顶空气相色谱法检测尿二氯乙酸和三氯乙酸  

Determination of dichloroacetic acid and trichloroacetic acid in urine using headspace gas chromatography

作　　者：杨清华[1] 施逸岚[1] 顾俊[1] 陈峰[1] 韦加梅 YANG Qinghua;SHI Yilan;GU Jun;CHEN Feng;WEI Jiamei(Department of Physics and Chemistry,Nantong Center for Disease Prevention and Control,Nantong,Jiangsu 226002,China;Pukou Center for Disease Prevention and Control,Nanjing,Jiangsu 210000,China)

机构地区：[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

出　　处：《预防医学》2022年第2期213-216,共4页CHINA PREVENTIVE MEDICINE JOURNAL

基　　金：南通市科技局项目(JC2020111)。

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10~500μg/L范围内的相关系数均大于0.9990,最低检出限分别为2.0μg/L和3.5μg/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。Objective To develop a headspace gas chromatography(HS-GC)assay for simultaneous determination of di⁃chloroacetic 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>0.9990 within the range of 10-500.0μg/L,and the lowest detection limits of DCA and TAC were 2.0 and 3.5μg/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 estab⁃lishment 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.

关 键 词：二氯乙酸 三氯乙酸 顶空气相色谱法 

分 类 号：R155.5[医药卫生—营养与食品卫生学]