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Eliminating and inhibiting hydroxylamine oxidation in DEPMPO spin trapping experiments

机译:消除和抑制DEPMPO旋转捕集实验中的羟胺氧化

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摘要

There exists hydroxylamine impurity in 5-(diethoxyphosphoryl)-5-methyl-1-pyrroline-1-oxide (DEPMPO) despite the purification by column separation and molecular distillation. Slow oxidation of hydroxylamine impurity to nitroxide is caused by a trace amount of transition metal ions in the solution instead by oxygen, and it can be conveniently inhibited upon the addition of diethylenetriaminepentaacetic acid, a transition metal ion chelator. Hydroxylamine impurity in DEPMPO can also be oxidized to electron spin resonance detectable paramagnetic nitroxide in the presence of mild oxidants, such as K3Fe(CN)(6) and CuSO4. The previously recommended procedure for elimination of hydroxylamines was further simplified in the present study. Both hydroxylamine and nitroxide impurities can be removed from the aqueous solution of DEPMPO by activated charcoal treatment.
机译:尽管通过柱分离和分子蒸馏进行了纯化,但是5-(二乙氧基磷酰基)-5-甲基-1-吡咯啉-1-氧化物(DEPMPO)中仍存在羟胺杂质。溶液中的痕量过渡金属离子代替氧气可导致羟胺杂质缓慢氧化为亚硝酸盐,添加二亚乙基三胺五乙酸(一种过渡金属离子螯合剂)可方便地抑制羟胺杂质氧化为亚硝酸盐。在存在轻度氧化剂(例如K3Fe(CN)(6)和CuSO4)的情况下,DEPMPO中的羟胺杂质也可被氧化成电子自旋共振可检测的顺磁性氮氧化物。本研究进一步简化了先前推荐的消除羟胺的程序。可以通过活性炭处理从DEPMPO水溶液中除去羟胺和氮氧化物杂质。

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