尿中二氯甲烷的顶空固相微萃取-气相色谱测定方法  

Determination of dichloromethane in urine by headspace solid phase microextraction-gas chromatography

作　　者：夏红芳[1] 梅勇[1] 张鑫[1] 刘佩佩[1] 吴宇伉 张博[1] 

机构地区：[1]武汉科技大学公共卫生学院,湖北武汉430065

出　　处：《中国卫生检验杂志》2016年第1期32-34,40,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立尿样中二氯甲烷的顶空固相微萃取-气相色谱分析方法,为我国二氯甲烷职业接触者生物监测提供方法参考。方法利用顶空固相微萃取技术进行分离富集,并对萃取涂层、平衡温度、平衡时间和盐析剂等萃取条件进行优化;气相色谱法测定,以保留时间定性,峰面积定量。结果二氯甲烷在0.015 mg/L^0.662 mg/L时,呈现良好的线性关系,相关系数(r)=0.999 5,检出限为0.015 mg/L。在0.166 mg/L、0.331 mg/L、0.662 mg/L 3种加标浓度下,方法的平均回收率为92.2%~104.2%,精密度为1.59%~3.64%。选择萃取涂层为50/30μm DVB/CAR/PDMS,平衡温度为25℃,顶空萃取时间为10 min,盐析剂为2.0 g无水Na2SO4,尿样体积为5.0 ml。结论该法操作简便,灵敏准确,适用于职业接触者尿中二氯甲烷的生物监测。Objective To establish a method for the determination of dichloromethane in urine using head space solid phase microextraction coupled with gas chromatography, to provide reference on methods monitoring occupational exposure to dichloromethane. Methods Head space solid phase microextraction was used for the separation and enrichment of dichloromethane, and the conditions of the coatings, extraction temperature, extraction time and the salt species were optimized. Gas chromatography method was used to determine the retention time and peak area. Results Dichloromethane showed a good linear relationship among 0. 015 mg/L -0.662mg/L, correlation coefficient（r） was 0. 999 5 ; the limit of detection was 0. 015 mg/L. At 3 additive concentration of 0. 166 mg/L, 0. 331 mg/L, 0. 662 mg/L, the average recoveries were from 92.2% to 104.2% , precision was among 1.59% - 3.64%. Parameters were optimized as the coating of 50/30 μm DVB/CAR/PDMS, extraction temperature of 25℃, extraction time of headspace of 10 min, salting - out agent of 2.0 g anhydrous Na2SO4 and the sample volume of 5.0 ml. Conclusion The method is simple, sensitive and accurate. It is suitable for the routine biomonitoring of workers ex- posed to dichloromethane.

关 键 词：顶空固相微萃取法 气相色谱法 二氯甲烷 尿样 

分 类 号：O657.71[理学—分析化学]