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《化学分析计量》 2018年第02期
DOI:10.3969/j.issn.1008-6145.2018.02.009
气相色谱-质谱法测定涂料中游离氨基甲酸乙酯
区棋铭,黄雨锟,朱国军,李振球,黎强科,谭煜亮
广东省江门市质量计量监督检测所,广东江门 529000 
Determination of free ethyl carbamate in coating by gas chromatography-mass spectrometry
OU Qiming,HUANG Yukun,ZHU Guojun,LI Zhenqiu,LI Qiangke,TAN Yuliang
Guangdong Jiangmen Supervision Testing Institute of Quality and Metrology, Jiangmen 529000, China 
摘要:采用气相色谱-质谱法测定涂料中游离氨基甲酸乙酯的含量,对样品进行超声波萃取和高速离心静化处理后,选用选择离子和保留时间定性、外标法定量,色谱柱选择RTX-WAX极性色谱柱。游离氨基甲酸乙酯的质量浓度在0.1~10.0 μg/mL范围内与色谱峰面积呈良好的线性,线性相关系数为0.9999,检出限为0.04 μg/mL。加标回收率在96.8%~100.5%之间,测定结果的相对标准偏差为2.0%~11.1%(n=6)。该方法样品预处理简单、重现性好、准确度高,适用于涂料中游离氨基甲酸乙酯的检测。 
Abstract:The method for determination of free ethyl carbamate in coating by gas chromatography-mass spectrometry was established. After being ultrasonic extracted and high speed centrifuge static treated, the sample qualitative analysis was carried according to selective ion and retention time, while quantitative analysis by external standard. RTX-WAX polar column was used. The concentration of free carbamate was linear with chromatographic area in the range of 0.1-10.0 μg/mL, the correlation coefficient was 0.9999, and the detection limit was 0.04 μg/mL. The standard addition recoveries were 96.8%-100.5%, and the relative standard deviation of detection results was 2.0%-11.1%(n=6). This method is simple in pretreatment, has high accuracy and good reproducibility, it can meet the needs of determination of free ethyl carbamate in coatings. 
关键词:涂料;气相色谱-质谱法;游离氨基甲酸乙酯; 超声波萃取 
Keywords:coating; gas chromatography-mass spectrometry; free ethyl carbamate; ultrasonic extraction 
本文引用格式:
区棋铭,黄雨锟,朱国军,等.气相色谱-质谱法测定涂料中游离氨基甲酸乙酯[J].化学分析计量,2018,27(2):36-39.
OU Q M,HUANG Y K,ZHU G J,et al. Determination of free ethyl carbamate in coating by gas chromatography-mass spectrometry[J]. Chemical analysis and meterage,2018,27(2):36-39. 

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