Analysis of Arsenic Compounds in Blood and Urine by HPLC-ICP-MS / 法医学杂志

Objective To establish an analysis method for the detection of 6 arsenic compounds [AsC, AsB, As(Ⅲ), DMA, MMA and As(V)] in blood and urine by high-performance liquid chromatography-inductively coupled plasma-mass spectrometry(HPLC-ICP-MS), and apply it to real cases. Methods Triton was used to damage cells, and then EDTA·2Na·2H2O was used to complex arsenic compounds in cells, and sonication and protein deposition by acetonitrile were performed for sample pretreatment. With the mobile phase consisted of ammonium carbonate and ultrapure water, gradient elution was per-formed for obtaining the arsenic compounds in samples, which were analysed by ICP-MS with Hamilton PRP-X100 column. Results The limits of detection in blood were 1.66-10 ng/mL, while the lower limits of quantitation in blood ranged from 5 to 30 ng/mL. The limits of detection in urine were 0.5-10 ng/mL, while the lower limits of quantitation in urine were 5-30 ng/mL. The relative standard deviation of inter-day and intra-day precisions was less than 10%. This method had been successfully applied to 3 cases. Conclusion This study has established an analysis method for detecting 6 common arsenic compounds in blood and urine, which can be used to detect the arsenic compounds in the blood and urine from ar-senic poisoning cases as well as the patients under arsenic treatment.

Biomonitoring of 33 Elements in Blood and Urine Samples from Coastal Populations in Sanmen County of Zhejiang Province / 法医学杂志

OBJECTIVE@#To determine the normal reference values of 33 elements, Ag, Al, As, Au, B, Ba, Be, Ca, Cd, Co, Cr, Cs, Cu, Fe, Ga, Hg, Li, Mg, Mn, Mo, Ni, Pb, Rb, Sb, Se, Sr, Th, Ti, Tl, U, V, Zn and Zr, in the blood and urine samples from the general population in Sanmen County of Zhejiang province, a typical coastal area of eastern China.@*METHODS@#The 33 elements in 272 blood and 300 urine samples were determined by inductively coupled plasma-mass spectrometry (ICP-MS). The normality test of data was conducted using SPSS 17.0 Statistics. The data was compared with other reports.@*RESULTS@#The normal reference values of the 33 elements in the blood and urine samples from the general population in Sanmen County were obtained, which of some elements were found to be similar with other reports, such as Co, Cu, Mn and Sr, while As, Cd, Hg and Pb were generally found to be higher than those previously reported. There was a wide variation between the reports from different countries in blood Ba.@*CONCLUSION@#The normal reference values of the 33 elements in the blood and urine samples from the general population in Sanmen County are established, and successfully applied to two poisoning cases.

Normal Range of 33 Elements in Blood Samples from General Population in Hunan Province / 法医学杂志

OBJECTIVE@#To determine the normal range of the 33 elements (Li, Be, B, Mg, Al, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Zr, Mo, Ag, Cd, Sb, Cs, Ba Au, Hg, Tl, Pb, Th and U) in human whole blood of general population in Hunan province.@*METHODS@#Blood samples were analyzed by inductively coupled plasma-mass spectrometry (ICP-MS) to determine the normal range. The influences of district, gender and age to the element content in blood samples were also observed.@*RESULTS@#The normal range of 33 elements in blood samples from general population in Hunan province were obtained. Gender was shown to statistically influence the concentrations of B, Mg, Ca, Ti, Mn, Fe, Co, Cu, Zn, As, Se, Rb, Sr, Ag, Cd, Cs, Hg and Pb (P < 0.05), while age was shown to influence the concentrations of Co, Ni, Cs and Hg in women (P < 0.05) as well as Cu, Se and Hg in men (P < 0.05).@*CONCLUSION@#Although there are variables in different districts, the normal ranges of trace element in blood of the four cities in Hunan province are established.

Method development and validation for determining 1,3-butadiene in human blood by gas chromatography-mass spectrometry and head-space gas chromatography / 法医学杂志

To develop a simple, validated method for identifying and quantifying 1,3-butadiene (BD) in human blood by gas chromatography-mass spectrometry (GC-MS) and head-space gas chromatography (HS-GC). BD was identified by GC-MS and HS-GC, and quantified by HS-GC. The method showed that BD had a good linearity from 50 to 500 microg/mL (r > 0.99). The limits of detection and quantification were 10 microg/mL and 50 microg/mL, respectively. Both the intra-day precision and inter-day precision were < 6.08%, and the accuracy was 96.98%-103.81%. The method was applied to an actual case, and the concentration of BD in the case was 242 microg/mL in human blood. This simple method is found to be useful for the routine forensic analysis of acute exposure to BD.

Determination of 33 inorganic elements in human hair by electricity plate digestion and inductively coupled plasma-mass spectrometry / 法医学杂志

OBJECTIVE@#To establish the electricity plate digestion and inductively coupled plasma-mass spectrometry (ICP-MS) method for determination of 33 inorganic elements in human hair.@*METHODS@#Lithium (6Li), Germanium (72Ge), Yttrium (89Y), Indium (115In), and Terbium (159Tb) were used as internal standards. The electric heating board digestion in a mixture of nitric acid and hydrogen peroxide was used as the pre-treatment of the hair. Thirty-three inorganic elements in human hair were analyzed by ICP-MS method.@*RESULTS@#The detection limit of ICP-MS was 0.0001 microg/g(Th)-10.9 microg/g (Ca) and the limit of quantitation was 0.0005 microg/g (Th)-25 microg/g (Ca). The recovery rate of this method was 86%-113%. The RSD for the intra-day and inter-day were less than 9.2%. The method was not statistically different from microwave digestion method.@*CONCLUSION@#This method is highly efficient and accurate. It can be used for analysis of 33 inorganic elements in human hair.

Developments in determination of elements using ICP-MS in blood and urine / 法医学杂志

Inductively coupled plasma-mass spectrometry (ICP-MS) is the most common technique for elements analysis at present. ICP-MS with high sensitivity and wide linear range can be applied to multi-elements analysis in blood and urine. This paper reviews the common means of sample pretreatment (direct dilution method and wet digestion method), the method for correction of mass spectral interference and non-interference, the main influence factors of analysis results, and provides an outlook of the application of ICP-MS in forensic toxicological analysis.