【摘要】 采用高效液相色谱-二极管阵列检测器对6种PAEs类物质进行测定,并对梯度洗脱条件、流速、检测波长等影响化合物色谱响应的关键参数进行优化。综合考虑样品测试效率、分析精度、实际样品中存在杂质干扰等因素,确定以乙腈-水为流动相进行梯度洗脱,洗脱0~11 min流动相乙腈-水梯度比例为50∶50,11 min后流动相调整为100%乙腈,各化合物均能完全分离;色谱分析流速为0.8 m L/min;PAEs的最佳吸收波长为225 nm。在优化的色谱条件下,6种PAEs的线性良好,相关系数均大于0.999 8,仪器检出限为0.08~0.12 mg/L,保留时间、峰面积的相对标准偏差分别为0.02%~0.60%、0.13%~0.86%。方法灵敏度较高,适合土壤等邻苯二甲酸酯含量较高基质样品的快速分析。更多还原

【Abstract】 Effects of key parameters such as gradient elution,flow rate,detection wavelength on the chromatographic response of target analytes were investigated,and the chromatographic conditions for determination of 6 kinds of phthalic acid esters by high performance liquid chromatography with diode array detector were optimized. The ultimate conditions were: chromatographic column: SupelcosilTMLC( 15 cm × 4. 6 mm,0. 5 μm); column temperature 25 ℃; injection volume 15 μL; mobile phase were acetonitrile and water; gradient eluted program: 0 ~ 11 min V( acetonitrile) : V( water) = 50 ∶ 50,after 11 min V( acetonitrile) :V( water) = 50 ∶ 50; flow rate 0. 8 m L / min; detection wavelength 225 nm. Results indicate that the method has a good linear relationship with all correlation coefficients over 0. 999 8,instrument detection limits of PAEs from 0. 08 to 0. 12 mg / L,relative standard deviations of retention time and chromatographic peak area range from 0. 02%-0. 60% and 0. 13%-0. 86% respectively,which indicated good method precision. The established method is efficient,accurate and repeatable which can be applied to the determination of soil samples.更多还原