The Application Of Chromatography-Mass Spectrometry Technique In The Analysis Of Organic Pollutant Residues

The quality and safety of food is one of the important factors influencing our life quality. However, the presence of organic pollutants residues in food has become one of the serious problems that have greatly attracted government and organization's concerns. As the maximum residue levels of organic pollutants adopted by the legislation in the world become more and more strict, it is very important to establish simple, fast and efficient analytical methods for the determination of these organic pollutants. In this thesis, novel analytical methods has been established for the determination of organic pollutants residues in animal fat and rehmannia with chromatography-mass spectrometry techniques.The dissertation consists of three chapters.The first chapter:The sample pre-treatment methods and the chromatographic analysis technologie were reviewed on the basis of 170 references. Samplepre-treatment methods such as homogenizing extraction, shaking extraction, ultrasonic extraction, solid phase extraction (SPE), solid phase microextraction (SPME), supercritical fluid extraction (SFE), accelerated solvent extraction (ASE), microwave assisted extraction (MAE), liquid-liquid extraction (LLE) and gel permeation chromatography (GPC) technique were introduced. The principles and applications of Gas chromatography (GC), liquid chromatography (LC) and mass spectrometry (MS) were summarized.The second chapter:A novel method was established for the determination of 15 polycyclic aromatic hydrocarbons (PAHs) residues in rehmannia by using solid phase extraction-gas chromatography-tandem mass spectrometry (GC-MS/MS). The extraction efficiency of three kinds of solvent and the purification effect of eight kinds of purification methods were investigated. Finally, cyclohexane-acetone (1:1, V/V) was selected as extraction solvent and PSA solid phase extraction was employed for purification. The limit of detection for 15 polycyclic aromatic hydrocarbons in rehmannia was between 0.10μg/kg and 11.00μg/kg. The average recoveries of the pesticide residues were between 68.1% and 106.9%, and the relative standard deviations were between 1.2% and 19.6%.The third chapter:The analysis of 111 pesticides residues in animal fat was carried out by using gel permeation chromatography (GPC) purification-liquid chromatography-tandem mass spectrometry (LC-MS/MS) method. The effects of seven kinds of solvent, three kinds of extraction methods and three kinds of purification methods were investigated for the extraction and purification of 111 kinds of pesticides. Finally, acetonitrile was selected as extraction solvent, homogeneous extraction and gel permeation chromatography was employed as extraction and purification methods. The limits of detection for 111 pesticides in animal fat were between 0.20μg/kg and 0.96 mg/kg. The average recoveries of the pesticide residues were between 60.0% and 119.9%, and the relative standard deviations were between 0.6% and 19.8%.