A high performance liquid chromatography tandem mass spectrometry/mass spectrometry(HPLC-MS/MS)protocol was developed for the determination of diphenylamine(DPA).Four productions of DPA were selected for qualitative a...A high performance liquid chromatography tandem mass spectrometry/mass spectrometry(HPLC-MS/MS)protocol was developed for the determination of diphenylamine(DPA).Four productions of DPA were selected for qualitative assay and the peak area of the main product ion for quantitation.By means of separation using an Agilent Extend-C18 column(CA,USA)(150 mm×4.6 mm,5μm)with methanol‑water(90:10)as the mobile phase,DPA was detected by electrospray ionization(ESI)tandem mass spectrometry in positive mode.The linearity of the peak area versus concentration ranged 5‑500 ng/mL,r^(2)=0.9978.The limit of detection(S/N=3)of this method was 0.3 ng/mL.This method is applicable for the determination of DPA in gunshot residue.展开更多
Gunshot Residue(GSR)has been a subject of interest for the forensic fraternity.Numerous analytical contributions towards the GSR analysis have been reported.Sensitivity,portability,cost-effectiveness,speed,etc.are suc...Gunshot Residue(GSR)has been a subject of interest for the forensic fraternity.Numerous analytical contributions towards the GSR analysis have been reported.Sensitivity,portability,cost-effectiveness,speed,etc.are such factors of electrochemical methods that have attracted the researchers across the globe to test the applicability of these as a potential analytical tool for forensic evaluation of GSR.With the development of scientific technology,efforts have been made towards the handheld device for the on-field analysis of GSR.Recently,chemometric treatment of data generated from the electrochemical analysis of GSR has offered more effective approach.It makes the analysis more conclusive and minimizes the chances of false-positive detection.It will be very fruitful to anticipate the analytical potential of electrochemical tools for GSR analysis.This article reviews the research progress towards the development of electrochemical sensor for GSR detection reported during 2013-2020 along with challenges and future perspectives.展开更多
The analysis of gunshot residue(GSR) has played an integral role within the legal system in relation to shooting cases. With a characteristic elemental composition of lead, antimony, barium, and a typically discrimina...The analysis of gunshot residue(GSR) has played an integral role within the legal system in relation to shooting cases. With a characteristic elemental composition of lead, antimony, barium, and a typically discriminative spheroidal morphology, the presence and distribution of GSR can aid in firearm investigations. In this experiment, three shots of low velocity rim-fire ammunition were fired over polished silicon collection substrates placed at six intervals over a 100 cm range. The samples were analysed using a Field Emission Gun Scanning Electron Microscope(FEG-SEM) in conjunction with an X-flash Energy Dispersive X-ray(EDX) detector, allowing for GSR particle analyses of composition and structure at the sub-micron level. The results of this experiment indicate that although classic spheroidal particles are present consistently throughout the entire range of samples their sizes vary significantly, and at certain distances from the firearm particles with an irregular morphology were discerned, forming "impactdisrupted" GSR particles, henceforth colloquially referred to as "splats". Upon further analysis, trends with regards to the formation of these splat particles were distinguished. An increase in splat frequency was observed starting at 10 cm from the firearm, with 147 mm^(-2) splat density, reaching a maximal flux at 40 cm(451 mm^(-2)), followed by a gradual decrease to the maximum range sampled. Moreover, the structural morphology of the splats changes throughout the sampling range. At the distances closest to the firearm, molten-looking particles were formed, demonstrating the metallic residues were in a liquid state when their flight path was disrupted. However, at increased distances-primarily where the discharge plume was at maximum dispersion and moving away from the firearm, the residues have had time to cool in-fight resulting in semi-congealed and solid particles that subsequently disrupted upon impact, forming more structured as well as disaggregated splats. The relative compositions of the charac展开更多
基金This study was supported by the Basal Research Fund Program of Institute of Forensic Science,Ministry of Public Security,China(2014JB006).
文摘A high performance liquid chromatography tandem mass spectrometry/mass spectrometry(HPLC-MS/MS)protocol was developed for the determination of diphenylamine(DPA).Four productions of DPA were selected for qualitative assay and the peak area of the main product ion for quantitation.By means of separation using an Agilent Extend-C18 column(CA,USA)(150 mm×4.6 mm,5μm)with methanol‑water(90:10)as the mobile phase,DPA was detected by electrospray ionization(ESI)tandem mass spectrometry in positive mode.The linearity of the peak area versus concentration ranged 5‑500 ng/mL,r^(2)=0.9978.The limit of detection(S/N=3)of this method was 0.3 ng/mL.This method is applicable for the determination of DPA in gunshot residue.
基金the University Grants Commission(UGC),Ministry of EducationGovernment of India,for providing financial assistance(UGC-JRF vide Letter No.190521040928)to the first author(AH).
文摘Gunshot Residue(GSR)has been a subject of interest for the forensic fraternity.Numerous analytical contributions towards the GSR analysis have been reported.Sensitivity,portability,cost-effectiveness,speed,etc.are such factors of electrochemical methods that have attracted the researchers across the globe to test the applicability of these as a potential analytical tool for forensic evaluation of GSR.With the development of scientific technology,efforts have been made towards the handheld device for the on-field analysis of GSR.Recently,chemometric treatment of data generated from the electrochemical analysis of GSR has offered more effective approach.It makes the analysis more conclusive and minimizes the chances of false-positive detection.It will be very fruitful to anticipate the analytical potential of electrochemical tools for GSR analysis.This article reviews the research progress towards the development of electrochemical sensor for GSR detection reported during 2013-2020 along with challenges and future perspectives.
文摘The analysis of gunshot residue(GSR) has played an integral role within the legal system in relation to shooting cases. With a characteristic elemental composition of lead, antimony, barium, and a typically discriminative spheroidal morphology, the presence and distribution of GSR can aid in firearm investigations. In this experiment, three shots of low velocity rim-fire ammunition were fired over polished silicon collection substrates placed at six intervals over a 100 cm range. The samples were analysed using a Field Emission Gun Scanning Electron Microscope(FEG-SEM) in conjunction with an X-flash Energy Dispersive X-ray(EDX) detector, allowing for GSR particle analyses of composition and structure at the sub-micron level. The results of this experiment indicate that although classic spheroidal particles are present consistently throughout the entire range of samples their sizes vary significantly, and at certain distances from the firearm particles with an irregular morphology were discerned, forming "impactdisrupted" GSR particles, henceforth colloquially referred to as "splats". Upon further analysis, trends with regards to the formation of these splat particles were distinguished. An increase in splat frequency was observed starting at 10 cm from the firearm, with 147 mm^(-2) splat density, reaching a maximal flux at 40 cm(451 mm^(-2)), followed by a gradual decrease to the maximum range sampled. Moreover, the structural morphology of the splats changes throughout the sampling range. At the distances closest to the firearm, molten-looking particles were formed, demonstrating the metallic residues were in a liquid state when their flight path was disrupted. However, at increased distances-primarily where the discharge plume was at maximum dispersion and moving away from the firearm, the residues have had time to cool in-fight resulting in semi-congealed and solid particles that subsequently disrupted upon impact, forming more structured as well as disaggregated splats. The relative compositions of the charac
