Repeatability and reproducibility of high concentration data in reversed-phase liquid chromatography. I. Overloaded band profiles on Kromasil-C18.

Repeatability and reproducibility of high concentration data in reversed-phase liquid chromatography. I. Overloaded band profiles on Kromasil-C18.
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反相液相色谱中高浓度数据的重复性和再现性。

DOI:
10.1016/s0021-9673(03)00685-x
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发表时间:
2003
期刊:
Journal of chromatography. A
影响因子:
--
通讯作者:
G. Guiochon
G. Guiochon
中科院分区:
--
文献类型:
--
作者:
F. Gritti;G. Guiochon

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在Kromasil-C18色谱柱上,以水-甲醇溶液(70:30 ~ 20:80,v/v)为移动的流动相,采用前沿分析法(FA)测定了6种低分子量化合物(苯酚、苯胺、咖啡因、茶碱、心得安和普萘洛尔)的单组分吸附等温线。还使用乙酸盐缓冲液(0.2 M)代替水获得普萘洛尔数据。数据进行建模计算和实验过载带配置文件之间的最佳协议。吸附能量分布也被推导出来,并用于选择最佳的等温模型。发现广泛不同的等温线模型最好地模拟这些化合物获得的数据,凸向上(即朗缪尔),凸向下(即反朗缪尔),和S形等温线。所有色谱柱均使用相同的样本量(上样因子,Lf ≥ 10%),在填充有相同批次Kromasil-C18的4个不同色谱柱和填充有不同批次Kromasil-C18的5个其他色谱柱上记录过载条带图谱。将这些实验谱带分布与由在第一柱上通过FA测量的等温线计算的分布进行比较。条带特征的重复性以及柱间和批间重现性均优于4%。
Single-component adsorption-isotherm data were acquired by frontal analysis (FA) for six low-molecular-mass compounds (phenol, aniline, caffeine, theophylline, ethylbenzene and propranolol) on one Kromasil-C18column, using water–methanol solutions (between 70:30 and 20:80, v/v) as the mobile phase. Propranolol data were also acquired using an acetate buffer (0.2 M) instead of water. The data were modeled for best agreement between calculated and experimental overloaded band profiles. The adsorption energy distribution was also derived and used for the selection of the best isotherm model. Widely different isotherm models were found to model best the data obtained for these compounds, convex upward (i.e. Langmuirian), convex downward (i.e. anti-Langmuirian), and S-shaped isotherms. Using the same sample size for all columns (loading factor, Lf≈10%), overloaded band profiles were recorded on four different columns packed with the same batch of Kromasil-C18and five other columns packed with different batches of Kromasil-C18. These experimental band profiles were compared to the profile calculated from the isotherm measured by FA on the first column. The repeatability as well as the column-to-column and the batch-to-batch reproducibilities of the band profiles are better than 4%.
DOI: 10.1021/ac0105686
发表时间: 2001-10-01
影响因子: 7.4
作者:
Umpleby, RJ;Baxter, SC;Shimizu, KD
通讯作者: Shimizu, KD