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The Determination Of PCBs And PAHs In Meat And Sea Food By GC-QqQ-MS/MS

Posted on:2013-11-24Degree:MasterType:Thesis
Country:ChinaCandidate:L G HuoFull Text:PDF
GTID:2231330374481775Subject:Chemical Engineering
Abstract/Summary:PDF Full Text Request
The problems of Persistent Organic Pollutants (POPs) have always been greatly concerned by both governments and organizations. They are easy to accumulate in organism through the biological concentration process for their high toxicity, durability, and transference and biological characteristics. So they can make potential threat to the ecological and human. PCBs and PAHs are both belonged to the Persistent Organic Pollutants.A new method was developed to determine the contents of PCBs and PAHs in meat and sea food by gas chromatography-triple quadrupole mass spectrometry (GC-QqQ-MS/MS). The selected reaction monitoring (SRM) mode was used.The dissertation consists three parts.Chapter1:The general situation of PCBs and PAHs was reviewed. The source and the toxicity of PCBs and PAHs were introduced. Meanwhile, sample pretreatment techniques and analytical techniques which were usually used to analysis the PCBs and PAHs were summarized. Sample pretreatment techniques mainly have soxhlet extraction, accelerated solvent extraction, solid phase extraction, solid phase micro extraction, ultrasonic extraction, microwave assisted extraction, supercritical fluid extraction, gel permeation chromatography, matrix solid phase dispersion and cloud point extraction. Analytical techniques are as follows:gas chromatography, gas chromatography-mass spectrum, enzyme-linked immunosorbent assay, surface plasmon resonance and so on.Chapter2:A new method was developed to determine the PCBs in meat and sea food by gas chromatography-triple quadrupole mass spectrometry (GC-QqQ-MS/MS). The method was based on ultrasonic extraction and Florisil column cleaning. The GC-QqQ-MS/MS was used in selected reaction monitoring (SRM) mode to determine the target compounds. The reliability of the method was verified. Recoveries of the12PCBs for spiked samples ranged from70.4%to100.6%and the relative standard deviations (RSD) were from0.5%to12.6%. The limits of detection (LODs) ranged from0.006to0.009μg/kg and the limits of quantitation (LOQs) ranged from0.02to 0.03μg/kg. The mass spectrum conditions (the selection of parent ion and product ion, optimization of collision energy) were discussed at the same time.Chapter3:A new method was developed to determine the contents of PAHs in fish by gas chromatography-triple quadrupole mass spectrometry (GC-QqQ-MS/MS) with SRM mode. In this method, ultrasonic extraction and florisil column cleaning were used as the sample pretreatment. Recoveries of the16PAHs for spiked samples were between68.5%and106.3%, the relative standard deviations (RSD) were between0.3%and17.8%. The limits of detection (LODs) ranged from0.024to0.06μg/kg and the limits of quantitation (LOQs) ranged from0.08to0.2μg/kg. The influence of different elution solvent to recoveries in SPE and the matrix effects were also discussed.
Keywords/Search Tags:PCBs, PAHs, Ultrasonic extraction, Gas chromatography-triplequadrupole mass spectrometry
PDF Full Text Request
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