Office of Cosmetics and Colors, Center for Food Safety and Applied Nutrition, U.S. Food and Drug Administration, HFS-106, 5100 Paint Branch Parkway, College Park, MD 20740, USA.
J Chromatogr A. 2011 Nov 11;1218(45):8249-54. doi: 10.1016/j.chroma.2011.09.049. Epub 2011 Sep 22.
In developing analytical methods for batch certification of the color additive D&C Green No. 8 (G8), the U.S. Food and Drug Administration needed the trisodium salt of 1,3,6-pyrenetrisulfonic acid (P3S) for use as a reference material. Since P3S was not commercially available, preparative quantities of it were separated from portions of a sample of G8 that contained ∼3.5% P3S. The separations were performed by pH-zone-refining counter-current chromatography using dodecylamine (DA) as the hydrophobic counterion. The added DA enabled partitioning of the polysulfonated components into the organic stationary phase of the two-phase solvent system used, 1-butanol-water (1:1). Thus, a typical separation that involved 20.3g of G8, using sulfuric acid as the retainer acid and 20% DA in the stationary phase and 0.1M sodium hydroxide as the mobile phase, resulted in ∼0.58 g of P3S of greater than 99% purity. The identification and characterization of the separated P3S were performed by elemental analyses, proton nuclear magnetic resonance, high-resolution mass spectrometry, ultra-violet spectra, and high-performance liquid chromatography.
在开发用于批量认证色淀绿 8 号（G8）的分析方法时，美国食品和药物管理局需要 1,3,6-苝三磺酸三钠盐（P3S）作为参考物质。由于 P3S 没有商业用途，因此从含有约 3.5% P3S 的 G8 样品中分离出了制备量的 P3S。分离是通过 pH 区带精制逆流色谱法用十二胺（DA）作为疏水性抗衡离子进行的。添加的 DA 使多磺酸化成分分配到所用两相溶剂系统的有机固定相 1-丁醇-水（1:1）中。因此，典型的分离涉及 20.3g 的 G8，使用硫酸作为保留酸，固定相中的 20% DA 和 0.1M 氢氧化钠作为流动相，得到了约 0.58g 纯度大于 99%的 P3S。通过元素分析、质子核磁共振、高分辨率质谱、紫外光谱和高效液相色谱对分离出的 P3S 进行了鉴定和表征。
