環保專案成果報告查詢系統

專案計畫編號	EPA-102-1604-02-01
經費年度	102
計畫經費	2,720 千元
專案開始日期	2013/04/22
專案結束日期	2013/12/31
專案主持人	黃平志
主辦單位	環檢所
承辦人	施育林
執行單位	正修科技大學
專案分類	環境監測及檢測
中文關鍵字	多環芳香烴;有機氯農藥;氣相層析串聯式質譜儀
英文關鍵字	Polycyclic Aromatic Hydrocarbons, PAHs;Organochlorine pesticides, OCPs;GC/MS/MS
協同主持人	桂椿雄
共同主持人
計畫聯絡人	吳漢鐘
計畫聯絡電話	07-7358800#6320
計畫聯絡信箱	wqp@csu.edu.tw

中文摘要	在底泥污染物的監測中，包含多環芳香烴(PAHs)及有機氯農藥(OCPs)等持久性有機污染物的含量為相當重要之調查對象，這類化合物在環境中多半具有不易降解、生物累積及毒性加成等特性，故被聯合國環境規劃署視為管制重點項目而具有環境監測的必要性。針對底泥中此兩類化合物之分析，我國行政院環境保護署係公告「多環芳香族碳氫化合物檢測方法－氣相層析法(NIEA R812.20C)」及「土壤、底泥及事業廢棄物中有機氯農藥檢測方法－氣相層析儀法(NIEA M618.04C)」等檢測方法，惟因底泥基質複雜具甚多干擾，故依現有公告方法之檢測技術所得結果，在欲符於土壤及地下水污染整治法中底泥品質指標下限值設立需求的條件下，不易取得具代表性之數據，鑑此，環保署係辦理本「底泥品質指標項目低濃度限值檢測技術建立及調查」計畫，調查彙整國內外相關參考文獻及公告方法，以氣相層析串聯式質譜儀(GC/MS/MS)為主要分析工具，建立符於法規需求之檢測技術。本計畫具三大項主要目標，已蒐集並建立國內外底泥中多環芳香烴及有機氯農藥分析技術28篇以GC/MS/MS分析PAHs、OCPs及QuEChERs的參考文獻，並已完成文獻中摘要等重點部分之翻譯，另儀器分析之最適化條件、檢量線、方法驗證等數據亦建置完成，並依計畫要求完成檢測技術轉移，及依環境檢驗所標準方法格式撰寫適用於底泥品質指標下限值中PAHs及OCPs之分析方法草案。整體而言，經由適當前處理與淨化流程後，以GC/MS/MS分析PAHs與OCPs所得之方法偵測極限(MDL)分別為0.004 mg/kg及0.0001 mg/kg，皆低於法規管制下限值，即底泥樣品中應可由GC/MS/MS定量分析。另本方法所建立之檢量線濃度範圍落於PAHs為0.1-1.0 μg/mL，OCPs則為50.7-101 ng/mL，各檢量線的線性關係良好，r2皆大於0.990且感應因子之相對標準偏差≦20％。而品質數據部分，由空白樣品(基質空白)分析結果顯示無污染導入。查核樣品分析結果PAHs回收率62.6~107 %，OCPs則為85.0~127 %。添加樣品分析結果得知底泥樣品基質效應對底泥樣品分析有一定影響，PAHs回收率25.2~125.3 %，OCPs則為24.0~192.4 %。重複樣品分析結果PAHs相對偏差6.7~15.8 %，OCPs則為8.5~27.0 %。與GC/MS及GC/ECD所得之分析結果比較，顯示GC/MS/MS所得測值受基質干擾影響較不顯著；在調查國內3處流域底泥中PAHs及OCPs含量之工作項目，參考近幾年環保署針對底泥樣品監測的研究成果，提出有調查需求之測點，並已完成4個流域與1個濕地29件底泥樣品分析，其中29件樣品檢出Naphthalene (0.038~0.359 mg/kg)，23件樣品檢出Acenaphthene (0.026~0.046 mg/kg)，1件樣品檢出DDE-p,p' (0.0024 mg/kg)。
中文關鍵字	多環芳香烴;有機氯農藥;氣相層析串聯式質譜儀

