doi: 10.1021/jf203602a. Epub 2011 Nov 23.
The application of nuclear magnetic resonance (NMR) for the quality control of fertilizers based on Fe(3+), Mn(2+), and Cu(2+) chelates and complexes is precluded by the strong paramagnetism of metals. Recently, a method based on the use of ferrocyanide has been described to remove iron from commercial iron chelates based on the o,o-EDDHA [ethylenediamine-N,N'bis(2-hydroxyphenylacetic)acid] chelating agent for their analysis and quantification by NMR. The present work extended that procedure to other paramagnetic ions, manganese and copper, and other chelating, EDTA (ethylenediaminetetraacetic acid), IDHA [N-(1,2-dicarboxyethyl)-d,l-aspartic acid], and complexing agents, gluconate and heptagluconate. Results showed that the removal of the paramagnetic ions was complete, allowing us to obtain (1)H NMR spectra characterized by narrow peaks. The quantification of the ligands by NMR and high-performance liquid chromatography showed that their complete recovery was granted. The NMR analysis enabled detection and quantification of unknown impurities without the need of pure compounds as internal standards.
基于 Fe(3+)、Mn(2+) 和 Cu(2+)螯合物和配合物的磁性,应用核磁共振(NMR)对肥料进行质量控制受到限制。最近,描述了一种基于使用亚铁氰化物的方法,用于从基于 o,o-EDDHA(乙二胺-N,N'-双(2-羟基苯基乙酸))螯合剂的商业铁螯合物中去除铁,以便通过 NMR 进行分析和定量。本工作将该方法扩展到其他顺磁性离子(锰和铜)以及其他螯合剂、EDTA(乙二胺四乙酸)、IDHA[N-(1,2-二羧基乙基)-d,l-天冬氨酸]和络合剂、葡萄糖酸盐和七葡萄糖酸盐。结果表明,顺磁性离子的去除是完全的,这使我们能够获得特征峰较窄的 (1)H NMR 光谱。通过 NMR 和高效液相色谱对配体进行定量,表明它们得到了完全回收。NMR 分析无需使用纯化合物作为内标即可检测和定量未知杂质。