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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 m L/min;柱温30℃;进样量20μL。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0.18μg/L~1.86μg/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 simultaneous determination of seven phthalates in drinking water based on a novel and efficient sample preparation technique, SPE-HPLC. Methods 3-Aminopropyltriethoxysilane as a functional monomer, tetraethoxysilane as a cross-linked body, and adding acetic acid to synthesize a new type of highly selective materials, and used as a solid phase extraction material, adsorption of seven kinds of o-ring Phthalate esters. Results The optimum conditions for the isocratic analysis of HPLC were as follows: mobile phase consisted of acetonitrile and water (96: 4, V: V); the running time was 20 min; the detection wavelength was 230 nm; the flow rate was 1.0 m L / min; Column temperature 30 ℃; injection volume 20μL. The linear range of the target compound ranged from 0.5 to 100 mg / L for DMP, DBP and DIDP, 0.5 to 25 mg / L for DCHP, 0.5 to 25 mg / L for DEHP and 0.5 to 10 mg / L for DEHP. The limits of detection were in the range of 0.18μg / L to 1.86μg / L. The precision of six replicates was between 1.18% and 5.20%. The standard recoveries ranged from 63.5% to 108.4%. Conclusion This method can be used for the quantitative determination of phthalic acid lipids in drinking water.