无论该薄层色谱法是否是药典方法,不满足使用需求时,展开剂比例均可以调节的。
欧洲药典2.2.46对薄层色谱法对允许调节的参数进行了具体说明,如下,供参考:
THIN-LAYER CHROMATOGRAPHY
Composition of the mobile phase: the amount of the minor solvent components may be adjusted by ± 30 per cent relative or ± 2 per cent absolute, whichever is the larger; no other component is altered by more than 10 per cent absolute. A minor component comprises less than or equal to (100/n) per
cent, n being the total number of components of the mobile phase. For a minor component at 10 per cent of themobile phase, a 30 per cent relative adjustment allows a range of 7-13 per cent whereas a 2 per cent absolute adjustment allows a range of 8-12 per cent, the relative value therefore being the larger ; for a minor component at 5 per cent of the mobile phase, a 30 per cent relative adjustment allows a range of 3.5-6.5 per cent whereas a 2 per cent absolute adjustment allows a range of 3-7 per cent, the absolute value being the larger in this case.
pH of the aqueous component of the mobile phase: ± 0.2 pH units, unless otherwise prescribed.
Concentration of salts in the buffer component of a mobile phase: ± 10 per cent.
Application volume: 10-20 per cent of the prescribed volume if using fine particle size plates (2-10 μm).
通常,这些参数在上述调节范围内,默认仍是药典分析方法的。
如展开剂调节超出了上述范围,需要补充研究证明满足使用目的的需求,通常至少对其Rf值、检出限值进行确认。
其他药典,展开剂调节后,类比做补充研究,同时注意满足对应市场药典的通则及色谱技术要求即可。
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