污泥中有机磷酸酯检测的预处理优化

Optimization of pretreatment method for determination of Organophosphate esters in sludge samples

基于"富集(加速溶剂萃取)+净化+检测"的步骤,进行污泥取样量、萃取条件、净化柱类型、淋洗液极性和洗脱液极性的优化.确定了0.2g污泥取样量、130℃萃取温度、1:1(V/V)的丙酮/二氯甲烷混合溶液为萃取剂、氨基柱净化、2:5(V/V)的二氯甲烷/正己烷混合溶液为淋洗液、二氯甲烷为洗脱液,最后用超高效液相色谱-串联质谱对有机磷酸酯进行定性定量检测.结果表明,各物质的基质加标回收率均在60%～120%之间,基质效应也基本控制在±15%.净化方法同样适用于污水样品,用此方法成功测定了北京市某污水处理厂各工艺单元的水相及固相样品,显示出良好的适用性.

In this his study,based on the steps of"enrichment(accelerated solvent extraction)+purification+detection",the operation parameters of sludge sampling volume,extraction conditions,purification column type,wash polarity and eluent polarity were optimized.The optimal parameters include:a sludge sampling volume of 0.2g,an extraction temperature of 130°C,a 1:1(v/v)solution mixing ratio of acetone/dichloromethane extractant,and an amino column purification operation.A 2:5(v/v)mixing ratio was used for the dichloromethane/n-hexane wash solution,and dichloromethane was used as the eluent.The qualitative and quantitative detection of organophosphate esters(OPEs)using an ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS)demonstrated:the matrix spike recoveries for all identified OPEs were between 60%and 120%with a matrix effect no more than±15%.The pretreatment method could also be appropriate for the determination of OPEs in wastewater samples.This pretreatment method was successfully applied to measure the concentrations of OPEs in the water phase and solid phase samples from the main units in a sewage treatment plant in Beijing,and a good result was achieved.