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预防医学  2022, Vol. 34 Issue (2): 213-216    DOI: 10.19485/j.cnki.issn2096-5087.2022.02.022
  实验技术 本期目录 | 过刊浏览 | 高级检索 |
顶空气相色谱法检测尿二氯乙酸和三氯乙酸
杨清华1, 施逸岚1, 顾俊1, 陈峰1, 韦加梅2
1.南通市疾病预防控制中心理化科,江苏 南通 226002;
2.南京市浦口区疾病预防控制中心,江苏 南京 210000
Determination of dichloroacetic acid and trichloroacetic acid in urine using headspace gas chromatography
YANG Qinghua1, SHI Yilan1, GU Jun1, CHEN Feng1, WEI Jiamei2
1. Department of Physics and Chemistry, Nantong Center for Disease Prevention and Control, Nantong, Jiangsu 226002, China;
2. Pukou Center for Disease Prevention and Control, Nanjing, Jiangsu 210000, China
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摘要 目的 建立同时检测尿二氯乙酸(DCA)和三氯乙酸(TCA)的顶空气相色谱法。方法 吸取5 mL尿样于22 mL顶空瓶中,加入0.5 mL 10%乙酸钠溶液后立即加盖密封,摇匀,置于顶空-气相色谱仪中,90 ℃平衡60 min后进样,经HP-INNOWAX气相色谱柱分离,氢火焰检测器检测DCA和TCA含量。结果 在最佳实验条件下,DCA和TCA在10~500 μg/L范围内的相关系数均大于0.999 0,最低检出限分别为2.0 μg/L和3.5 μg/L,加标回收率为87.40%~101.44%,相对标准偏差(RSD)为1.89%~3.25%。抽检35份职业人群尿样,DCA和TCA均未检出。结论 通过加入乙酸钠、优化顶空条件建立的顶空气相色谱法回收率和精密度等指标良好,能满足尿二氯乙酸和三氯乙酸的日常检测需求。
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杨清华
施逸岚
顾俊
陈峰
韦加梅
关键词 二氯乙酸三氯乙酸顶空气相色谱法    
AbstractObjective To develop a headspace gas chromatography ( HS-GC ) assay for simultaneous determination of dichloroacetic acid ( DCA ) and trichloroacetic acid ( TCA ) in urine. Methods Urine samples (5 mL) were transferred to a 22 mL headspace bottle, added with 0.5 mL 10% sodium acetate solution , immediately sealed, and shaken evenly. The bottle was placed in the HS-GC system, and equilibrated at 90 ℃ for 60 minutes. The mixture was separated with the HP-INNOWAX chromatographic column, and the DCA and TCA concentrations were detected with the hydrogen flame detector. Results Under the optimal experimental conditions, the correlation coefficient of DCA and TAC was both > 0.999 0 within the range of 10-500.0 μg/L, and the lowest detection limits of DCA and TAC were 2.0 and 3.5 μg/L, with the spike recovery rate of 87.40% to 101.44%, and relative standard deviations of 1.89% to 3.25%. Of the 35 urine samples sampled from occupational populations, DCA and TCA were not detected. Conclusions The establishment of the HS-GAS assay through addition of sodium acetate and optimization of the headspace conditions, has high recovery and precision, which is effective to meet the requirements for daily determination of DCA and TCA in urine samples.
Key wordsdichloroacetic acid    trichloroacetic acid    headspace gas chromatography
收稿日期: 2021-08-09      修回日期: 2021-10-28      出版日期: 2022-02-10
中图分类号:  R155.5  
基金资助:南通市科技局项目(JC2020111)
通信作者: 韦加梅,E-mail: qhyang0822@163.com   
作者简介: 杨清华,硕士,高级工程师,主要从事理化检验工作
引用本文:   
杨清华, 施逸岚, 顾俊, 陈峰, 韦加梅. 顶空气相色谱法检测尿二氯乙酸和三氯乙酸[J]. 预防医学, 2022, 34(2): 213-216.
