For purpose of purification and enrichment, environmental samples usually need to be pretreated before analysis because of low concentration of residual organic matters. Solid-phase extraction （SPE） is one of the fr...For purpose of purification and enrichment, environmental samples usually need to be pretreated before analysis because of low concentration of residual organic matters. Solid-phase extraction （SPE） is one of the frequently used methods of pretreatment. This article introduces the methodological principle and flow channel of SPE as well as the categories of frequently used small extraction column, analyzes the application of online SPE technology in environmental analysis, generalizes the advantages of online SPE and sets forth its developmental trend.展开更多
A simple and efficient dithizone-functionalized solid-phase extraction(SPE)procedure,online coupled with high-performance liquid chromatography(HPLC)-inductively coupled plasma mass spectrometry,was developed for the ...A simple and efficient dithizone-functionalized solid-phase extraction(SPE)procedure,online coupled with high-performance liquid chromatography(HPLC)-inductively coupled plasma mass spectrometry,was developed for the first time for enrichment and determination of ultra-trace mercury(Hg)species(inorganic divalent Hg(Hg(Ⅱ)),methylmercury(CH_(3)Hg(Ⅱ))and ethylmercury(C_(2)H_(5)Hg(Ⅱ))in cereals and environmental samples.In the proposed method,functionalization of the commercial C_(18) column with dithizone,enrichment,and elution of the above Hg species can be completed online with the developed SPE device.A simple solution of 2-mercaptoethanol(1%(V/V))could be used as an eluent for both the SPE and HPLC separation of Hg species,significantly simplifying the method and instrumen-tation.The online SPE method was optimized by varying dithizone dose,2-mercaptoethanol concentration,and sample volume.In addition,the effect of pH,coexisting interfering ions,and salt effect on the enrichment was also discussed.Under the optimized conditions,the detection limits of Hg species for 5 mL water sample were 0.15 ng/L for Hg(Ⅱ),0.07 ng/L for CH_(3)Hg(Ⅱ),and 0.04 ng/L for C_(2)H_(5)Hg(Ⅱ)with recoveries in the range of 85%-100%.The developed dithizone-functionalized C_(18) SPE column can be reused after a single function-alization,which significantly simplifies the enrichment step.Moreover,the stability of Hg species enriched on the SPE column demonstrated its suitability for field sampling of Hg species for later laboratory analysis.This environment-friendly method offers a robust tool to detect ultra-trace Hg species in cereals and environmental samples.展开更多
文摘For purpose of purification and enrichment, environmental samples usually need to be pretreated before analysis because of low concentration of residual organic matters. Solid-phase extraction （SPE） is one of the frequently used methods of pretreatment. This article introduces the methodological principle and flow channel of SPE as well as the categories of frequently used small extraction column, analyzes the application of online SPE technology in environmental analysis, generalizes the advantages of online SPE and sets forth its developmental trend.
基金This work was supported by the National Key Research and Development Project(No.2020YFA0907400)the National Natural Science Foundation of China(Nos.21777178,21976193)+1 种基金Y.Yin acknowledges the supports from the National Young Top-Notch Talents(No.W03070030)the Youth Innovation Promotion Association of the Chinese Academy of Sciences(No.Y202011).
文摘A simple and efficient dithizone-functionalized solid-phase extraction(SPE)procedure,online coupled with high-performance liquid chromatography(HPLC)-inductively coupled plasma mass spectrometry,was developed for the first time for enrichment and determination of ultra-trace mercury(Hg)species(inorganic divalent Hg(Hg(Ⅱ)),methylmercury(CH_(3)Hg(Ⅱ))and ethylmercury(C_(2)H_(5)Hg(Ⅱ))in cereals and environmental samples.In the proposed method,functionalization of the commercial C_(18) column with dithizone,enrichment,and elution of the above Hg species can be completed online with the developed SPE device.A simple solution of 2-mercaptoethanol(1%(V/V))could be used as an eluent for both the SPE and HPLC separation of Hg species,significantly simplifying the method and instrumen-tation.The online SPE method was optimized by varying dithizone dose,2-mercaptoethanol concentration,and sample volume.In addition,the effect of pH,coexisting interfering ions,and salt effect on the enrichment was also discussed.Under the optimized conditions,the detection limits of Hg species for 5 mL water sample were 0.15 ng/L for Hg(Ⅱ),0.07 ng/L for CH_(3)Hg(Ⅱ),and 0.04 ng/L for C_(2)H_(5)Hg(Ⅱ)with recoveries in the range of 85%-100%.The developed dithizone-functionalized C_(18) SPE column can be reused after a single function-alization,which significantly simplifies the enrichment step.Moreover,the stability of Hg species enriched on the SPE column demonstrated its suitability for field sampling of Hg species for later laboratory analysis.This environment-friendly method offers a robust tool to detect ultra-trace Hg species in cereals and environmental samples.
