Detecting human urinary thiocyanate by gas chromatography with pre-column derivatization / 中国职业医学

ABSTRACT

OBJECTIVE: To establish a method for detecting human urinary thiocyanate by gas chromatographic and pre-column derivatization with 2,3,4,5,6-pentafluorobenzyl bromide( PFB-Br). METHODS: A total of 20. 0 μL of urine was taken and 1. 0 m L of acetonitrile and 100. 0 μL of PFB-Br were added for derivative reaction. The gas chromatography was directly used for measurement. RESULTS: The urinary thiocyanate concentration showed a good linear range of 1. 000-10. 000 mg/L. The linear correlation coefficient was 0. 999 6. The minimum detection concentration was 0. 112 mg/L,and the minimum quantitative concentration was 0. 411 mg/L( 20. 0 μL urine sample). The standard recovery rate was 97. 22%-102. 04%.The within-run relative standard deviation( RSD) of this method was 1. 56%-5. 35%. The between-run RSD was 1. 46%-5. 10%. Hydrocyanic acid ions interfered with the measurement. Other common inorganic ions such as chloride,sulfate,and nitrate ions did not interfere with the measurement results. The samples can be stored at 4 ℃ for at least 15 days. CONCLUSION: This method is suitable for detecting human urinary thiocyanate.