Determination of 1-bromopropane in human urine by headspace gas chromatography-mass spectrometry / 中国职业医学

ABSTRACT

OBJECTIVE: To establish a detection method for 1-bromopropane in human urine by headspace gas chromatography-mass spectrometry( GC-MS). METHODS: A 4. 00 m L portion of the urine sample was placed in a 15. 00 m L headspace vial and 20. 00 μL of 1-bromobutane internal standard solution( 204. 200 mg / L mass concentration) was added.The bottle cap was immediately sealed. The sample was heated to 80 ℃ with an equilibrium time of 20 minutes in the headspace device. The vapor in the headspace vial was separated by GSBP-FFAP( 30. 00 m × 0. 25 mm × 0. 25 μm)capillary chromatography column and the ion was used to carry out quantitative determination of 1-bromopropane in human urine. RESULTS: The good linearity range of 1-bromopropan mass concentration was 0. 025-1. 012 mg / L, and the correlation coefficient was 0. 999 8. The detection limit was 7. 5 μg / L( urine sample volume,4. 00 m L) and the limit of quantitation was 25. 0 μg / L( urine sample volume,4. 00 m L). The relative standard deviation( RSD) of within-run precision was 2. 61%-4. 08%,and the RSD of between-run precision was 2. 79%-6. 25%. The average recovery rate was99. 34%-105. 94%. CONCLUSION: The method of determining 1-bromopropane in human urine by headspace GC-MS has the features of high sensitivity,good linear relationship,low interference,good precision and easy operation,which is suitable for detecting 1-bromopropane mass concentration in human urine.