期刊
MONATSHEFTE FUR CHEMIE
卷 152, 期 9, 页码 1075-1080出版社
SPRINGER WIEN
DOI: 10.1007/s00706-021-02789-5
关键词
Dibenzofulvene; Dibenzofulvene-piperidine adduct; Fmoc protection; Internal standard; Loading determination; RP-HPLC; Solid-phase synthesis
资金
- Charles University [Progress Q46]
The simple RP-HPLC method using an internal standard accurately determines resin loading in solid-phase peptide synthesis, suitable for common synthesis types with reliable results for monitoring in multi-step synthesis.
A simple RP-HPLC method based on an internal standard is proposed to determine the resin loading in solid-phase peptide synthesis. The method is applicable for the most common type of synthesis, where 9-fluorenylmethoxycarbonyl (Fmoc) is used as the protective group and piperidine as the deprotecting agent. Both products of the deprotection reaction (dibenzofulvene and dibenzofulvene-piperidine adduct) are separated by RP-HPLC and quantified by a UV detector. Biphenyl serves as the internal standard for both analytes. The resin loading is calculated using the equation resulting from the combination of internal standard method equations for each of the two analytes. The method provides true results, as evidenced by their comparison with the independent method. The relative standard deviation of the method is 1.52%. A further advantage of the method is that it allows determination from the waste solution of the synthesis, and, therefore, can also be used for monitoring during multi-step synthesis. [GRAPHICS] .
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