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.

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 (r) was 0.9999; DMA linear relationship was 3.21-100.00 μg/L, The detection limit was 3.21 μg/L. The r was 0.9992; MMA linear relationship was 3.41-100.00 μg/L, The detection limit was 3.41 μg/L. The r was 0.9998; As (V) linear relationship was 3.90-100.00 μg/L, The detection limit was 3.90 μg/L. The r was 0.9996. The average recovery of four species arsenic in tested samples ranged from 91.3%-99.8% with the relative standard deviation (RSD) from 2.39% to 4.05%. The within-run and between-run relative standard deviations (RSD) of repetitive measurement at 10.00, 40.00, 80.00 μg/L concentration levels were 1.99%-4.59% and 2.72%-4.53%. Conclusion This method is low detection limit, good accurate and high sensitivity, proposed method had been applied to the analysis of arsenic species in blood samples those who acute intoxication or poisoning diagnosis.

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.

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.

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.

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.