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    气相色谱-质谱法选择离子存储检测模式测定皮革和纺织品中富马酸二甲酯

    GC-MS Determination of Dimethylfumarate in Leather and Textile with Detection Mode of Selected Ion Storage

    • 摘要: 提出了用气相色谱-质谱法选择离子存储检测模式测定皮革和纺织品中富马酸二甲酯的方法.试样经乙酸乙酯提取后,在40 ℃真空旋转蒸发器中浓缩至2.0 mL.用乙酸乙酯稀释定容至50 mL,离心后取1 mL上清液过中性氧化铝固相萃取小柱净化,用乙酸乙酯淋洗定容至2 mL,通过VF-5ms色谱柱分离,采用离子阱的选择离子存储检测模式,结合保留时间、特征离子的相对丰度比及谱库检索信息对富马酸二甲酯进行定性检测,用外标法进行定量分析.富马酸二甲酯质量浓度在0.01~50.0 mg·L-1内与峰面积呈线性关系,检出限(3S/N)为0.02 mg·kg-1.用标准加入法做回收试验,测得平均回收率在80%~92%之间,相对标准偏差(n=6)小于5.5%.

       

      Abstract: A rapid method for determination of dimethylfumarate (DMFU) in leather and textiles by GC-MS with selected ion storage (SIS) detection mode was proposed.DMFU in sample was extracted with ethylacetate ultrasonically and the extract was concentrated to 2.0 mL in a rotary evaporator at 40 ℃.After diluting to 5.0 mL with ethylacetate,the solution was centrifuged,and 1 mL of the supernatant was taken and purified by SPE on a neutral Al2O3 column.Eluant (in a total volume of 2 mL of ethylacetate) obtained was used for GC-MS analysis.The VF-5ms column was used for separation.Identification of DMFU was performed on the base of retention time,relative abundance of the characteristic ions and inspection of the spectra database;and its determination was carried out by the external standard method.Linear relationship was obtained between values of peak area and concentration of DMFU in the range of 0.01-50.0 mg·L-1,with detection limit (3S/N) of 0.02 mg·kg-1.Recovery was tested and values of average recovery were found in the rnage of 80%-92% with RSD′s (n=6) less than 5.5%.

       

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