Zhang Min, Khripin Constantine Y, Fagan Jeffrey A, McPhie Peter, Ito Yoichiro, Zheng Ming
Shanghai Key Laboratory of New Drug Design, School of Pharmacy, East China University of Science and Technology , 130 Meilong Road, Shanghai 200237, China.
Anal Chem. 2014 Apr 15;86(8):3980-4. doi: 10.1021/ac5003189. Epub 2014 Apr 4.
Development of simple processes to fractionate synthetic mixtures of single-wall carbon nanotubes (SWCNTs) into individual species is crucial to many applications. Existing methods for single-chirality SWCNT purification are cumbersome, often requiring multiple steps and different conditions for different species. Here, we report a method to achieve total fractionation of a synthetic SWCNT mixture by countercurrent chromatography, resulting in purification of many single-chirality SWCNT species in a single run. This method is based on a tunable partition of sodium deoxycholate dispersed SWCNTs in a polyethylene glycol/dextran aqueous two-phase system. By running the mobile phase with 0.02% of sodium deoxycholate and a gradient of sodium dodecyl sulfate from 0.1% to 0.7% (w/w), we observe clear diameter-dependent elution, with ∼ 90% total recovery. Among all the fractions collected, a number of them are enriched in single-chirality (9,4), (7,5), (7,6), (8,3), (6,5) species, while most of the remaining ones contain no more than 2-3 major species. We also observe strong (n,m)-dependent elution peak width due to the enantiomer-resolved partition. These results demonstrate countercurrent chromatography (CCC) as an effective way to obtain high purity (n, m) species, and suggest the potential of CCC as an analytical tool for chirality distribution mapping of synthetic SWCNT mixtures.
开发将单壁碳纳米管(SWCNT)的合成混合物分离成单个种类的简单方法对许多应用至关重要。现有的单手性SWCNT纯化方法很繁琐,通常需要针对不同种类进行多个步骤和不同条件的操作。在此,我们报告一种通过逆流色谱法实现合成SWCNT混合物完全分离的方法,从而在一次运行中纯化多种单手性SWCNT种类。该方法基于脱氧胆酸钠分散的SWCNT在聚乙二醇/葡聚糖水两相系统中的可调分配。通过使用含0.02%脱氧胆酸钠的流动相和0.1%至0.7%(w/w)的十二烷基硫酸钠梯度,我们观察到明显的直径依赖性洗脱,总回收率约为90%。在收集的所有馏分中,有一些富含单手性(9,4)、(7,5)、(7,6)、(8,3)、(6,5)种类,而其余大部分馏分包含不超过2 - 3种主要种类。由于对映体拆分分配,我们还观察到强烈的(n,m)依赖性洗脱峰宽。这些结果证明逆流色谱法(CCC)是获得高纯度(n,m)种类的有效方法,并表明CCC作为合成SWCNT混合物手性分布图分析工具的潜力。