McKellop K, Davidson W, Hansen G, Freeman D, Pallai P
Boehringer Ingelheim Pharmaceuticals, Inc., Ridgefield, CT 06877.
Pept Res. 1991 Jan-Feb;4(1):40-6.
Crude product mixtures from the solid-phase synthesis of a series of peptides were analyzed by on-line packed, fused silica column mu-HPLC/Continuous Flow Fast Atom Bombardment Mass Spectrometry (mu-HPLC/CF-FABMS). The technique is superior to the direct FAB analysis of crude product mixtures since competitive ionization and suppression effects are not generally observed. Positive correlation between a chromatographic peak and the desired synthetic product may be obtained. An accurate assessment of peptide deprotection can be made without ambiguity arising from the MS fragmentation of the more labile t-butyl and BOC protecting groups used in FMOC-based solid-phase peptide synthesis strategies. mu-HPLC combined with in-line UV detection and MS analysis allows the use of minimum sample and injection volumes, typically 10-50 pmol contained in 0.2-0.5 microliters.
通过在线填充熔融石英柱微高效液相色谱/连续流快原子轰击质谱法（μ-HPLC/CF-FABMS）对一系列肽固相合成的粗产物混合物进行了分析。该技术优于对粗产物混合物的直接快原子轰击分析，因为通常不会观察到竞争性电离和抑制效应。可以获得色谱峰与所需合成产物之间的正相关关系。对于肽脱保护可以进行准确评估，而不会因基于芴甲氧羰基（FMOC）的固相肽合成策略中使用的更不稳定的叔丁基和叔丁氧羰基（BOC）保护基团的质谱裂解而产生歧义。μ-HPLC与在线紫外检测和质谱分析相结合，允许使用最少的样品量和进样体积，通常0.2 - 0.5微升中含有10 - 50皮摩尔。
