顶空-气相色谱-质谱法测定人尿中1-溴丙烷

Determination of 1-bromopropane in human urine by headspace gas chromatography-mass spectrometry

目的建立人尿中1-溴丙烷的顶空-气相色谱-质谱检测方法。方法准确移取4.00 m L待检尿样于15.00 m L顶空瓶中,加入质量浓度为204.200 mg/L的1-溴丁烷内标溶液20.00μL后立刻密封顶空瓶盖,于顶空装置中80℃加热平衡20.00 min,顶空瓶上方蒸气经GSBP-FFAP毛细管色谱柱（30.00 m×0.25 mm×0.25μm）分离,选择离子定量测定尿中1-溴丙烷。结果尿中1-溴丙烷在质量浓度为0.025～1.012 mg/L范围内线性关系良好,相关系数为0.999 8,方法检出限为7.5μg/L（以4.00 m L尿样计算）,定量限为25.0μg/L（以4.00 m L尿样计算）。批内相对标准偏差（RSD）为2.61%～4.08%,批间RSD为2.79%～6.25%。加标回收率为99.34%～105.94%。结论本方法测定尿中1-溴丙烷灵敏度高、线性关系好、干扰少、精密度好、操作简单,适用于人尿中1-溴丙烷质量浓度的检测。

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.