吹扫捕集—气相色谱/质谱同位素内标法测定尿中挥发性有机物

林强; 周志荣; 胡小键; 林少彬

doi:10.13421/j.cnki.hjwsxzz.2017.03.013

吹扫捕集—气相色谱/质谱同位素内标法测定尿中挥发性有机物

Determination of Volatile Organic Compounds in Urine by Purge and Trap-Gas Chromatography -Mass Spectrometry with Isotope Internal Standard

摘要

摘要:
目的建立测定尿中12种挥发性有机物（VOCs）的分析方法。
方法样品冷却至室温后，在氮气环境下，利用排液装置，使样品体积为30 mL，依次加入消泡剂和同位素内标，震荡摇匀后，在进样瓶中加满纯水，采用选择离子扫描模式检测12种挥发性有机物的含量。
结果加标浓度为0.184 ng/mL、0.553 ng/mL时，回收率76.6%~104.8%，RSD为1.7%~11.2%。该方法在（0.045~5.76）ng/mL的浓度线性良好，线性系数均大于0.995。待测尿液体积为30.00 mL时，方法检出限为（0.006~0.15）ng/mL，检测限为（0.010~0.27）ng/mL。
结论本方法检出限低，适用于非暴露人群中VOCs内暴露测定。

Abstract:
Objective To develop an analytical method for the determination of 12 volatile organic compounds (VOCs) in urine.
Methods After the urine sample being cooled to room temperature, the volume of urine in the introduction bottle was adjusted to 30 mL under nitrogen atmosphere, a defoamer and an isotope internal standard was added successively. After shaking, the bottle was filled with pure water. The content of 12 kinds of volatile organic compounds was determined by gas chromatography-mass spectrometry in an ion scanning mode.
Results The recoveries of standard addition at the concentration of 0.184 ng/mL and 0.553 ng/mL were in the range of 76.6%~104.8%, and the RSD degrees of precision were in the range of 1.7%~11.2%. The linearity of the standard curve was good over the range of 0.045 ng/mL to 5.76 ng/mL, and the linear correlation coefficient was greater than 0.995. When the volume of urine sample was 30.00 mL, the detection limit was (0.006~0.15) ng/mL, and the range of determination were (0.010~0.27) ng/mL.
Conclusion The detection limit of this method was low and the method was suitable for the determination of internal VOCs exposure in non-exposed population.

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