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采用两步催化的溶胶-凝胶法合成了一种新型的有机-无机杂化高效液相色谱整体柱。首先以γ-氨基丙基三乙氧基硅烷(HG-550)作为扩链剂与环氧树脂反应形成带有双苯基的有机长链双硅烷,反应生成的长链双硅烷再与四乙氧基硅烷(TEOS)发生脱水缩合形成带有双苯基且具有一定孔结构和机械强度的整体柱材料。新型整体柱作为固相萃取柱对尿液中的倍他米松进行了富集及分析。实验结果表明,倍他米松在5 mg/L~30 mg/L线性范围内线性关系良好,A=-1.61×104+1.89×104C(R=0.9994,n=6),检测限为0.006mg/L;绝对回收率79.44%~83.03%之间;日内、日间精密度均<5.0%,能满足分析的要求
A novel organic-inorganic hybrid HPLC column was synthesized by a two-step catalytic sol-gel method. First, using γ-aminopropyltriethoxysilane (HG-550) as a chain extender and epoxy resin reaction with the formation of long chain bis-silane with bisphenyl, the reaction of long-chain bis-silane and then tetraethyl Dehydration condensation of the polyoxy silane (TEOS) results in the formation of a monolithic column material with biphenyl and a certain pore structure and mechanical strength. The new monolithic column as a solid phase extraction column on the urine of betamethasone enrichment and analysis. The experimental results showed that betamethasone had good linearity in the linear range of 5 mg / L to 30 mg / L, with A = -1.61 × 104 + 1.89 × 104C (R = 0.9994, n = 6) L; the absolute recoveries were between 79.44% and 83.03%; the intra-day and inter-day precision were less than 5.0%, which could meet the analytical requirements