Stapley J, Buckton G, Merrifield D
GlaxoSmithKline, New Frontiers Science Park, Third Avenue, Harlow, Essex CM19 5AW, UK.
Int J Pharm. 2006 Aug 2;318(1-2):22-7. doi: 10.1016/j.ijpharm.2006.03.011. Epub 2006 Mar 17.
The purpose of this study was to find a suitable material for use as a system suitability test material for inverse gas chromatography (IGC). The purpose of a system check is to measure the variability of the instrument being used rather than the material being analysed. Having such a system check for IGC enables a basic GMP requirement to be met. IGC results can then be used in regulatory submissions to support other already established techniques for characterising pharmaceutical materials. Alpha-alumina was chosen because it is inorganic, stable at high temperatures, resistant to hydration and is already established as a system check material for surface area determination by nitrogen adsorption. Two columns (1 and 2) packed from the same reference sample jar of alpha-alumina and analysed under the same conditions yielded dispersive surface energies of 34.8+/-0.8 and 35.3+/-0.8 mJ/m(2), respectively, at 15% RH. Column 1 was analysed on a second IGC system, and gave a dispersive surface energy of 34.7+/-0.2 mJ/m(2). No significant change was evident after 7 months storage under laboratory ambient conditions. Analysis of material from a second reference sample jar of alpha-alumina produced results not noticeably different to those of the first, yielding a dispersive surface energy of 35.3+/-0.1 mJ/m(2). A change was seen to occur in the surface properties alpha-alumina when the humidity was varied, but the change appeared to be consistent across the two columns reported. Based upon the data in this experimental, alpha-alumina appears to be a suitable material for use as a system suitability test material for IGC.
本研究的目的是找到一种适合用作反相气相色谱法（IGC）系统适用性测试材料的物质。系统检查的目的是测量所用仪器的变异性，而非被分析物质的变异性。对IGC进行这样的系统检查能够满足基本的GMP要求。然后，IGC结果可用于监管申报，以支持其他已确立的用于表征药物材料的技术。选择α-氧化铝是因为它是无机的，在高温下稳定，抗水化，并且已经被确立为通过氮吸附测定表面积的系统检查材料。从同一α-氧化铝参考样品罐装填的两根色谱柱（1号和2号）在相同条件下进行分析，在15%相对湿度下分别得到的分散表面能为34.8±0.8和35.3±0.8 mJ/m²。1号色谱柱在第二个IGC系统上进行分析，得到的分散表面能为34.7±0.2 mJ/m²。在实验室环境条件下储存7个月后，未观察到明显变化。对来自第二个α-氧化铝参考样品罐的材料进行分析，得到的结果与第一个样品罐的结果没有明显差异，分散表面能为35.3±0.1 mJ/m²。当湿度变化时，α-氧化铝的表面性质发生了变化，但在所报道的两根色谱柱上，这种变化似乎是一致的。基于本实验中的数据，α-氧化铝似乎是一种适合用作IGC系统适用性测试材料的物质。
