Catalysis-Based Fluorometric Method for Trace Palladium Detection with Improved Convenience,Organic Process Research & Development

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Catalysis-Based Fluorometric Method for Trace Palladium Detection with Improved Convenience
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2020-11-12 , DOI: 10.1021/acs.oprd.0c00377
Jessica M. Williams ₁ , Annelise K. Wanner ₁ , Kazunori Koide ₁

Affiliation

There is a need for rapid estimation of the quantities of trace palladium in synthetic samples. To address the need, we previously reported a rapid method based on the palladium-catalyzed conversion of nonfluorescent allyl resorufin ether to fluorescent resorufin in NH₄OAc buffer, which has been implemented in industry. The nuisance of the method is the need for NaBH₄, which cannot be stored in solution for more than half a day. Herein we report the development of a NaBH₄-free method; the reaction is faster in HEPES buffer than in NH₄OAc buffer. The resulting colorimetric/fluorometric method enjoys high sensitivity and a greater degree of metal selectivity and is compatible with many drug-like molecules, except those containing sulfur. Unlike the previous method, all of the assay solutions can be stored for weeks to months, potentially enabling more widespread use of the palladium detection method in the synthetic community.

中文翻译：

催化方便的痕量钯检测的荧光荧光法

需要快速估计合成样品中痕量钯的量。为了满足需求，我们先前报道了一种在NH ₄ OAc缓冲液中基于钯催化的非荧光烯丙基间苯二酚醚向荧光间苯二酚转化的快速方法，该方法已在工业中实施。该方法的麻烦之处在于需要NaBH ₄，而NaBH ₄不能在溶液中保存超过半天。在此，我们报告了无NaBH _4的方法的发展。HEPES缓冲液中的反应比NH _4中的反应更快OAc缓冲区。所得的比色/荧光法具有较高的灵敏度和较高的金属选择性，并且与除含有硫的分子外的许多类药物分子兼容。与以前的方法不同，所有化验溶液可以存储数周至数月，从而有可能在合成社区中更广泛地使用钯检测方法。

更新日期：2020-12-18

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