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柱前衍生气相色谱法测定工作场所空气中的硫酸二甲酯(PDF)

《现代预防医学》[ISSN:1003-8507/CN:51-1365/R]

期数:
2018年12期
页码:
2137-2140
栏目:
环境与职业卫生
出版日期:
2018-06-30

文章信息/Info

Title:
Determination of dimethylsulfate in workplace air by gas chromatography with pre-column derivatization
作者:
张耕12许兵3梅勇12
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
关键词:
气相色谱法火焰离子化检测器硫酸二甲酯工作场所空气
Keywords:
Gas chromatography FID Dimethyl sulfate Workplace air
分类号:
R134
DOI:
-
文献标识码:
A
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.

参考文献/References

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备注/Memo

备注/Memo:
基金项目:职业危害识别与控制湖北省重点实验室开放基金项目(OHIC2017G13)
作者简介:张耕(1985 - ),男,在读硕士,主管理化检验技师,研究方向:卫生检验与检疫
通讯作者:梅勇,E-mail:meiyong2006@163.com
更新日期/Last Update: 2018-06-27