新型固相萃取-高效液相色谱检测饮用水中的 邻苯二甲酸脂类物质
目的 建立基于新型高效的样品前处理技术即固相萃取-高效液相色谱联用技术同时检测饮用水中七种邻苯二甲酸酯类物质的方法。方法 以3-氨基丙基三乙氧基硅烷作为功能单体, 四乙氧基硅烷作为交联体, 并加入醋酸, 合成新型的高选择性材料, 并用作为固相萃取材料, 吸附七种邻苯二甲酸脂类物质。结果 高效液相色谱等度分析方法的最佳检测条件为: 流动相为乙腈和水(96:4, V:V); 运行时间20 min; 检测波长为230 nm; 流速1.0 mL/min; 柱温30 ℃; 进样量20 μL。目标化合物线性范围较宽, 其中DMP、DBP、DIDP为0.5~100 mg/L, DCHP、BBP、DEHP为0.5~25 mg/L, DEP为0.5~10 mg/L; 该方法对7种目标化合物的检测限在0.18 μg/L~1.86 μg/L范围内, 6次重复实验精密度在1.18%~5.20%之间, 标准添加回收率在63.5%~108.4%之间。结论 该方法可以用于饮用水中苯二甲酸脂类物质的定量检测。
Objective To establish a method for the determination of 7 phthalates in drinking water developed based on solid-phase extraction coupled with high performance liquid chromatography (SPE-HPLC) technology. Methods The high selectivity material was synthesized by 3-aminopropyltriethoxysilane (APTES)as the functional monomer, tetraethoxysilane (TEOS) as the crosslinking agent, and 0.1 mol/L acetic acid as the initiator. The characteristics of preparative material were selective adsorption, and could be used as solid phase extraction adsorbent. Results The optimal testing conditions were as follow: acetonitrile and water (96:4, V:V) as mobile phase, running time 20 min, detection wavelength of 230 nm, flow rate 1.0 mL/min, column temperature 30 ℃, and injection volume 20 μL. The SPE-HPLC method for the determination of 7 phthalates was validated, and the results showed a wide linear range of target compounds that DMP, DBP, and DIDP 0.5~100 mg/L, DCHP, BBP, and DEHP 0.5~25 mg/L, and DEP 0.5~10 mg/L. This detection limit of 7 target compounds ranged from 0.18 μg/L to 1.86 μg/L with RSD in the range of 1.18%~5.20%, and standard recoveries between 63.5% to 108.4%. Conclusion This method can be applied for the quantitative analysis of phthalates in drinking water.
标题：新型固相萃取-高效液相色谱检测饮用水中的 邻苯二甲酸脂类物质
英文标题：Determination of phthalates in drinking water by new solid-phase extraction coupled with high performance liquid chromatography
作者：
何金兴 齐鲁工业大学食品科学与工程学院
张伟 齐鲁工业大学食品科学与工程学院
崔一笑 齐鲁工业大学食品科学与工程学院
刘宝发 齐鲁工业大学食品科学与工程学院
马雪 齐鲁工业大学食品科学与工程学院
中文关键词:邻苯二甲酸酯,固相萃取,高效液相色谱,聚合物材料,饮用水,
英文关键词:phthalates,solid phase extraction,high performance liquid chromatography,polymeric,drinking water,
发表日期：2015-05-27
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