1. Determination of arsenic species compound in blood by high performance liquid chromatographyatomic fluorescence spectrometry
Lezhou ZHOU ; Lu YANG ; Sheng FU
Chinese Journal of Industrial Hygiene and Occupational Diseases 2019;37(12):928-931
Objective:
To establish a method for determination of arsenic species in blood with high performance liquid chromatography-atomic fluorescence spectrometry (HPLC-AFS) .
Methods:
The effect of mobile phase about chromatography separation and sample pretreatment conditions and atomic fluorescence spectrometry detection parameters has been optimized to reliably measure the following four kinds of species arsenic compound including arsenic[As (III) ]、dimethylarsinic acid (DMA) 、monomethylarsonic acid (MMA) and arsenate[As (V) ] in acute intoxication human blood. The method of technical standard about within-run, between-run and recoveries of standard were optimized.
Results:
The method showed As (III) linear relationship was 2.63-100.00 μg/L, The detection limit was 2.63 μg/L. The relative coefficient (
2.Determination of trace gallium by graphite furnace atomic absorption spectrometry in urine
Lezhou ZHOU ; Sheng FU ; Shouquan GAO ; Guowen HE
Chinese Journal of Industrial Hygiene and Occupational Diseases 2016;34(6):465-467
Objective To establish a method for determination trace gallium in urine by graphite furnace atomic absorption spectrometry (GFAAS).Methods The ammonium dihydrogen phosphate was matrix modifier.The temperature effect about pyrolysis (Tpyr) and atomization temperature were optimized for determination of trace gallium.The method of technical standard about within-run,between-run and recoveries of standard were optimized.Results The method showed a linear relationship within the range of 0.20~80.00 μg/L(r=0.998).The within-run and between-run relative standard deviations (RSD) of repetitive measurement at 5.0,10.0,20.0 μg/L concentration levels were 2.1%~5.5% and 2.3%~3.0%.The detection limit was 0.06 μg/L.The recoveries of gallium were 98.2%~101.1%.Conclusion This method is simple,low detection limit,accurate,reliable and reproducible.It has been applied for determination of trace gallium in urine samples those who need occupation health examination or poisoning diagnosis.
3.Determination of trace bismuth by atomic fluorescence spectrometry in blood
Lezhou ZHOU ; Sheng FU ; Shouquan GAO ; Guowen HE
Chinese Journal of Industrial Hygiene and Occupational Diseases 2016;34(12):939-941
Objective To establish a method for determination trace bismuth in blood by atomic fluorescence spectrometry (AFS).Methods 4.0 ml nitric acid and 1.0 ml perchloric acid was added into 1.0 ml blood sample then through automation graphite digestion instrument digested,after that 1.0 ml thiocarbamidevitamin (10%) was injected,8% HC1 constant volume to 10.0 ml,the bismuth was detected by atomic fluorescence spectrometry with 5.0 ml digestive sample.Results The method showed a linear relationship within the range of 0.4-50.0 μg/L (r=0.999 7).The within-run and between-run relative standard deviations (RSD) of repetitive measurement at 10.0,20.0,40.0 μg/L concentration levels were 2.2%-4.9% and 3.0%-4.0%.The detection limit was 0.032 μg/L.The recoveries of bismuth were 93.0%-103.9%.Conclusion This method is low detection limit,good accurate and high sensitivity.It has been applied for determination of trace bismuth in blood samples those who need occupation health examination or poisoning diagnosis.
4.Determination of trace gallium by graphite furnace atomic absorption spectrometry in urine
Lezhou ZHOU ; Sheng FU ; Shouquan GAO ; Guowen HE
Chinese Journal of Industrial Hygiene and Occupational Diseases 2016;34(6):465-467
Objective To establish a method for determination trace gallium in urine by graphite furnace atomic absorption spectrometry (GFAAS).Methods The ammonium dihydrogen phosphate was matrix modifier.The temperature effect about pyrolysis (Tpyr) and atomization temperature were optimized for determination of trace gallium.The method of technical standard about within-run,between-run and recoveries of standard were optimized.Results The method showed a linear relationship within the range of 0.20~80.00 μg/L(r=0.998).The within-run and between-run relative standard deviations (RSD) of repetitive measurement at 5.0,10.0,20.0 μg/L concentration levels were 2.1%~5.5% and 2.3%~3.0%.The detection limit was 0.06 μg/L.The recoveries of gallium were 98.2%~101.1%.Conclusion This method is simple,low detection limit,accurate,reliable and reproducible.It has been applied for determination of trace gallium in urine samples those who need occupation health examination or poisoning diagnosis.
5.Determination of trace bismuth by atomic fluorescence spectrometry in blood
Lezhou ZHOU ; Sheng FU ; Shouquan GAO ; Guowen HE
Chinese Journal of Industrial Hygiene and Occupational Diseases 2016;34(12):939-941
Objective To establish a method for determination trace bismuth in blood by atomic fluorescence spectrometry (AFS).Methods 4.0 ml nitric acid and 1.0 ml perchloric acid was added into 1.0 ml blood sample then through automation graphite digestion instrument digested,after that 1.0 ml thiocarbamidevitamin (10%) was injected,8% HC1 constant volume to 10.0 ml,the bismuth was detected by atomic fluorescence spectrometry with 5.0 ml digestive sample.Results The method showed a linear relationship within the range of 0.4-50.0 μg/L (r=0.999 7).The within-run and between-run relative standard deviations (RSD) of repetitive measurement at 10.0,20.0,40.0 μg/L concentration levels were 2.2%-4.9% and 3.0%-4.0%.The detection limit was 0.032 μg/L.The recoveries of bismuth were 93.0%-103.9%.Conclusion This method is low detection limit,good accurate and high sensitivity.It has been applied for determination of trace bismuth in blood samples those who need occupation health examination or poisoning diagnosis.
6. Determining 6 arsenic species in human urine by high performance liquid chromatography-atomic fluorescence spectrometry
Lezhou ZHOU ; Lu YANG ; Sheng FU
China Occupational Medicine 2020;47(02):204-208
OBJECTIVE: To establish a methodology using high performance liquid chromatography-atomic fluorescence spectrometry(HPLC-AFS) for the determination of 6 arsenic species including arsenite, dimethyl arsenic acid, monomethyl arsenic acid, dimethyl arsenic acid, monomethyl arsenic acid and arsenite in human urine. METHODS: The PRP-X100 anion exchange chromatographic column was used with 4.0 mmol/L ammonium carbonate, ammonium sulfate and ammonium phosphate mixed solution with pH 8.9 as mobile phase. The carrier current was hydrochloric acid with volume fraction of 10.0% and reducing agent was potassium borohydride with mass fraction of 3.5%. After centrifugal separation of urine sample, 6 forms of arsenics were detected by HPLC-AFS. RESULTS: The linear range of 6 forms of arsenics in urine was 3.90-100.00 μg/L. The correlation coefficient was 0.999 1-0.999 9, and the detection limit was 1.31-3.90 μg/L. The recovery rate was 91.2%-103.5%. The within-run and between-run relative standard deviations were 0.5%-4.9% and 1.8%-5.0%, respectively. The samples could be stored for at least 7 days under the temperature of-80 ℃. CONCLUSION: The method has low detection limit, good precision and high sensitivity, which is suitable for the determination of arsenics in human urine.