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
Determination methods of trace Hg(Ⅱ),Cu(Ⅱ) and Cd(Ⅱ) were established based on the combination of LPME of dithizone-chelate for high enrichment,strip shape sampling-TLC and digital image-processing for quantitative...Determination methods of trace Hg(Ⅱ),Cu(Ⅱ) and Cd(Ⅱ) were established based on the combination of LPME of dithizone-chelate for high enrichment,strip shape sampling-TLC and digital image-processing for quantitative analysis.Detection limits of Cu(Ⅱ),Hg(Ⅱ) and Cd(Ⅱ) were 1.5 ng/mL,1.3 ng/mL and 2.5ng/mL,respectively.RSDs were 1.2%,4.0% and 2.7%,respectively.The proposed methods have the advantages of convenience,sensitiveness,precise and economicls.The methods were applied to the determination of these elements in a pool water and mud,with satisfying results.展开更多
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.
基金Supported by the National Natural Science Foundation of China( No.2 0 0 2 5 312,2 9992 5 90 - 3) and the Major State BasicResearch Development Program( No.G2 0 0 0 0 7810 3)
文摘Determination methods of trace Hg(Ⅱ),Cu(Ⅱ) and Cd(Ⅱ) were established based on the combination of LPME of dithizone-chelate for high enrichment,strip shape sampling-TLC and digital image-processing for quantitative analysis.Detection limits of Cu(Ⅱ),Hg(Ⅱ) and Cd(Ⅱ) were 1.5 ng/mL,1.3 ng/mL and 2.5ng/mL,respectively.RSDs were 1.2%,4.0% and 2.7%,respectively.The proposed methods have the advantages of convenience,sensitiveness,precise and economicls.The methods were applied to the determination of these elements in a pool water and mud,with satisfying results.