中文摘要

在底泥污染物的監測中，包含多環芳香烴(PAHs)及有機氯農藥(OCPs)等持久性有機污染物的含量為相當重要之調查對象，這類化合物在環境中多半具有不易降解、生物累積及毒性加成等特性，故被聯合國環境規劃署視為管制重點項目而具有環境監測的必要性。針對底泥中此兩類化合物之分析，我國行政院環境保護署係公告「多環芳香族碳氫化合物檢測方法－氣相層析法(NIEA R812.20C)」及「土壤、底泥及事業廢棄物中有機氯農藥檢測方法－氣相層析儀法(NIEA M618.04C)」等檢測方法，惟因底泥基質複雜具甚多干擾，故依現有公告方法之檢測技術所得結果，在欲符於土壤及地下水污染整治法中底泥品質指標下限值設立需求的條件下，不易取得具代表性之數據，鑑此，環保署係辦理本「底泥品質指標項目低濃度限值檢測技術建立及調查」計畫，調查彙整國內外相關參考文獻及公告方法，以氣相層析串聯式質譜儀(GC/MS/MS)為主要分析工具，建立符於法規需求之檢測技術。本計畫具三大項主要目標，已蒐集並建立國內外底泥中多環芳香烴及有機氯農藥分析技術28篇以GC/MS/MS分析PAHs、OCPs及QuEChERs的參考文獻，並已完成文獻中摘要等重點部分之翻譯，另儀器分析之最適化條件、檢量線、方法驗證等數據亦建置完成，並依計畫要求完成檢測技術轉移，及依環境檢驗所標準方法格式撰寫適用於底泥品質指標下限值中PAHs及OCPs之分析方法草案。整體而言，經由適當前處理與淨化流程後，以GC/MS/MS分析PAHs與OCPs所得之方法偵測極限(MDL)分別為0.004 mg/kg及0.0001 mg/kg，皆低於法規管制下限值，即底泥樣品中應可由GC/MS/MS定量分析。另本方法所建立之檢量線濃度範圍落於PAHs為0.1-1.0 μg/mL，OCPs則為50.7-101 ng/mL，各檢量線的線性關係良好，r2皆大於0.990且感應因子之相對標準偏差≦20％。而品質數據部分，由空白樣品(基質空白)分析結果顯示無污染導入。查核樣品分析結果PAHs回收率62.6~107 %，OCPs則為85.0~127 %。添加樣品分析結果得知底泥樣品基質效應對底泥樣品分析有一定影響，PAHs回收率25.2~125.3 %，OCPs則為24.0~192.4 %。重複樣品分析結果PAHs相對偏差6.7~15.8 %，OCPs則為8.5~27.0 %。與GC/MS及GC/ECD所得之分析結果比較，顯示GC/MS/MS所得測值受基質干擾影響較不顯著；在調查國內3處流域底泥中PAHs及OCPs含量之工作項目，參考近幾年環保署針對底泥樣品監測的研究成果，提出有調查需求之測點，並已完成4個流域與1個濕地29件底泥樣品分析，其中29件樣品檢出Naphthalene (0.038~0.359 mg/kg)，23件樣品檢出Acenaphthene (0.026~0.046 mg/kg)，1件樣品檢出DDE-p,p' (0.0024 mg/kg)。

中文關鍵字

多環芳香烴;有機氯農藥;氣相層析串聯式質譜儀

類型	檔名	檔案大小	說明	最新版公開日期
期末報告	EPA-102-1604-02-01.pdf	7MB	期末報告定稿本	2014/2/1 上午 12:00:00

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).
英文關鍵字	Polycyclic Aromatic Hydrocarbons, PAHs;Organochlorine pesticides, OCPs;GC/MS/MS

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).

英文關鍵字

Polycyclic Aromatic Hydrocarbons, PAHs;Organochlorine pesticides, OCPs;GC/MS/MS