Determination of Six Phthalates in Sludge by Rapid Solvent Extraction -LC-MS/MS
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 C18 trapping column.The six phthalates in the six isotope internal calibration were separated by the second C18 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 0.41～0.99 μg/kg.Limit of quantification(LOQ)was 1.23～2.97 μg/kg.During 3 horizontal spiking recovery tests(5.00,10.0,50.0 μg/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.
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