气相色谱-质谱法测定涂料漆膜中禁用偶氮染料  

Determination of the banned azo dyes in paint films by gas chromatography-mass spectrometry

作　　者：肖湾 马红青[1] 顾春思 XIAO Wan;MA Hongqing;GU Chunsi(Shanghai Institute of Quality Inspection and Technical Research,Shanghai 201114,China)

机构地区：[1]上海市质量监督检验技术研究院,上海201114

出　　处：《化学分析计量》2024年第5期29-35,共7页Chemical Analysis And Meterage

基　　金：上海市质量监督检验技术研究院科研项目(KY-2022-18-QH);上海市科学技术委员会研发公共服务平台建设项目(14DZ2293000)。

摘　　要：建立一种测定涂料漆膜中禁用偶氮染料含量的气相色谱-质谱分析方法。在柠檬酸盐缓冲溶液中,用低亚硫酸钠将涂料漆膜样品中的偶氮染料还原裂解为芳香胺,然后加入氯化钠,调节溶液的离子强度,加入氢氧化钠调节溶液的酸碱性,以乙酸乙酯作为溶剂提取其中的芳香胺,提取液经0.45μm有机滤膜过滤,采用气相色谱-质谱法测定,以内标法进行定量。23种芳香胺在质量浓度为1~30mg/L范围内线性相关系数均不小于0.996,检出限均小于5 mg/kg。高、中、低3个水平的加标回收率为71.2%~101.3%,测定结果的相对标准偏差为1.2%~9.7%(n=6)。该方法满足涂料漆膜中禁用偶氮染料含量的检测要求。A method was established to determine the content of banned azo dyes in paint films by gas chromatography-mass spectrometry.The azo dyes in the paint film samples were reductively cleaved to aromatic amines in citrate buffer solution using sodium hydrosulfite,and then sodium chloride was added to adjust the ionic strength of the solution,sodium hydroxide was added to adjust the acidity and alkalinity of the solution,and ethyl acetate was used as the solvent for extracting aromatic amines in the sample,and the extract was filtered through a 0.45μm organic filter for the determination by gas chromatography-mass spectrometry and the method of quantification was performed by the internal standard method.The linear correlation coefficients of 23 aromatic amines were not less than 0.996 in the range of 1-30 mg/L,and the limits of detection were all less than 5 mg/kg.The recoveries of 23 aromatic amines spiked at three levels of high,medium and low were in the range of 71.2%-101.3%,and the relative standard deviations were in the range of 1.2%-9.7%(n=6).The method can meet the requirements for the determination of the banned azo dyes in paint films.

关 键 词：气相色谱-质谱色谱法 涂料 禁用偶氮染料 

分 类 号：O657.7[理学—分析化学]