顶空-气相色谱/质谱法测定尿中丁酮

Determination of butanone in urine by headspace-gas chromatography/mass spectrometry

目的建立顶空-气相色谱/质谱法测定尿中丁酮的方法。方法尿样加入3.0 g氯化钠,经顶空处理后,用HP-5MSUI毛细管色谱柱(30 m×0.32 mm×0.15μm)分离,以氢火焰离子化检测器(FID)和质谱检测器(MSD)检测,以保留时间结合质谱定性,FID峰面积定量。结果采用本法,丁酮在0.5 mg/L~10.0 mg/L浓度内呈线性,回归方程为y=13.89x+2.27,相关系数为0.9993,以3倍噪音值估算方法检出限为0.013 mg/L。在0.5 mg/L~10.0 mg/L内添加低、中、高3个浓度水平,丁酮的加标回收率为90.0%~93.8%;批内精密度为2.6%~6.9%(n=6),批间精密度为5.7%~8.1%(n=6);尿样在4℃冷藏条件下,至少可保存7 d。结论本法操作简单,灵敏度高,方法学指标符合《职业卫生标准制定指南-第5部分:生物材料中化学物质测定方法》(GBZ/T 210.5—2008)的要求,可以应用于职业人群尿样中丁酮的测定。

Objective To establish a method for the determination of butanone in urine byheadspace-gas chromatography/mass spectrometry.Methods A total of 3.0 g sodium chloride was added to the samples.Then the samples were processed through the headspace sampling process,and separated by HP-5MSUI capillary chromatographic column(30 m×0.32 mm×0.15μm).Butanone was detected by flame ionization detector(FID)and mass detector(MSD),and then qualified by the retention time plus mass spectrum,quantified by the peak area.Results By the proposed method,the concentration of butanone was linear in 0.5 mg/L-10.0 mg/L.The regression equation was y=13.89x+2.27,with the correlation coefficient(r)of 0.9993.The detection limit was 0.013 mg/L using the three-fold noise estimation method.The recoveries of butanone ranged from 90.0%to 93.8%when low,medium and high concentrations were added in the range of 0.5 mg/L to 10.0 mg/L.The intra-batch precision was 2.6%-6.9%(n=6),and the inter-batch precision was 5.7%-8.1%(n=6).Urine samples can be stored at 4℃for at least 7 days.Conclusion The new developed method was proved to be simple,practical,and highly sensitive.Moreover,it can meet the requirements of GBZ/T 210.5-2008 Guide for Establishing Occupational Health Standards:Part 5 Determination Methods of Chemicals in Biological Materials.Thus,it can be utilized for butanone detection in occupational population.