氣相色譜-質譜法檢測食品中多氯聯苯的研究

化工論文編號:HG208  論文字數:10726,頁數:31

目錄
 中文摘要 I
英文摘要 II
目錄 III
1 緒論 1
1.1實驗研究的目的、意義 2
1.2實驗的提取檢測方法 3
2 實驗部分 6
2.1 PCBs的物理和環境化學性質、固相萃取(SPE)技術簡介 6
2.1.1 PCBs的物理和環境化學性質 6
2.1.2  固相萃取(SPE) 7
2.2 實驗方案 7
2.3儀器和試劑 7
2.3.1儀器 7
2.3.2試劑及樣品 8
2.4操作方法 9
2.5測定 11
2.5.1氣相色譜分析條件 11
2.5.2質譜分析條件 11
2.5.3空白實驗 11
2.5.4方法限量 11
2.5.5回收率 11
2.5.6計算 12
3.結果與討論 13
結論 25
致謝 26
參考文獻 28

摘要：本文研究了食品中毒性較大的PCBs77、81、105、114、118、123、126、156、157、167、169、189測定方法，采用高速冷凍離心法、固相萃取小柱法對測試的式樣提純、凈化，采用高效分離的氣相色譜-電子捕獲檢測法(GC-ECD)，和高靈敏度、良好定性定量特點的質譜法(MS)，對食品中的多氯聯苯進行了檢測研究。
 通過對氣相色譜法中恒壓程序、恒流程序以及程序升溫法所得結果的比較，得出了氣質聯用分析多氯聯苯的最佳實驗操作條件。并且發現在氣相色譜法中采用載氣的恒線速度控制方式可以提高分離度，縮短分析時間。
 利用所建立的方法測定了食品中毒性較大的樣品，12種多氯聯苯的線性范圍0.001-2µg/L；相關系數r在0.99左右，回收率范圍在96.25%-117.5%之間，RSD%<21%，方法檢測限在0.4ppb-0.5ppb范圍內。
 隨著公眾對多氯聯苯（PCBs）認知度的提高，PCBs和PCBs污染廢物必須引起高度重視、合理收集和安全處置，以防止PCBs擴大環境污染。目前我國PCBs的研究工作主要集中在清單調查、環境污染水平監測和分析方法上，對PCBs的檢測技術尚缺乏研究，特別是食品中的PCBs殘留檢測亟待加強。隨著我國履行斯德哥爾摩公約的國家行動方案的制定和開展，PCBs的檢測技術將成為持久性有機污染物控制領域的研究熱點之一。
 
關鍵詞：多氯聯苯；電子捕獲檢測器；氣相色譜-質譜；冷凍離心；固相萃取；

Abstract:  This paper studies determination of larger toxicity the PCBs77, 81,105,114, 118,123,126,156,157,167,169,189 in food, high-speed freezing centrifuge, solid phase extraction column test method style purification, purification, separation with high efficiency gas chromatography - electron capture detection (GC-ECD), and high sensitivity, good qualitative and quantitative characteristics of mass spectrometry (MS).       Through the constant pressure on the gas chromatography process, constant process and the programmed temperature method comparison of results obtained with GC-MS operating conditions for optimum PCBs. And found that the use of gas chromatography carrier gas of constant linear speed control method can improve the separation, shortening analysis time.      With the established method of determination of toxicity of food in larger samples, 12 kinds of PCBs in the linear range of 0.001-2μg / L; correlation coefficient r is about 0.99, recoveries of 96.25% -117.5%, and RSD% <21%, detection limit in 0.4ppb-0.5ppb range.
 With the public polychlorinated biphenyls (PCBs) increase awareness, PCBs and PCBs contaminated waste must be identified as soon as possible, reasonable collection and safe disposal, to prevent PCBs continue to pollute the environment. PCBs present our research work mainly in the list of investigations, the level of environmental pollution monitoring and analysis methods for detection of PCBs is still a lack of technology. Along with the Stockholm Convention implementation of national action programs to develop and carry out, PCBs in the detection technology will be a persistent organic pollutant control one of the hot area of research.

Keyword: PCBs; electron capture detector; gas chromatography - mass spectrometry; freeze centrifuged; solid phase extraction;