| 英文摘要 |
To monitor pollutants containing polycyclic aromatic hydrocarbons (PAHs) and organochlorine pesticides (OCPs) and other persistent organic pollutants in sediment content is quite important. Most of these compounds are not easily degradable, bioaccumulative and toxic in the environment; therefore it is considered to control the focus of the UNEP project with the need for environmental monitoring. For this two types of compounds analyzed for sediment, the department of environmental protection administration announced " polycyclic aromatic hydrocarbons detection methods - gas chromatography (NIEA R812.20C) " and " soil, sediment and career organochlorine pesticide waste detection methods - gas chromatography assay method (NIEA M618.04C) ", etc. However, the complexity of the sediment matrix might disturbs the analytical results and hence it is not easy to obtain the representative data with announced methods, which would not fit sediment quality index limit demand. Therefore, the EPA handled the " sediment quality index project of low concentration limit detection technology establish and investigation " plan, which survey methods related references and announcements abroad as well as gas chromatography tandem mass spectrometry (GC/MS/MS) is as the main tool to create detection technology with the regulatory requirements. The main objective of this project has three items. The first is to collect references and establish analytical techniques about polycyclic aromatic hydrocarbons and organochlorine pesticide in sediments. This team has been collected 28 references about GC/MS/MS analysis of PAHs, OCPs and QuEChERs and also has completed the translation of literature summaries. The second item is to optimize the conditions of instruments, calibration curve, method validation and other data, the second items also have been built completely. The third item is to transfer the detection technology and write the format standard methods applicable to the draft analysis of PAHs and OCPs limit under sediment quality index. Overall, after appropriate pre-treatment and purification, the method detection limit (MDL) of PAHs and OCP with GC/MS/MS are 0.004 mg/kg and 0.0001 mg/kg respectively, which below regulatory control under should by GC/MS/MS analysis of quantitative limits. The calibration curve of the concentration range of PAHs was 0.1-1.0 μg/mL and that of OCPs was 50.7-101 ng/mL, which also shown a good linear relationship of the calibration curve with r2 were greater than 0.990 and standard deviation were less than 20 %. For the quality of the data, the blank sample (matrix blank) results showed no influences were imported in the system. QC sample results shown the recoveries of PAHs 62.6 to 107%, OCPs 85.0 to 127%.Spiked sample results shown that sediment samples had certain matrix effects for analysis, the recoveries of PAHs recoveries were 25.2 to 125.3 %, and OCPs were 24.0 to 192.4 %. Duplicate sample results shown the relative deviation of PAHs were 6.7 to 15.8 % and OCPs were 8.5 to 27.0 %. Compared results from different instruments such as GC/MS, GC/ECD and GC/MS/MS shown GC/MS/MS had less affects by significant matrix; The team also has completed 4 wetland basins and 29 sediment samples analysis in the item of investigation of 3 sediment basin, which surveyed the study of the EPA monitoring results of sediment samples presented a measuring point demand in recent years. Real samples detected 29 Naphthalene (0.038~0.359mg/kg), Acenaphthene (0.026~0.046 mg/kg) and one DDE-p,p' (0.0024 mg/kg).
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