CAMAG, Sonnenmattstrasse 11, 4132 Muttenz, Switzerland;.
CAMAG, Sonnenmattstrasse 11, 4132 Muttenz, Switzerland.
J Chromatogr A. 2021 Feb 8;1638:461830. doi: 10.1016/j.chroma.2020.461830. Epub 2021 Jan 5.
The use of chromatographic methods in routine analysis includes System Suitability Tests (SST). This paper presents a novel approach to SST in HPTLC, which allows qualification of the entire R range of an HPTLC plate independently of the samples. It is based on the Universal HPTLC mix (UHM), a pre-defined mixture of eight reference substances: guanosine, sulisobenzone, thymidine, paracetamol, phthalimide, 9-hydroxyfluorene, thioxanthen-9-one, and 2-(2H-benzotriazol-2-yl)-4-(1,1,3,3-tetramethylbutyl)phenol, selected to cover a broad range of polarities and functional groups. The chromatographic behavior of the UHM was evaluated for 20 different mobile phases on Silica gel 60 F. At least three constituents were baseline separated. In a collaborative trial with four laboratories the reproducibility of R values for three representative mobile phases, was found to be within a confidence interval of 0.040 R units. The response characteristics of the UHM were assessed with respect to changes in chromatographic conditions, such as variation of the relative humidity, improperly employed saturation, or mistakes in the preparation of the mobile phase. Based on the R values of the individual constituents significant responses were found for most changes. This qualifies the UHM for use in SST.
在常规分析中使用色谱方法包括系统适用性测试(SST)。本文提出了一种新的 HPTLC 中 SST 的方法,该方法允许独立于样品对整个 HPTLC 板的 R 范围进行定性。它基于通用 HPTLC 混合物(UHM),这是一种预定义的八种参考物质混合物:鸟苷、磺酰苯酮、胸腺嘧啶、扑热息痛、邻苯二甲酰亚胺、9-羟基芴、噻吨酮-9-酮和 2-(2H-苯并三唑-2-基)-4-(1,1,3,3-四甲基丁基)苯酚,选择这些物质以涵盖广泛的极性和官能团。在硅胶 60 F 上评估了 UHM 在 20 种不同流动相下的色谱行为,至少有三种成分实现了基线分离。在与四个实验室的协作试验中,发现三种代表性流动相的 R 值重现性在置信区间内为 0.040 R 单位。还评估了 UHM 的响应特性,例如色谱条件的变化,如相对湿度的变化、不当的饱和、或移动相制备中的错误。基于各成分的 R 值,发现大多数变化都会产生显著的响应。这使 UHM 有资格用于 SST。