The Analysis Research Of Polychlorinated Biphenyl Pesticides And Heavy Metals In Marine Environment

In recent years, marine environmental pollution was affected by the terrestrialpollution, coastal and marine aquaculture, fishing and transportation, with the rapiddevelopment of economy. To marine environmental pollution condition, the paper hadstudied the analysis method and content level of polychlorinated biphenyls （PCBs）,pesticides and heavy metals in marine environmental.The optimization of the pretreatment in seawater, marine sediment and marineproduct was developed for Gas Chromatography-tandem Mass Spectrometry（GC-MS/MS） to determinne PCBs and residual pesticides. PCBs and pesticides werefull enriched by OasisHLB SPE cartridge in adding1%methanol and pH3.0. Allcompounds were eluted by6mL a mixture of hexane and dichlormethane （1:1, v: v）for chromatographic analysis. Calibration curves showed good linearity in the rangeof0.002to1ug·L^-1for34PCBs and76pesticides （R²>0.99）, and the limit ofdetection （LOD） ranged from0.10to208.48ng·L^-1. The number of compounds withthe average spiked recoveries of which were between60%and120%was103withRSD of0.5%to16.4%.The pretreatment method was Accelerated Solvent Extraction（ASE） which combined with solid-phase extraction （SPE） in marine sediments．Thesimultaneous extraction temperature and time were100℃and5min, respectively.Under sample extracted with a mixture of hexane and acetone （1:1,v:v） and cleanedup on a Carbon SPE cartridge, calibration curves showed good linearity in the rangeof1.0ug·kg^-1to500ug·kg^-1for32PCBs and71pesticides （R²>0.99）, and the limit ofdetection（LOD） ranged from0.23ug·kg^-1to108.43ug·kg^-1. The number ofcompounds with the average spiked recoveries of which were between70%and110%was102with RSD of0.1%to14.0%.The marine product samples were extracted with acetonitrile, dehydrated with salting out method and cleaned-up by gel permeationchromatography （GPC）. The GPC eluant collected from26min to50min wasconcentrated to1mL. Calibration curves showed good linearity in the range of1.0to500ug·kg^-1for34PCBs and76pesticides （R²﹥0.99）, and the limit of detection（LOD） ranged from0.02to43.4ug·kg^-1. The number of compounds with the averagespiked recoveries of which were between70%and110%was97with RSD of0.84%to24.5%. A microwave-assisted digestion-Inductively Coupled Plasma-MassSpectrometry （ICP-MS） method combined was developed for the simultaneousdetermination of12heavy metais in seawater, marine sediment and marine product.This method was accurate and easy to operate, and could be used for quantitative ofcomplex samples.Last article analysis method was applied to determine the Marine environmentactual samples and the established pretreatment method and instrument analysismethod were feasible and accuracy, which could play a monitoring role in the Marineenvironment quality conditions.