An effective method for determination of polychlorinated biphenyls (PCBs) in contaminated soil by means of accelerate solvent extraction (ASE) followed with gas chromatography-mass spectrometry (GC/MS) was studied. Th...An effective method for determination of polychlorinated biphenyls (PCBs) in contaminated soil by means of accelerate solvent extraction (ASE) followed with gas chromatography-mass spectrometry (GC/MS) was studied. The reliability and efficiency of ASE for extracting PCBs from contaminated soil has been investigated by comparing with soxhlet extraction. The influence of extract parameters such as temperature, static cycle were discussed. RSD was 1.8%-9.3% .The detection limits is in the range of 0.33-1.33μg/kg. The result showed the method was rapid, sensitive and economic.展开更多
目的建立加速溶剂萃取-凝胶渗透色谱-气相色谱-串联质谱法同时测定鱼类中7种新型有机污染物(咔唑和卤代咔唑类化合物)的分析方法。方法样品与硅藻土研磨混匀后经加速溶剂萃取仪提取,使用凝胶渗透色谱法净化并氮吹至近干,用1mL丙酮复溶...目的建立加速溶剂萃取-凝胶渗透色谱-气相色谱-串联质谱法同时测定鱼类中7种新型有机污染物(咔唑和卤代咔唑类化合物)的分析方法。方法样品与硅藻土研磨混匀后经加速溶剂萃取仪提取,使用凝胶渗透色谱法净化并氮吹至近干,用1mL丙酮复溶。目标化合物采用多反应监测(multiplereactionmonitoring,MRM)模式分析,外标法进行定量。结果咔唑、3-氯咔唑、3-溴咔唑和3,6-二氯咔唑在0.5~50.0μg/kg范围内线性关系良好,相关系数r>0.997;3,6-二溴咔唑、2,7-二溴咔唑和1,3,6,8-四溴咔唑在1.0~100.0μg/kg范围内线性关系良好,相关系数r>0.998。定量限(limits of quantification,LOQs)在0.50~1.00μg/kg之间,在各目标物的1LOQs、2LOQs和10LOQs3个加标水平下,7种咔唑和卤代咔唑类化合物的平均回收率为87.22%~107.27%,相对标准偏差(relative standard deviations,RSDs)为2.70%~8.17%(n=6)。结论该方法自动化程度高、灵敏度高、稳定性好,适用于鱼类中7种咔唑和卤代咔唑类化合物的检测。展开更多
文摘An effective method for determination of polychlorinated biphenyls (PCBs) in contaminated soil by means of accelerate solvent extraction (ASE) followed with gas chromatography-mass spectrometry (GC/MS) was studied. The reliability and efficiency of ASE for extracting PCBs from contaminated soil has been investigated by comparing with soxhlet extraction. The influence of extract parameters such as temperature, static cycle were discussed. RSD was 1.8%-9.3% .The detection limits is in the range of 0.33-1.33μg/kg. The result showed the method was rapid, sensitive and economic.
文摘目的建立加速溶剂萃取-凝胶渗透色谱-气相色谱-串联质谱法同时测定鱼类中7种新型有机污染物(咔唑和卤代咔唑类化合物)的分析方法。方法样品与硅藻土研磨混匀后经加速溶剂萃取仪提取,使用凝胶渗透色谱法净化并氮吹至近干,用1mL丙酮复溶。目标化合物采用多反应监测(multiplereactionmonitoring,MRM)模式分析,外标法进行定量。结果咔唑、3-氯咔唑、3-溴咔唑和3,6-二氯咔唑在0.5~50.0μg/kg范围内线性关系良好,相关系数r>0.997;3,6-二溴咔唑、2,7-二溴咔唑和1,3,6,8-四溴咔唑在1.0~100.0μg/kg范围内线性关系良好,相关系数r>0.998。定量限(limits of quantification,LOQs)在0.50~1.00μg/kg之间,在各目标物的1LOQs、2LOQs和10LOQs3个加标水平下,7种咔唑和卤代咔唑类化合物的平均回收率为87.22%~107.27%,相对标准偏差(relative standard deviations,RSDs)为2.70%~8.17%(n=6)。结论该方法自动化程度高、灵敏度高、稳定性好,适用于鱼类中7种咔唑和卤代咔唑类化合物的检测。