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采用加速溶剂萃取法(ASE)-固相萃取净化法(SPE),联合高效液相色谱法(HPLC-UV)测定城市污泥堆肥中三氯生。通过对加速溶剂萃取条件、固相萃取净化和高效液相色谱条件的优化,最后确定ASE萃取溶剂为二氯甲烷,SPE净化采用HLB固相萃取柱,甲醇/丙酮(V∶V=1∶1)为洗脱溶剂,流动相为甲醇/水(V∶V=80∶20),检测波长λ=280 nm。当三氯生浓度在1~20μg/m L时,其HPLC峰面积与其浓度呈良好的线性关系,相关系数r~2=0.997 4,加标回收率在79.7%~104.1%之间,检出限(S/N=3)为0.16μg/g,RSD<13%。该方法简便、快速、准确、重复性较好,能满足城市污泥堆肥中三氯生定量分析要求。
Triclosan in municipal sludge compost was determined by accelerated solvent extraction (ASE) -pure solid phase extraction (SPE) combined with high performance liquid chromatography (HPLC-UV). The conditions of accelerated solvent extraction, solid-phase extraction and high performance liquid chromatography were optimized. Finally, the ASE extraction solvent was determined to be methylene chloride. The SPE purification was performed on an HLB solid phase extraction cartridge with methanol / acetone (V: V = ) As the eluting solvent, the mobile phase was methanol / water (V:V = 80:20), detection wavelength λ = 280 nm. When triclosan concentration was 1 ~ 20μg / m L, the HPLC peak area showed a good linear relationship with the concentration, the correlation coefficient r = 2 = 0.997 4, the recoveries were between 79.7% and 104.1% The limit (S / N = 3) was 0.16 μg / g with RSD <13%. The method is simple, rapid, accurate and reproducible, and can meet the quantitative analysis of triclosan in municipal sludge compost.