CAJ | 학술논문

针对目前毛细管色谱柱装柱效率低、不同批次装填的毛细管色谱柱之间性能差异大的问题，我们发展了一种多通道匀浆装填毛细管色谱柱的新装置。该装置以液相色谱泵提供压力、采用磁力搅拌保持匀浆液均匀分散，一次可装填多达6根毛细管色谱柱。以牛血清白蛋白（ BSA）的胰蛋白酶酶切肽段混合物为样本，选择峰容量、蛋白覆盖率、3个特定离子的保留时间以及毛细管色谱柱柱压为指标，在毛细管液相色谱-质谱联用系统上对装填的反相毛细管色谱柱的性能进行了评价。分别考察了一次装填的6根毛细管色谱柱、两次装填的12根毛细管色谱柱以及一次装填1根与一次装填6根毛细管色谱柱的性能及稳定性。实验结果表明：同一批次装填的6根毛细管色谱柱的性能相近；不同批次装填的12根毛细管色谱柱的峰容量和覆盖率没有明显的区别，但保留时间和毛细管色谱柱柱压的稳定性较差；一次装填1根和一次装填6根毛细管色谱柱柱性能的稳定性与两次分别装填6根毛细管色谱柱的稳定性相近，即采用本装置可显著提高毛细管色谱柱的装填效率且每次装填毛细管色谱柱的数量不会对柱性能产生影响。
침대목전모세관색보주장주효솔저、불동비차장전적모세관색보주지간성능차이대적문제，아문발전료일충다통도균장장전모세관색보주적신장치。해장치이액상색보빙제공압력、채용자력교반보지균장액균균분산，일차가장전다체6근모세관색보주。이우혈청백단백（ BSA）적이단백매매절태단혼합물위양본，선택봉용량、단백복개솔、3개특정리자적보류시간이급모세관색보주주압위지표，재모세관액상색보-질보련용계통상대장전적반상모세관색보주적성능진행료평개。분별고찰료일차장전적6근모세관색보주、량차장전적12근모세관색보주이급일차장전1근여일차장전6근모세관색보주적성능급은정성。실험결과표명：동일비차장전적6근모세관색보주적성능상근；불동비차장전적12근모세관색보주적봉용량화복개솔몰유명현적구별，단보류시간화모세관색보주주압적은정성교차；일차장전1근화일차장전6근모세관색보주주성능적은정성여량차분별장전6근모세관색보주적은정성상근，즉채용본장치가현저제고모세관색보주적장전효솔차매차장전모세관색보주적수량불회대주성능산생영향。
A novel multiple-channel apparatus for packing capillary chromatographic column was designed and manufactured for packing six capillary chromatographic columns with close column efficiency at the same time. Briefly,it consists of a magnetic stirrer,a liquid chromato-graphic pump and a multiple-channel can. The reagents used for preparing ODS( C18)slurry and stirring condition of the magnetic stirrer were optimized in the study. Two batches of capil-lary chromatographic columns were packed under the optimum condition,and these packed capillary chromatographic columns were evaluated in the terms of peak capacity,sequence cov-erage,retention times of three peptide ions and column pressure using the tryptic digest of a bovine serum albumin( BSA)and detected by LC-MS in electrospray ionization( ESI)mode. The experimental results showed that the six capillary chromatographic columns packed at the same time had close column efficiencies,however,the column efficiencies of twelve capillary chromatographic columns packed at two times were significantly different. In addition ,there was no significant column efficiency difference when packing one or six capillary chromato-graphic columns at the same time. The multiple-channel apparatus designed by us is simple, time-saving,and can be applied to pack capillary chromatographic columns with similar column efficiencies,thus it is of evident advantage over traditional one-channel apparatus.