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Third-Generation Method for High-Throughput Quantification of Trace Palladium by Color or Fluorescence
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2019-12-26 , DOI: 10.1021/acs.oprd.9b00472 Lydia Lukomski 1 , Ivanna Pohorilets 1 , Kazunori Koide 1
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2019-12-26 , DOI: 10.1021/acs.oprd.9b00472 Lydia Lukomski 1 , Ivanna Pohorilets 1 , Kazunori Koide 1
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Chemists frequently encounter problems associated with trace palladium in synthetic samples because palladium is widely used in synthetic organic chemistry. We previously reported a colorimetric method for trace palladium quantification, the only high-throughput method implemented in the pharmaceutical industry. However, slight changes from the published reaction conditions have caused reproducibility problems, with little understanding of underlying molecular mechanisms. In the current study, we took a combinatorial approach to investigate the method and found that excess NaOH was a culprit for the lack of reproducibility. We changed the reaction conditions and procedure accordingly, which substantially improved reproducibility. The reaction under current conditions followed Michaelis–Menten kinetics, allowing for predicting reaction rates on the basis of the substrate concentrations. The current method showed 57 and 72% average error, respectively, when drugs spiked with known amounts of palladium and synthetic samples with unknown amounts of palladium were analyzed. The trend of palladium concentrations determined by the current method boded well with actual palladium concentrations.
中文翻译：
彩色或荧光高通量定量痕量钯的第三代方法
化学家经常遇到与合成样品中痕量钯相关的问题，因为钯已广泛用于合成有机化学中。我们之前曾报道过用于痕量钯定量的比色法，这是制药行业中唯一实施的高通量方法。但是，与已公布的反应条件相比，微小的变化已导致了可再现性问题，而对基本的分子机理却知之甚少。在当前的研究中，我们采取了一种组合方法来研究该方法，发现过量的NaOH是缺乏可重复性的罪魁祸首。我们相应地改变了反应条件和步骤，从而大大提高了重现性。当前条件下的反应遵循迈克尔尼斯·门腾动力学，可以根据底物浓度预测反应速率。当分析掺有已知数量钯的药物和合成样品却含未知数量的钯时，当前方法分别显示出57％和72％的平均误差。通过当前方法确定的钯浓度趋势与实际钯浓度预示着良好的契合。
更新日期：2019-12-27
中文翻译：
彩色或荧光高通量定量痕量钯的第三代方法
化学家经常遇到与合成样品中痕量钯相关的问题，因为钯已广泛用于合成有机化学中。我们之前曾报道过用于痕量钯定量的比色法，这是制药行业中唯一实施的高通量方法。但是，与已公布的反应条件相比，微小的变化已导致了可再现性问题，而对基本的分子机理却知之甚少。在当前的研究中，我们采取了一种组合方法来研究该方法，发现过量的NaOH是缺乏可重复性的罪魁祸首。我们相应地改变了反应条件和步骤，从而大大提高了重现性。当前条件下的反应遵循迈克尔尼斯·门腾动力学，可以根据底物浓度预测反应速率。当分析掺有已知数量钯的药物和合成样品却含未知数量的钯时，当前方法分别显示出57％和72％的平均误差。通过当前方法确定的钯浓度趋势与实际钯浓度预示着良好的契合。
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