气相色谱法测定工作场所空气中氯甲甲醚和双氯甲醚  

Detection of chloromethyl methyl ether and bis-chloromethyl ether in workplace air by gas chromatography

作　　者：戎伟丰[1] 凌伟洁[2] 胡嘉雯 何嘉恒[1] 丘静静 蒙瑞波[1] 阮小林[1] 

机构地区：[1]广东省职业病防治院,广东省职业病防治重点实验室,广东广州510300 [2]广州市职业病防治院,510620

出　　处：《中国职业医学》2017年第1期75-79,共5页China Occupational Medicine

基　　金：广东省职业病防治重点实验室(2012A061400007);广东省医学科研基金(A2015626)

摘　　要：目的建立工作场所空气中氯甲甲醚(CMME)和双氯甲醚(BCME)的气相色谱测定方法。方法空气中的CMME和BCME经吸收液采集后,经衍生化处理,衍生产物在碱性条件下用正己烷萃取,毛细管色谱柱分离,电子捕获检测器检测,标准曲线法定量。结果本方法测定CMME和BCME的质量分别在2.00~80.00和1.32~52.80 ng时线性关系良好,线性相关系数均为0.999 93;最低检出浓度均为0.030μg/m3,最低定量浓度均为0.100μg/m3(以采集7.50 L空气计);加标回收率分别为99.35%~101.00%和97.99%~101.70%;批内相对标准偏差(RSD)分别为2.73%~4.46%和2.61%~3.82%,批间RSD分别为3.10%~5.50%和3.89%~5.38%;采样效率分别为92.43%~96.25%和91.43%~94.03%;CMME和BCME样品在室温下至少可储存15 d。结论本方法适用于工作场所空气中CMME和BCME的检测。Objective To establish a methodology for simultaneous detection of chloromethyl methyl ether（ CMME） and bis-chloromethyl ether（ BCME） in workplace air by gas chromatography. Methods CMME and BCME in workplace air were collected with absorption solution which was also derivatization solution. The derivative products were extracted using n-hexane alkaline medium. The extracts were separated by capillary column and detected with electron capture detector.The quantification was performed by use of standard curves. Results The linearity ranges of CMME and BCME were2. 00-80. 00 and 1. 32-52. 80 ng,respectively. The correlation coefficients were both 0. 999 93. The minimum detectable concentrations were both 0. 030 μg / m^3 and the minimum quantification concentrations were both 0. 100 μg / m3（ 7. 50 L sample）. The recovery rates were 99. 35%-101. 00% and 97. 99%-101. 70% respectively. The within-run relative standard deviations（ RSD） were 2. 73%-4. 46% and 2. 61%-3. 82% respectively,and the between-run RSD were3. 10%-5. 50% and 3. 89%-5. 38% respectively. The sampling efficiencies were 92. 43%-96. 25% and 91. 43%-94. 03%respectively. The samples were stable at room temperature for at least 15 days. Conclusion This method is suitable for simultaneous detection of CMME and BCME in workplace air.

关 键 词：工作场所 空气 氯甲甲醚 双氯甲醚 衍生反应 气相色谱法 

分 类 号：R134.4[医药卫生—劳动卫生]