Substitution determination of Fmoc-substituted resins at different wavelengths.
Substitution determination of Fmoc-substituted resins at different wavelengths.
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DOI：
10.1002/psc.3021
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发表时间：
2017-10
期刊：
影响因子：
--
通讯作者：
Samson D
中科院分区：
文献类型：
--
作者：
Eissler S;Kley M;Bächle D;Loidl G;Meier T;Samson D
在固相肽合成中，使用起始树脂取代和起始树脂的质量计算标称批量。起始树脂取代构成了计算一整套重要工艺参数的基础，例如氨基酸衍生物当量数。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）哌啶的DMF溶液中以生成二苯并富烯-哌啶加合物（通过紫外-可见光谱法进行定量）来进行取代测定。在二苯并富烯-哌啶加合物的最大吸收波长，即301.0 nm处进行光谱测定。将记录的吸光度值、树脂重量和体积与301.0 nm处的物质特定摩尔吸光系数一起输入根据朗伯-比尔定律推导的方程中，以计算标称取代度。据我们所知，在301.0 nm处，二苯并呋喃-哌啶加合物的摩尔吸光系数在7100 l mol−1 cm−1和8100 l mol−1 cm−1之间。根据应用值，标称批量可能相差14%。在该出版物中，报道了在301.0和289.8 nm处的摩尔吸光系数的测定。此外，证明了通过测量289.8 nm处的吸收，波长精度的影响降低。© 2017 The Authors Journal of Peptide Science由European Peptide Society和John Wiley & Sons Ltd出版。
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.
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DOI：
10.1039/c39780000537
发表时间：
1978-01-01
影响因子：
--
作者：
ATHERTON, E;FOX, H;WILLIAMS, BJ
通讯作者：
WILLIAMS, BJ
DOI：
10.1039/p19810000538
发表时间：
1981-01-01
期刊：
JOURNAL OF THE CHEMICAL SOCIETY-PERKIN TRANSACTIONS 1
影响因子：
--
作者：
ATHERTON, E;LOGAN, CJ;SHEPPARD, RC
通讯作者：
SHEPPARD, RC
影响因子：
3.6
作者：
CARPINO, LA;HAN, GY
通讯作者：
HAN, GY
影响因子：
1.8
作者：
RAMAGE, R;IRVING, SL;MCINNES, C
通讯作者：
MCINNES, C
影响因子：
3.6
作者：
CARPINO, LA;MANSOUR, EME;KNAPCZYK, J
通讯作者：
KNAPCZYK, J