Objective: To establish a method for determination of acetone in urine by headspace gas chromatography-mass spectrometry. Methods: From March to June 2021, the 3.0 ml urine sample was placed in a headspace bottle with 4.0 g of anhydrous sodium sulfate and sealed. Equilibration time was 30 min at 85 ℃. The separation was carried out on a DB-5MS column. The urine sample was detected by mass spectrometry and quantified by external standard method. Results: The method for the determination of acetone in urine by headspace gas chromatography-mass spectrometry had good linearity in the range of 51.2-1024.0 μg/L, and the correlation coefficient was 0.9995. The detection limit and the lower limit of quantification of acetone were 16.4 μg/L and 54.6 μg/L. The average recoveries of samples ranged from 94.9% to 96.8%. The intra-assay precision and inter-assay precision were both less than 10%. Samples can be stored at least 7 d at 4 ℃ or -20 ℃. Conclusion: This method has simple sample preparation and high sensitivity. It can be used for monitoring and evaluation of urinary acetone in the general population and occupationally exposed populations.
目的： 建立尿中丙酮的顶空气相色谱-质谱检测方法。 方法： 于2021年3至6月，取3.0 ml尿样于顶空瓶，加4.0 g无水硫酸钠，密封。85 ℃下平衡30 min，DB-5MS色谱柱分离，质谱检测，外标法定量。 结果： 尿中丙酮测定的顶空气相色谱-质谱方法在51.2~1 024.0 μg/L范围内线性良好，r=0.999 5；方法检出限和定量限分别为16.4、54.6 μg/L；样品加标回收率94.9%~96.8%；批内和批间精密度均<10%。样品在4 ℃或-20 ℃下至少保存7 d。 结论： 顶空气相色谱-质谱法测定尿中丙酮含量的样品前处理简单、灵敏度高，可准确测定正常人群和丙酮职业暴露人群尿中丙酮含量。.
Keywords: Acetone; Gas chromatography-mass spectrometry; Headspace; Urine.