李思燕, 钟苑琴, 蔡小璇, 周常侠, 庄小舟, 马争, 叶立和, 杨佩珊, 熊劲光, 陈满连. 自动顶空-气相色谱法测定人尿中1，1，2，2-四氯乙烷[J]. 职业卫生与应急救援, 2024, 42(4): 528-532. DOI: 10.16369/j.oher.issn.1007-1326.2024.04.027
引用本文: 李思燕, 钟苑琴, 蔡小璇, 周常侠, 庄小舟, 马争, 叶立和, 杨佩珊, 熊劲光, 陈满连. 自动顶空-气相色谱法测定人尿中1，1，2，2-四氯乙烷[J]. 职业卫生与应急救援, 2024, 42(4): 528-532. DOI: 10.16369/j.oher.issn.1007-1326.2024.04.027
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LI Siyan, ZHONG Yuanqin, CAI Xiaoxuan, ZHOU Changxia, ZHUANG Xiaozhou, MA Zheng, YE Lihe, YANG Peishan, XIONG Jinguang, CHEN Manlian. Determination of 1, 1, 2, 2-tetrachloroethene in human urine by automated headspace-gas chromatography[J]. Occupational Health and Emergency Rescue, 2024, 42(4): 528-532. DOI: 10.16369/j.oher.issn.1007-1326.2024.04.027
Citation: LI Siyan, ZHONG Yuanqin, CAI Xiaoxuan, ZHOU Changxia, ZHUANG Xiaozhou, MA Zheng, YE Lihe, YANG Peishan, XIONG Jinguang, CHEN Manlian. Determination of 1, 1, 2, 2-tetrachloroethene in human urine by automated headspace-gas chromatography[J]. Occupational Health and Emergency Rescue, 2024, 42(4): 528-532. DOI: 10.16369/j.oher.issn.1007-1326.2024.04.027
shu

自动顶空-气相色谱法测定人尿中1，1，2，2-四氯乙烷

Determination of 1, 1, 2, 2-tetrachloroethene in human urine by automated headspace-gas chromatography

    摘要
  • 摘要:
    目的 建立人尿中1，1，2，2-四氯乙烷的自动顶空-气相色谱检测方法。
    方法 准确移取5.00 mL待检尿样于20 mL顶空瓶中，加入2.0 g无水亚硫酸钠后立刻密封顶空瓶盖，置于自动顶空仪中80℃加热平衡50 min。在加热条件下，同时加入无水亚硫酸钠使得尿中1，1，2，2-四氯乙烷发生完全消去反应生成三氯乙烯，顶空瓶上方三氯乙烯蒸气经DB-624毛细管色谱柱分离，火焰离子化检测器检测，以三氯乙烯的峰面积对1，1，2，2-四氯乙烷的质量浓度绘制标准曲线进行定量。
    结果 实验结果表明，尿中1，1，2，2-四氯乙烷在质量浓度为0.008 3~32.000 mg/L范围内线性关系良好，相关系数> 0.999 4，方法检出限为2.5 μg/L，定量下限为8.3 μg/L。批内相对标准偏差为4.79%~5.28%，批间相对标准偏差为4.61%~6.44%。加标回收率为87.53%~101.17%。
    结论 自动顶空-气相色谱法测定尿中1，1，2，2-四氯乙烷灵敏度高、线性关系好、干扰少、精密度好、样品前处理简单，可用于人尿中1，1，2，2-四氯乙烷质量浓度的测定。

     

    Abstract:
    Objective To establish an automated headspace-gas chromatography method for the determination of 1, 1, 2, 2-tetrachloroethene in human urine.
    Methods A urine sample of 5.00 mL was placed in a 20 mL headspace vial, and 2.0 g of anhydrous sodium sulfite was added before sealing the vial. The vial was placed in an automated headspace sampler and heated at 80 ℃ for 50.00 min to equilibrate. Under these heating conditions, 1, 1, 2, 2-tetrachloroethene in human urine was completely reacted with anhydrous sodium sulfite to form trichloroethylene. The trichloroethylene vapor above the headspace vial was separated by a DB-624 capillary column and detected with a flame ionization detector. Quantification was achieved by plotting a standard curve with the peak area of trichloroethylene and the mass concentration of 1, 1, 2, 2-tetrachloroethane.
    Results The results showed good linear ranges of 1, 1, 2, 2-tetrachloroethene in urine between 0.008 3 and 32.000 mg/L, and the correlation coefficient was higher than 0.999 4. For this method, the limit of detection was 2.5 μg/L, and the lower limit of quantification was 8.3 μg/L; the intra-batch precision was 4.79% to 5.28%, and the inter-batch precision was 4.61% to 6.44%; the average recovery rate was 87.53% to 101.17%.
    Conclusions The automated headspace gas chromatography method for determining 1, 1, 2, 2-tetrachloroethene in human urine was characterized by high sensitivity, good linearity, minimal interference, high precision, and simple sample preparation. It is suitable for measuring the concentration of 1, 1, 2, 2-tetrachloroethene in human urine.

     

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