School of Chemistry and Environment, South China Normal University, Guangzhou 510006, China.
Talanta. 2011 May 15;84(3):644-50. doi: 10.1016/j.talanta.2011.01.035. Epub 2011 Jan 22.
A triazolam-imprinted silica microsphere was prepared by combining a surface molecular-imprinting technique with the sol-gel process. The results illustrate that the triazolam-imprinted silica microspheres provided using γ-aminopropyltriethoxysilane and phenyltrimethoxysilane as monomers exhibited higher selectivity than those provided from γ-aminopropyltriethoxysilane and methyltriethoxysilane. In addition, the optimum affinity occurred when the molar ratio of γ-aminopropyltriethoxysilane, phenyltrimethoxysilane, and the template molecule was 4.2:4.7:0.6. Retention factor (k) and imprinting factor (IF) of triazolam on the imprinted and non-imprinted silica microsphere columns were characterized using high performance liquid chromatography (HPLC) with different mobile phases including methanol, acetonitrile, and water solutions. The molecular selectivity of the imprinted silica microspheres was also evaluated for triazolam and its analogue compounds in various mobile phases. The better results indicated that k and IF of triazolam on the imprinted silica microsphere column were 2.1 and 35, respectively, when using methanol/water (1/1, v/v) as the mobile phase. Finally, the imprinted silica was applied as a sorbent in solid-phase extraction (SPE), to selectively extract triazolam and its metabolite, α-hydroxytriazolam, from human urine samples. The limits of detection (LOD) for triazolam and α-hydroxytriazolam in urine samples were 30 ± 0.21 ng mL(-1) and 33 ± 0.26 ng mL(-1), respectively.
采用表面分子印迹技术与溶胶-凝胶过程相结合的方法制备了三唑仑印迹硅胶微球。结果表明,以γ-氨丙基三乙氧基硅烷和苯基三甲氧基硅烷为单体制备的三唑仑印迹硅胶微球比以γ-氨丙基三乙氧基硅烷和甲基三甲氧基硅烷为单体制备的微球具有更高的选择性。此外,当γ-氨丙基三乙氧基硅烷、苯基三甲氧基硅烷和模板分子的摩尔比为 4.2:4.7:0.6 时,出现最佳亲和力。采用不同的流动相,包括甲醇、乙腈和水溶液,通过高效液相色谱(HPLC)对印迹和非印迹硅胶微球柱上的三唑仑的保留因子(k)和印迹因子(IF)进行了表征。在各种流动相中还评估了印迹硅胶微球对三唑仑及其类似物化合物的分子选择性。更好的结果表明,当使用甲醇/水(1/1,v/v)作为流动相时,三唑仑在印迹硅胶微球柱上的 k 和 IF 分别为 2.1 和 35。最后,将印迹硅胶作为固相萃取(SPE)的吸附剂,从人尿液样品中选择性地提取三唑仑及其代谢物α-羟基三唑仑。尿液样品中三唑仑和α-羟基三唑仑的检测限(LOD)分别为 30±0.21ng mL(-1)和 33±0.26ng mL(-1)。