气相色谱——串联质谱联用法检测尿液中1-溴丙烷代谢物的方法研究

Study on Method for the Determination of 1-Bromopropane Metabolites in Urine by GC-MS/MS

目的建立尿液中1-溴丙烷代谢物(溴丙酮、1-溴-2-丙醇)的定性定量检测方法。方法把小白鼠经呼吸道进行1-溴丙烷染毒制做动物模型,取染毒后小白鼠尿液于顶空瓶中,用动态顶空法进行样品处理,气相色谱-串联质谱联用仪进行定性定量检测,外标定量法。结果采用动态顶空法对化合物进行浓缩、富集,DB-5MS(30 m×0.25 mm×0.25μm)型毛细管柱进行目标峰分离,EI离子源,选择离子扫描法(SIM)进行质谱检测,可对尿液中溴丙酮和1-溴-2-丙醇进行有效分离和准确定性、定量。批内重复性2.8%~4.9%,加标回收率91.8%~109.6%。染毒动物尿液中溴丙酮和1-溴-2-丙醇的检出率100%。结论动态顶空-气相色谱-串联质谱联用法可对1-溴丙烷代谢物(溴丙酮、1-溴-2-丙醇)进行准确定性、定量检测,溴丙酮和1-溴-2-丙醇可以作为1-溴丙烷暴露的生物标志物。

Objectives To develope a qualitative and quantitative method for the determination of 1-bro- mopropane metabolites （bromoacetone, 1-bromo-2-propanol） in urine. Methods The exposure of mice to 1-bro- mine propane through respiratory tract was used to set up an animal model. Urine samples collected in headspace vials were processed with dynamic headspace method, which were determined qualitatively and quantitatively by GC-MS, and quantified by external standard method. Results These chemical compounds in urine were concen- trated and enriched by dynamic headspace method, and the target peaks were separated by a DB-5MS （30 m ×0.25 mm×0.25μm） capillary column. Electron Ionization （EI） was selected as an ion source, single ion monito- ring （SIM） was used for the separation of bromoacetone and 1-bromo-2-propanol in mice urine, which were deter- mined qualitatively and quantitatively by mass spectrometric method. The reproducibilities within-run were 2. 8% - 4.9% and the recoveries were 91.8% - 109.6%. The determination rates of bromoaeetone and 1-bromo-2-pro- panol in urine collected from exposed animals were 100%. Conclusions The dynamic headspace-gas chromatog- raphy-tandem mass spectrometry could be used to qualitatively, quantitatively and accurately determine the level of 1-bromopropane metabolite （bromoacetone, 1-bromo-2-propanol） in urine. Bromoacetone and 1-bromo-2-propanol could be used as biomarkers for 1-hromopropane exposure.