采用同位素稀释高分辨气相色谱-高分辨质谱法(isotope dilution high resolution gas chromatography and high resolution mass spectrometry,ID-HRGC-HRMS)测定土壤样品中二恶英类化合物(polychlorinated dibenzo-p-dioxins and diben...采用同位素稀释高分辨气相色谱-高分辨质谱法(isotope dilution high resolution gas chromatography and high resolution mass spectrometry,ID-HRGC-HRMS)测定土壤样品中二恶英类化合物(polychlorinated dibenzo-p-dioxins and dibenzofurans,PCDD/Fs)的等价毒性当量(toxic equivalent quantity,TEQ)。讨论并确定了测定土壤样品中二恶英类化合物2,3,7,8位异构体不确定度的来源并合成了各异构体的相对标准不确定度;在此基础上,计算了3种等价毒性当量因子(toxic equivalent factor,TEF)框架下土壤样品中PCDD/Fs的TEQ浓度及其合成不确定度和扩展不确定度。展开更多
Labeled polychlorinated dibenzo-p-dioxins and dibenzofurans(PCDD/Fs)were extracted by three different methods,i.e.,soxhlet extraction,hot extraction and accelerated solvent extraction(ASE).The PCDD/Fs were detected by...Labeled polychlorinated dibenzo-p-dioxins and dibenzofurans(PCDD/Fs)were extracted by three different methods,i.e.,soxhlet extraction,hot extraction and accelerated solvent extraction(ASE).The PCDD/Fs were detected by high resolution gas chromatography-high resolution mass spectrometry.Comparisons of the three methods were carried out by recovery of PCDD/Fs,solvent consumption and extraction time.The results showed that all of the method could extract labeled PCDD/Fs efficiently.ASE was a time saving procedure with lowest consumption of solvents compared with the other two methods.展开更多
A rapid pretreatment method of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) in soil and analysis by high resolution gas chromatograph-high resolution mass spectrometry was present.The extraction and a...A rapid pretreatment method of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) in soil and analysis by high resolution gas chromatograph-high resolution mass spectrometry was present.The extraction and alumina clean up of PCDD/Fs in soil was achieved by accelerated solvent extractor.Then the multi-layer silica-gel column was used for further clean up.The whole method has been evaluated on certified reference soil and farm soil.Accuracy and precision of this method was tested with satisfactory results.展开更多
利用高分辨气相色谱/高分辨质谱联用仪(HRGC/HRMS)和高分辨气相色谱/低分辨质谱仪(HRGC/LRMS)对实际生物样品中二恶英(polychlorinated dibenzo-p-dioxins and dibenzofurans,PCDD/Fs)的分析过程中13 C标记的2,3,7,8-四氯代二苯并呋喃(1...利用高分辨气相色谱/高分辨质谱联用仪(HRGC/HRMS)和高分辨气相色谱/低分辨质谱仪(HRGC/LRMS)对实际生物样品中二恶英(polychlorinated dibenzo-p-dioxins and dibenzofurans,PCDD/Fs)的分析过程中13 C标记的2,3,7,8-四氯代二苯并呋喃(13 C12-2,3,7,8-TCDF)监测碎片离子通道的两个常见干扰峰进行了分析鉴定。通过实际样品分析结果首先推测这两个干扰峰可能为有机氯农药类化合物滴滴涕(DDT)降解产物滴滴伊(DDE)的两个异构体,其次采用DDE的标准溶液(包括o,p′-DDE和p,p′-DDE)进行分析确认。通过HRGC/HRMS的色谱峰分离效果分析、色谱保留时间匹配以及与DDE碎片离子的理论丰度比进行比较,最终确认实际样品分析中的两个干扰峰依次为o,p′-DDE和p,p′-DDE。本文可为生物样品中二恶英的准确识别提供重要参考。展开更多
文摘采用同位素稀释高分辨气相色谱-高分辨质谱法(isotope dilution high resolution gas chromatography and high resolution mass spectrometry,ID-HRGC-HRMS)测定土壤样品中二恶英类化合物(polychlorinated dibenzo-p-dioxins and dibenzofurans,PCDD/Fs)的等价毒性当量(toxic equivalent quantity,TEQ)。讨论并确定了测定土壤样品中二恶英类化合物2,3,7,8位异构体不确定度的来源并合成了各异构体的相对标准不确定度;在此基础上,计算了3种等价毒性当量因子(toxic equivalent factor,TEF)框架下土壤样品中PCDD/Fs的TEQ浓度及其合成不确定度和扩展不确定度。
文摘Labeled polychlorinated dibenzo-p-dioxins and dibenzofurans(PCDD/Fs)were extracted by three different methods,i.e.,soxhlet extraction,hot extraction and accelerated solvent extraction(ASE).The PCDD/Fs were detected by high resolution gas chromatography-high resolution mass spectrometry.Comparisons of the three methods were carried out by recovery of PCDD/Fs,solvent consumption and extraction time.The results showed that all of the method could extract labeled PCDD/Fs efficiently.ASE was a time saving procedure with lowest consumption of solvents compared with the other two methods.
文摘A rapid pretreatment method of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) in soil and analysis by high resolution gas chromatograph-high resolution mass spectrometry was present.The extraction and alumina clean up of PCDD/Fs in soil was achieved by accelerated solvent extractor.Then the multi-layer silica-gel column was used for further clean up.The whole method has been evaluated on certified reference soil and farm soil.Accuracy and precision of this method was tested with satisfactory results.
