何宗剑, 周武旺, 李燕, 肖梅, 朱杰. 控制三氯甲烷干扰后用顶空-气质联用法测定尿中三氯乙酸[J]. 职业卫生与应急救援, 2023, 41(3): 366-369. DOI: 10.16369/j.oher.issn.1007-1326.2023.03.021
引用本文: 何宗剑, 周武旺, 李燕, 肖梅, 朱杰. 控制三氯甲烷干扰后用顶空-气质联用法测定尿中三氯乙酸[J]. 职业卫生与应急救援, 2023, 41(3): 366-369. DOI: 10.16369/j.oher.issn.1007-1326.2023.03.021
HE Zongjian, ZHOU Wuwang, LI Yan, XIAO Mei, ZHU Jie. Determination of urinary trichloroacetic acid by headspace gas chromatography mass spectrometry after controlling chloroform interference[J]. Occupational Health and Emergency Rescue, 2023, 41(3): 366-369. DOI: 10.16369/j.oher.issn.1007-1326.2023.03.021
Citation: HE Zongjian, ZHOU Wuwang, LI Yan, XIAO Mei, ZHU Jie. Determination of urinary trichloroacetic acid by headspace gas chromatography mass spectrometry after controlling chloroform interference[J]. Occupational Health and Emergency Rescue, 2023, 41(3): 366-369. DOI: 10.16369/j.oher.issn.1007-1326.2023.03.021

控制三氯甲烷干扰后用顶空-气质联用法测定尿中三氯乙酸

Determination of urinary trichloroacetic acid by headspace gas chromatography mass spectrometry after controlling chloroform interference

  • 摘要:
      目的  建立能解决三氯甲烷干扰的尿中三氯乙酸顶空-气质联用测定方法。
      方法  利用三氯乙酸水浴加热脱羧后形成三氯甲烷的原理,使用顶空-气质联用法分别检测样品水浴前、水浴后的三氯甲烷峰面积,依据峰面积差值对应的浓度计算三氯乙酸浓度。
      结果  采用该方法测定尿中三氯乙酸,在0.01 ~ 50 mg/L范围内线性良好,相关系数为0.999 9,方法检出限0.2 μg/L,回收率为96.8% ~ 100.4%,相对标准偏差为1.5% ~ 2.3%。样品在室温、4 ℃和-25 ℃中可保存14 d。三氯甲烷低于10 mg/L时对测定无干扰。
      结论  该方法简便、快捷、准确,适用于职业人群和中毒患者尿中三氯乙酸的测定。

     

    Abstract:
      Objective  To establish a headspace-gas chromatography-mass spectrometry (HS-GC-MS) method for determining trichloroacetic acid (TCA) in urine that can solve the interference of chloroform.
      Methods  According to the principle that trichloroacetic acid transforms into chloroform after heating and decarboxylation in a water bath, the HS-GCMS method was used to detect the peak area of chloroform before and after the water bath of the sample, and the accurate concentration of TCA was calculated according to the difference in peak area.
      Results  The method was used to determine TCA in urine, and it showed good linearity in the range of 0.01-50 mg/L, with a correlation coefficient of 0.999 9, a detection limit of 0.2 μg/L, a recovery rate of 96.8%-100.4%, and a relative standard deviation of 1.5%-2.3%. The sample can be stored at room temperature, 4 ℃, or-25 ℃ for 14 days without degradation. When chloroform was less than 10 mg/L, there was no interference with the determination.
      Conclusions  The method is simple, fast, and accurate and is suitable for determining TCA in the urine of occupational populations and poisoned patients.

     

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