ABSTRACT
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.
ABSTRACT
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.
ABSTRACT
OBJECTIVE: To establish a method for detecting tin in human blood by microwave digestion-atomic fluorescence spectrometry. METHODS: The microwave digestion instrument was used to digest 1. 00 mL blood sample with 4. 00 mL concentrated nitric acid( mass fraction 65. 00%) and 1. 00 mL perchloric acid( mass fraction 68. 00%). After 1. 00 mL of thiocarbamide-ascorbic acid( mass fraction 10. 00%) was added,hydrochloric acid( concentration 1. 5 mol / L) was added to a total constant volume of 10. 00 mL. Then 5. 00 mL of the sample was collected and detected by atomic fluorescence spectrophotometry. RESULTS: The good linear relationship was shown in the range of 0. 00-60. 00 μg / L,and the correlation coefficient was 0. 999 5. The limit of detection was 0. 01 μg / L. The average recovery rate was 98. 80%-103. 30%. The relative standard deviation( RSD) of within-run precision was 3. 74%-5. 26%,and the RSD of betweenrun precision was 1. 23%-4. 45%. The samples can be stored for at least 7 days under the temperature of 4 ℃.CONCLUSION: This method has the advantages of low detection limit,good precision and high sensitivity,which is suitable for the determination of tin in human blood.