Johnston Cliff T, Wang Shan-Li, Hem Stanley L
Department of Agronomy, Purdue University, West Lafayette, Indiana 47907, USA.
J Pharm Sci. 2002 Jul;91(7):1702-6. doi: 10.1002/jps.10166.
The traditional method of determining surface area, nitrogen gas sorption, requires complete drying of the sample prior to analysis. This technique is not suitable for aluminum hydroxide adjuvant because it is composed of submicron, fibrous particles that agglomerate irreversibly upon complete removal of water. In this study, the surface area of a commercial aluminum hydroxide adjuvant was determined by a gravimetric/FTIR method that measures the water adsorption capacity. This technique does not require complete drying of the adjuvant. Five replicate determinations gave a mean surface area of 514 m(2)/g and a 95% confidence interval of 36 m(2)/g for a commercial aluminum hydroxide adjuvant. The X-ray diffraction pattern and the Scherrer equation were used to calculate the dimensions of the primary crystallites. The average calculated dimensions were 4.5 x 2.2 x 10 nm. Based on these dimensions, the mean calculated surface area of the commercial aluminum hydroxide adjuvant was 509 m(2)/g, and the 95% confidential interval was 30 m(2)/g. The close agreement between the two surface area values indicates that either method may be used to determine the surface area of aluminum hydroxide adjuvant. The high surface area, which was determined by two methods, is an important property of aluminum hydroxide adjuvants, and is the basis for the intrinsically high protein adsorption capacity.
传统的测定表面积的方法——氮气吸附法,在分析之前需要将样品完全干燥。这种技术不适用于氢氧化铝佐剂,因为它由亚微米级的纤维状颗粒组成,在完全除去水分后会不可逆地团聚。在本研究中,一种商业氢氧化铝佐剂的表面积通过重量法/傅里叶变换红外光谱法测定,该方法测量水吸附容量。此技术不需要将佐剂完全干燥。五次重复测定得出一种商业氢氧化铝佐剂的平均表面积为514 m²/g,95%置信区间为36 m²/g。利用X射线衍射图谱和谢乐方程计算初级微晶的尺寸。计算出的平均尺寸为4.5×2.2×10 nm。基于这些尺寸,计算得出的商业氢氧化铝佐剂的平均表面积为509 m²/g,95%置信区间为30 m²/g。两种表面积值之间的密切一致性表明,两种方法均可用于测定氢氧化铝佐剂的表面积。通过两种方法测定的高表面积是氢氧化铝佐剂的一个重要特性,也是其本质上高蛋白吸附能力的基础。