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Ion-pair chromatographic separation of water-soluble gold monolayer-protected clusters

机译:水溶性金单层保护簇的离子对色谱分离

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We demonstrate the efficacy of ion-pair chromatography for separations of samples of charged, polydisperse, water-soluble gold nanoparticles protected by monolayers of N-acetyl-L-cysteine and of tiopronin ligands. These nanoparticle mixtures have 1-2-nm-diameter Au core sizes as estimated from UV-visible spectra of the separated components. This size range encompasses the transition from bulk metal to molecular properties. The nanoparticle mixtures were resolved, the smallest nanoparticles eluting first, on an octadecylsilyl (C18) column using isocratic elution with a methanol/water mobile phase containing tetrabutylammonium fluoride (Bu4N+F-) and phosphate buffer. The column retention increases with Bu4N+F- concentration, lowered pH, and decreasing methanol volume fraction. The retention mechanism is dominated by ion-pairing in either the mobile phase or at the stationary/mobile-phase interface. Size exclusion effects, used in many previous nanoparticle separations, are insignificant.
机译:我们证明了离子对色谱法用于分离带电,多分散,水溶性金纳米颗粒样品的功效,该纳米颗粒受N-乙酰基-L-半胱氨酸和硫普罗宁配体的单层保护。这些纳米颗粒混合物具有从分离的组分的UV-可见光谱估计的1-2nm直径的Au核尺寸。该尺寸范围包括从块状金属到分子性质的过渡。纳米颗粒混合物在十八烷基甲硅烷基(C18)色谱柱上进行分离,首先洗脱出最小的纳米颗粒,使用含有氟化四丁基铵(Bu4N + F-)和磷酸盐缓冲液的甲醇/水流动相进行等度洗脱。色谱柱保留度随Bu4N + F-浓度增加,pH降低和甲醇体积分数降低而增加。在流动相中或在固定相/流动相界面处,离子对都是对固位机理的主导。在许多先前的纳米颗粒分离中使用的尺寸排阻效应微不足道。

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