Fmoc取代树脂在不同波长下的取代测定。,Journal of Peptide Science

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Fmoc取代树脂在不同波长下的取代测定。
Journal of Peptide Science ( IF 1.8 ) Pub Date : 2017-06-21 , DOI: 10.1002/psc.3021
Stefan Eissler ₁ , Markus Kley ₁ , Dirk Bächle ₁ , Günther Loidl ₂ , Thomas Meier ₁ , Daniel Samson ₁

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在固相肽合成中，使用起始树脂替代物和起始树脂的质量计算标称批次大小。起始树脂取代构成了计算整套重要工艺参数（例如氨基酸衍生物当量的数量）的基础。对于Fmoc取代的树脂，通常通过将Fmoc保护的起始树脂悬浮在20％（v / v）的DMF中的哌啶中，以生成二苯并富勒烯-哌啶加合物，并通过紫外-可见光谱对其进行定量，从而确定取代基。光谱测定是在二苯并富勒烯-哌啶加合物的最大吸收波长处进行的，即在301.0 nm处进行。记录的吸收值，树脂重量和体积输入到根据兰伯特-比尔定律得出的方程式中，连同在301.0 nm处的特定于物质的摩尔吸收系数，以计算名义取代。据我们所知，摩尔吸收系数为7100 l mol据报道，在301.0 nm下，二苯并富勒烯-哌啶加合物的^-1 cm ^-1和8100 l mol ^-1 cm ^-1。根据应用的值，标称批量大小可能相差高达14％。在该出版物中，报道了在301.0和289.8nm处的摩尔吸收系数的测定。此外，有证据表明，通过测量289.8 nm处的吸收率，可以降低波长精度的影响。©2017欧洲多肽协会和John Wiley＆Sons Ltd.出版的《作者多肽科学杂志》。

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Substitution determination of Fmoc-substituted resins at different wavelengths.

In solid‐phase peptide synthesis, the nominal batch size is calculated using the starting resin substitution and the mass of the starting resin. The starting resin substitution constitutes the basis for the calculation of a whole set of important process parameters, such as the number of amino acid derivative equivalents. For Fmoc‐substituted resins, substitution determination is often performed by suspending the Fmoc‐protected starting resin in 20% (v/v) piperidine in DMF to generate the dibenzofulvene–piperidine adduct that is quantified by ultraviolet–visible spectroscopy. The spectrometric measurement is performed at the maximum absorption wavelength of the dibenzofulvene–piperidine adduct, that is, at 301.0 nm. The recorded absorption value, the resin weight and the volume are entered into an equation derived from Lambert–Beer's law, together with the substance‐specific molar absorption coefficient at 301.0 nm, in order to calculate the nominal substitution. To our knowledge, molar absorption coefficients between 7100 l mol⁻¹ cm⁻¹ and 8100 l mol⁻¹ cm⁻¹ have been reported for the dibenzofulvene–piperidine adduct at 301.0 nm. Depending on the applied value, the nominal batch size may differ up to 14%. In this publication, a determination of the molar absorption coefficients at 301.0 and 289.8 nm is reported. Furthermore, proof is given that by measuring the absorption at 289.8 nm the impact of wavelength accuracy is reduced. © 2017 The Authors Journal of Peptide Science published by European Peptide Society and John Wiley & Sons Ltd.

更新日期：2017-06-21

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