顶空气相色谱-质谱联用法同时测定尿中14种氯代烃  

Simultaneous determination of 14 chlorinated hydrocarbons in urine by headspace gas chromatography-mass spectrometry

作　　者：蔡小璇[1] 唐斯[1] 彭建梅 庄小舟[1] 叶立和 李思燕 钟苑琴[1] 马争[1] 陈惠鹏[1] 张凤华[1] CAI Xiaoxuan;TANG Si;PENG Jianmei;ZHUANG Xiaozhou;YE Lihe;LI Siyan;ZHONG Yuanqin;MA Zheng;CHEN Huipeng;ZHANG Fenghua(Dongguan Prevention and Treatment Center for Occupational Disease,Dongguan City Key Laboratory of Occupational Health Dectection,Dongguan,Guangdong 523008,China)

机构地区：[1]东莞市职业病防治中心,东莞市职业卫生检测重点实验室,广东东莞523008

出　　处：《中国职业医学》2020年第4期470-474,共5页China Occupational Medicine

基　　金：广东省医学科学技术研究基金(A2020316)。

摘　　要：目的建立尿中14种氯代烃的顶空气相色谱-质谱联用测定方法。方法于10.00 mL顶空瓶中加入3.00 g无水硫酸钠,加入4.00 mL尿样,于70℃下控温40.0 min。顶空前处理后,顶空气中的14种氯代烃经气相色谱仪DB-5MS毛细管色谱柱分离,质谱检测器检测。结果尿中14种氯代烃在0.62~1630.00μg/L内线性关系良好,相关系数均大于0.9990,最低检出浓度为0.19~0.43μg/L,最低定量浓度为0.62~1.44μg/L,平均加标回收率为89.8%~107.1%,批内相对标准偏差(RSD)为4.0%~8.5%,批间RSD为6.3%~9.1%。尿样于4℃或-8℃下可保存3 d,-20℃以下可保存7 d。结论本方法快速、简便、灵敏、准确、干扰少,可作为职业中毒患者尿样中14种氯代烃的检测方法。Objective To establish a headspace gas chromatography-mass spectrometry method for the determination of 14 chlorinated hydrocarbons in urine.Methods The urine sample 4.00 mL and anhydrous sodium sulfate 3.00 g were added into a 10.00 mL headspace bottle,then the headspace bottle was maintained at 70℃for 40.0 min.After headspace pretreatment,14 chlorinated hydrocarbons in headspace air were separated in the DB-5 MS capillary column of the gas chromatography and detected by mass spectrometer.Results There was a good linear relationship of 14 chlorinated hydrocarbons in urine in the range of 0.62-1630.00μg/L.The linear correlation coefficient was greater than 0.9990.The minimum detectable concentration was 0.19-0.43μg/L and the minimum quantitative concentration was 0.62-1.44μg/L.The average recovery rate was 89.8%-107.1%.The within-run relative standard deviation(RSD)was 4.0%-8.5%and the between-run RSD was 6.3%-9.1%.Urine samples can be stored at 4℃or-8℃for 3 days and below-20℃for 7 days.Conclusion This method is rapid,simple,sensitive,accurate and has little interference,which can be used as a method for detecting 14 kinds of chlorinated hydrocarbons in urine samples of patients with occupational poisoning.

关 键 词：尿样 氯代烃 气相色谱-质谱联用法 顶空分析法 

分 类 号：R135.1[医药卫生—劳动卫生]