YANG Qinghua, SHI Yilan, GU Jun, CHEN Feng, WEI Jiamei. Determination of dichloroacetic acid and trichloroacetic acid in urine using headspace gas chromatography. Preventive Medicine, 2022, 34(2): 213-216.
链接本文:  
http://www.zjyfyxzz.com/CN/10.19485/j.cnki.issn2096-5087.2022.02.022      或      http://www.zjyfyxzz.com/CN/Y2022/V34/I2/213
[1] 刘德坚,马忠元.职业接触三氯乙烯引起皮肤和肝脏损害的调查[J].职业与健康,2007,23(23):2143-2144.
LIU D J,MA Z Y.Investigation of dermal and liver impairment induced by occupational exposure to trichloroethylene[J].Occup Health,2007,23(23):2143-2144.
[2] 陈华宜,吴惠刚,廖国荣.气相色谱/质谱联用法鉴定一起职业中毒事件中车间空气的毒物[J].中国职业医学,2002,29(5):46.
CHEN H Y,WU H G,LIAO G R.Identification of toxicants in the air of workplace in an occupational poisoning accident by gas chromatography/mass spectrometry[J].Chin Occup Med,2002,29(5):46.
[3] 钟逸菲,马立明,熊俊,等.东莞市2003—2013年职业中毒发病情况分析[J].中华劳动卫生职业病杂志,2014,32(8):600-601.
ZHONG Y F,MA L M,XIONG J,et al.Analysis on the incidence of occupational poisoning in Dongguan from 2003 to 2013[J].Chin J Ind Hyg Occup Dis,2014,32(8):600-601.
[4] 阮小林,黄汉林,越飞,等.衍生化气相色谱法同时测定尿中三氯乙烯的3种氯代乙酸代谢产物[J].分析测试学报,2013,23(3):377-380.
RUAN X L,HUANG H L,YUE F,et al.Simultaneous determination of three halogenated acetic acids in urine by derivatization gas chromatography[J].J Instr Anal,2013,23(3):377-380.
[5] 李添娣,易娟,张文,等.顶空气相色谱-质谱联用法测定尿中三氯乙酸[J].中国职业医学,2013,40(1):68-70.
LI T D,YI J,ZHANG W,et al.Determination of trichloroacetic acid in urine by head-space-gas chromatography-mass spectrometry[J].Chin Occup Med,2013,40(1):68-70.
[6] 赵小彤,杨海明,鞠茂伟.分光光度法测定水样中三氯乙酸的影响因素[J].辽宁科技大学学报,2015,38(5):351-353.
ZHAO X T,YANG H M,JU M W.Influence factors of determination trichloroacetic acid in water by spectrophotometry[J].J Liaoning Univ Sci Technol,2015,38(5):351-353.
[7] 陈际,周永芳,杜双双,等.超高效液相色谱-串联质谱法检测饮用水中二氯乙酸和三氯乙酸[J].净水技术,2018,37(4):66-70.
CHEN J,ZHOU Y F,DU S S,et al.Determination of dichloroacetic acid and trichloroacetic acid in drinking water by ultra performance liquid chromatography-tandem mass spectrometry[J].Water Purif Technol,2018,37(4):66-70.
[8] 曾钰,陈军,王海瑞,等.高效液相色谱法测定饮用水中的一氯乙酸和二氯乙酸[J].理化检验-化学分册,2014,50(9):1173-1174.
ZENG Y,CHEN J,WANG H R,et al.Determination of monochloroacetic acid and dichloroacetic acid in drinking water by high-performance liquid chromatography[J].Phys Test Chem Anal(Part B:Chem Anal),2014,50(9):1173-1174.
[9] 中华人民共和国卫生部.尿中三氯乙酸顶空气相色谱测定方法:WS/T 96—1996[S].北京:中国标准出版社,1997.
Ministry of Health of the People's Republic of China.Urine-determination of trichloroacetic acid-headspace gas chromatographic method:WS/T 96-1996[S].Beijing:Standards Press of China,1997.
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