尿中1-甲氧基-2-丙醇测定的顶空固相微萃取-气相色谱法  

Determination of 1-methoxy-2-propanol in urine by headspace solid-phase microextraction coupled with gas chromatography

作　　者：高宏民 宋世震 梅勇 聂梦涵 方若丹 苏婉婷 Gao Hongmin;Song Shizhen;Mei Yong;Nie Menghan;Fang Ruodan;Su Wanting(School of Public Health,Wuhan University of Science and Technology,Hubei Province Key Laboratory of Occupational Hazard Identification and Control,Wuhan 430065,China)

机构地区：[1]武汉科技大学医学院公共卫生学院,"职业危害识别与控制"湖北省重点实验室,430065

出　　处：《中华劳动卫生职业病杂志》2020年第1期52-55,共4页Chinese Journal of Industrial Hygiene and Occupational Diseases

摘　　要：目的建立尿中1-甲氧基-2-丙醇(1-methoxy-2-propanol,1M2P)的顶空固相微萃取-气相色谱测定方法。方法采用碳分子筛/聚二甲基硅氧烷(CAR/PDMS)涂层固相微萃取头对尿样进行顶空萃取;单因素轮换法对萃取温度、盐析量、萃取时间进行优化;以DB-5(30 m×0.32 mm×0.25μm)毛细管柱为分离柱,氢火焰离子化检测器(FID)检测,外标法定量。结果尿中1M2P浓度在0.50~10.0 mg/L线性关系良好,相关系数为0.9993,方法检出限为0.14 mg/L,定量下限为0.45 mg/L,回收率为85.8%~104.7%,日内精密度为3.25%~6.65%,日间精密度为0.81%~3.96%。结论该方法灵敏度高,操作简便,适用于职业暴露1M2P人群尿中1M2P的测定。Objective To establish a method for the determination of 1-methoxy-2-propanol in urine using headspace solid phase micro-extraction coupled with gas chromatography.Methods The 1-methoxy-2-propanol was enriched by headspace solid phase micro-extraction fiber coated with carbene/polydimethylsiloxane(CAR/PDMS).Single factor rotation method was used to optimize the conditions of extraction temperature,salt amount,and extraction time.The separation was performed on DB-5(30 m×0.32 mm×0.25μm)capillary column and detected with flame ionization detector.The quantification was based on the standard curve.Results The concentration of 1-methoxy-2-propanol in urine was linear in the range of 0.50-10.0 mg/L,and the linear correlation coefficient was 0.9993.The detection limit of the method was 0.14 mg/L,and the limit of quantification was 0.45 mg/L.The recovery was 85.8%to 104.7%,and the RSD of intra-and inter-batch precision were 3.25%-6.65%and 0.81%-3.96%,respectively.Conclusion The method is high sensitivity and simple operation,and is suitable for the determination of 1-methoxy-2-propanol in urine of occupational exposure population.

关 键 词：色谱法 气相 固相微萃取 1-甲氧基-2-丙醇 丙二醇甲醚 尿 

分 类 号：R446[医药卫生—诊断学] O65[医药卫生—临床医学]