顶空固相微萃取/气相色谱-质谱联用测定尿液中8种苯系物和17种挥发性卤代烃

展学旺 李彭辉 徐琳

引用本文: 展学旺, 李彭辉, 徐琳. 顶空固相微萃取/气相色谱-质谱联用测定尿液中8种苯系物和17种挥发性卤代烃[J]. 分析化学, 2023, 51(6): 1033-1041. doi: 10.19756/j.issn.0253-3820.221372 shu
Citation:  ZHAN Xue-Wang,  LI Peng-Hui,  XU Lin. Determination of 8 Kinds of Benzenes and 17 Kinds of Volatile Halogenated Hydrocarbons in Urine by Headspace-Solid Phase Microextraction/Gas Chromatography-Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2023, 51(6): 1033-1041. doi: 10.19756/j.issn.0253-3820.221372 shu

顶空固相微萃取/气相色谱-质谱联用测定尿液中8种苯系物和17种挥发性卤代烃

    通讯作者: 李彭辉,E-mail:lipenghui406@163.com; 徐琳,E-mail:linxu@rcees.ac.cn
  • 基金项目:

    国家自然科学基金项目(Nos.22036007,21876189)和中国科学院青年创新促进会项目(No.2018059)资助。

摘要: 建立了尿液样品中8种苯系物(BTEX)和17种挥发性卤代烃(VHC)的顶空固相微萃取/气相色谱-质谱分析方法(GC-MS)。通过单因素实验考察了萃取纤维、萃取温度、萃取时间、尿液pH值、搅拌速度和盐效应等因素对实验结果的影响,然后根据Box-Behnken试验设计原理,以25种目标化合物色谱图总峰面积为响应值进行因素之间交互作用的分析。优化后的条件为:将2 mL调至pH=4的尿样、40 μL内标(氟苯和氯苯-d5,500 μg/L)和0.55 g NaCl加入40 mL顶空瓶中,选用75 μm羧基/聚二甲基硅氧烷(Carboxen/PDMS)纤维于51℃、搅拌速度为400 r/min条件下顶空萃取35 min。25种目标物在0.05~50 μg/L范围内具有良好的线性关系(R2 > 0.990),方法检出限为0.008~5.780 ng/L,定量限为0.027~19.268 ng/L; 25种目标物的回收率为78.9%~115.2%,相对标准偏差为0.7%~16.2%。将本方法应用于山东省莱阳地区健康人群尿液的测定,结果表明,在15个人体尿液样本中共检出20种目标化合物,总浓度范围为3.13~43.17 μg/L,中位浓度为5.78 μg/L。1,2,4三甲基苯(1,2,4-TMB)是BTEX中位数含量最高的化合物,1,3二氯苯(1,3-DCB)是VHC中位数含量最高的化合物。本方法灵敏度高、重现性好,适用于尿液样品中BTEX和VHC的同时检测,可为这两类化合物的人体暴露研究提供重要的方法学基础。

English


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  • 收稿日期:  2022-07-24
  • 修回日期:  2023-02-07
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