Microwave-Assisted Steam Distillation for Simple Determination of Polychlorinated Biphenyls and Organochlorine Pesticides in Sediments
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文摘
A novel sample extraction technique for polychlorinatedbiphenyls (PCBs) and organochlorine pesticides (OCPs)analysis using microwave-heating device is developed. Inthis study, microwave-assisted extraction (MAE) andsteam distillation techniques were combined. Desorptionof the anatytes from solid matrixes was accelerated withwater vapor which was generated by microwave irradiation. A sample holder in a commercial microwave extraction cell kept the sample from direct contact with theorganic solvent for analytes trapping during the treatmentprocess. Therefore, relatively clean extracts were obtainedwith small amount of solvents. Without any cleanup steps,the obtained extract could be analyzed with gas chromatograph/mass spectrometers (GC/MS). Six PCB congeners(PCB15, 28, 70, 101, 180, 194, 209) and three OCPs(-HCH, 4,4'-DDE, 4,4'-DDD) in two marine sedimentsamples (a sediment collected from a bay of KyusyuIsland, Japan, and a certified reference material NISTSRM1944) were analyzed by using this microwave-assisted steam distillation (MASD) technique and anotherextraction method (exhaustive steam distillation, MAE,and Soxhlet extraction); and comparisons of the resultsare shown in this report. Although recovery yields ofhighly chlorinated biphenyls (PCB180, 194, 209) andrelatively polar OCPs (-HCH, 4,4'-DDD) were low (30-60%) compared with other analytes (PCB15, 28, 70, 101,4,4'-DDE; recovery, 80-100%), use of isotope labeledinternal standards for the MASD technique gave comparable results with the values obtained by other extractionmethods and the certified values in the samples.

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