建立了气相色谱-串联质谱(GC-MS/MS)准确、快速测定皮革和纺织品中富马酸二甲酯(DMF)的分析方法.样品经乙酸乙酯提取、浓缩及固相萃取柱净化处理,通过VF-5ms色谱柱分离、串联质谱对DMF进行定性和定量分析.实验结果表明:优化样品预处理条件、固相萃取条件、质谱分析条件后,该方法可进一步消除杂质干扰,结果准确可靠,灵敏度、精密度、线性关系良好,回收率较高.3种浓度水平的加标回收率(n=6)保持在84% ～93%之间,相对标准偏差小于7.2% ;DMF在8种皮革和纺织品中的检出限 (S/N=3)为0.012～0.039 mg/kg, 0.05～100 mg/L 质量浓度范围内线性相关系数为 0.9990,适用于皮革和纺织品中DMF的日常检测.
An effective method for the determination of dimethyl fumarate (DMF) in leather and textiles by gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed. Samples of leather or textiles were extracted with ethyl acetate and concentrated, DMF was separated on a VF-5ms column and analyzed by GC-MS/MS after solid phase extraction (SPE) process. The result shows that this method is sensitive, accurate and reliable. The linear relationship was perfect and the interference with background signal was further eliminated after pretreatment, SPE and GC-MS/MS analytical conditions were optimized. The average recoveries of DMF in leather and textiles at three levels ranged from 84% to 93% , the relative standard deviations (n=6) were lower than 7.2% , the limits of detection in the range from 0.012 to 0.039 mg/kg (S/N=3), the correlation coefficient was 0.9990 over the range 0.05-100 mg/L. It has been applied to routine determination of DMF in leather and textiles with satisfactory results.
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