An experimental study of sampling time effects on the resolving power of on-line two-dimensional high performance liquid chromatography.
An experimental study of sampling time effects on the resolving power of on-line two-dimensional high performance liquid chromatography.
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DOI：
10.1016/j.chroma.2011.03.032
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发表时间：
2011-05-20
期刊：
影响因子：
--
通讯作者：
Carr PW
中科院分区：
文献类型：
--
作者：
Huang Y;Gu H;Filgueira M;Carr PW
研究了取样时间对在线LC×LC分辨能力的影响。系统地改变第一维梯度时间（1 tg）和采样时间（ts）（1 tg = 5、12、24和49 min; ts = 6、12、21和40 s）。以玉米种子提取物的分离中观察到的峰数和获得的有效二维峰容量两个指标来评价在线LC×LC的分离能力。LC×LC的最大有效峰容量和观察到的峰数始终在12 - 21 s之间的采样时间内达到，在所有的第一维梯度时间。此外，这两个指标都表明，完全优化的1DLC和LC×LC具有相同分辨率的“交叉”时间随采样时间略有变化，但对于12和21 s的采样时间，仅约为5分钟。当采样时间为6 s时，交叉时间最长。此外，增加第一维梯度时间使LC×LC相对于1DLC的分辨能力有很大提高。最后，校正和有效的2D峰容量以及观察到的峰的数量的比较表明，覆盖因子的影响是相当显着的。
The experimental effects of sampling time on the resolving power of on-line LC×LC were investigated. The first dimension gradient time (1tg) and sampling time (ts) were systematically varied (1tg = 5, 12, 24 and 49 min; ts = 6, 12, 21 and 40 s). The resolving power of on-line LC×LC was evaluated in terms of two metrics namely the numbers of observed peaks and the effective 2D peak capacities obtained in separations of extracts of maize seeds. The maximum effective peak capacity and number of observed peaks of LC×LC was always achieved at sampling times between 12 and 21 s, at all first dimension gradient times. In addition, both metrics showed that the “crossover” time at which fully optimized 1DLC and LC×LC have equal resolving power varied somewhat with sampling time but is only about 5 minutes for sampling times of 12 and 21 s. The longest crossover time was obtained when the sampling time was 6 s. Furthermore, increasing the first dimension gradient time gave large improvements in the resolving power of LC×LC relative to 1DLC. Finally, comparisons of the corrected and effective 2D peak capacities as well as the number of peaks observed showed that the impact of the coverage factor is quite significant.
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