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Title:: Determination of dimethylsulfate in workplace air by gas chromatography with pre-column derivatization

作者:: 张耕¹; ²; 许兵³; 梅勇¹; ²; 1. 武汉科技大学医学院公共卫生学院，湖北武汉 430063；
2. 职业危害识别与控制湖北省重点实验室，湖北武汉 430063；
3. 十堰市职业病防治院湖北十堰 442000

Author(s):: ZHANG Geng*; XU Bing; MEI Yong; *Medical College, Wuhan University of Science and Technology, Wuhan 430063, China

摘要:: 目的建立新的柱前衍生气相色谱-火焰离子化检测器测定工作场所空气中硫酸二甲酯方法。方法空气中硫酸二甲酯经过苯胺、氢氧化钠和异丙醇混合吸收液吸收，60℃水浴加热反应30 min后，硫酸二甲酯衍生化生成N - 甲基苯胺，经DB - 5毛细管色谱柱分离，火焰离子化检测器检测，标准曲线法定量。结果硫酸二甲酯线性回归方程为y = 0.950x - 0.100；在0.36～133.2 μg/ml范围内，相关系数为0.9998，相对标准偏差小于6.35%，检出限为0.12 μg/ml（以3倍信噪比计），最低检出浓度为0.05 mg/m3（以采集4.5 L空气计）；加标回收率为100.98%～104.48%，样品在室温条件下至少保存7 d。结论该方法快速、简便、结果可靠，适用于工作场所空气中硫酸二甲酯的测定。

Abstract:: Objective To establish a gas chromatography method for the determination of dimethylsulfate (DMS) in workplace air using pre-column derivation. Methods DMS in air sample was collected with a mixture of aniline, isopropanol and sodium hydroxide solution and then DMS was derivatized in 60℃ waterbath for 30 min to form N-methylaniline which was analyzed by gas chromatography with flame ionization detection. The sample was separated with DB-5 chromatographic column and the quantitative detection was performed based on the standard curve method. Results The linear regression equation was y=0.950x-0.100 with a regression coefficient of 0.9998 in the range of 0.36μg/mL to 133.20μg/mL. The relative standard deviation (RSD) was less than 6.35% (n=6). The limit of detection (LOD) was 0.12μg/mL (S/N=3), and the lowest detectable concentration was 0.05mg/m3(4.5L air sample). The recoveries were 100.98%-104.48%. The samples could be stable for at least 7 days at room temperature. Conclusion The method is fast, convenient, accurate and sensitive and it can be applied for the determination of dimethylsulfate in workplace air.