快速溶剂萃取-LC-MS/MS法测定污泥中的6种邻苯二甲酸酯

Determination of Six Phthalates in Sludge by Rapid Solvent Extraction-LC-MS/MS

建立了快速溶剂萃取-LC-MS/MS法测定污泥中的6种邻苯二甲酸酯的分析检测方法。污泥经冷冻干燥,研磨过0.250 mm(60目)筛,在快速溶剂萃取仪上用正己烷-丙酮(V_(正己烷)∶V_(丙酮)=1∶1)溶剂萃取,经干燥、浓缩,加入内标。先经C_(18)捕获柱分离开液相自带的酯类污染,再在第二根C_(18)柱子进行第二次分离,在质谱上使用MRM模式进行分析,内标法定量。结果表明,6种邻苯二甲酸酯在5~500 ng/mL范围内线性关系良好,相关系数(R)均大于0.999。检出限(LOD)为0.41~0.99μg/kg,定量限(LOQ)为1.23~2.97μg/kg;在3个浓度添加水平(5.00,10.0,50.0μg/kg)内,回收率为74.2%~110%,相对标准偏差为1.4%~12%。该方法快速、准确、稳定,能够满足污泥中6种邻苯二甲酸酯的痕量测定。

The accelerated solvent extraction-LCMS/MS method was established for the determination of six phthalates in sludge.The sludge was freeze-dried,ground through a 0.250 mm(60 mesh)sieve,and extracted with n-hexane acetone(1∶1,volume ratio)solvent on a accelerated solvent extractor.After drying and concentration,internal standards were added.The phthalates contamination in the liquid phase was separated by the C_(18) trapping column.The six phthalates in the six isotope internal calibration were separated by the second C_(18) columnh.analysised on mass spectrometry by MRM mode,and the internal standard method was used for quantification.The results showed that the linear relationships of the six phthalates were good in the range of 5~500 ng/mL,and the correlation coefficient(R)was greater than 0.999.Limit of detection(LOD)were 0.41~0.99μg/kg.Limit of quantification(LOQ)was 1.23~2.97μg/kg.During 3 horizontal spiking recovery tests(5.00,10.0,50.0μg/kg),the accuracy were 74.2%~110%,the precision were 1.4%~12%.The method is rapid,accurate and stable,and can satisfy the determination of trace phthalate in sludge.