高级检索

高效液相色谱–串联质谱法测定家具用皮革中2,4–二氨基甲苯和4,4′–二氨基二苯甲烷

Determination of 2, 4-Diaminotoluene and 4, 4'-Diaminodiphenylmethane in Furniture Leather by High Performance Liquid Chromatography-tandem Mass Spectrometry

  • 摘要: 文章建立了高效液相色谱–串联质谱法测定家具用皮革中2,4–二氨基甲苯和4,4′–二氨基二苯甲烷含量的分析方法。试验选用Shim–pack GIST–HP C18色谱柱进行分离,以0.005 mol/L乙酸铵水溶液–甲醇为流动相进行洗脱,流速为0.3 mL·min–1。质谱分析中采用电喷雾离子源及多反应监测模式,外标曲线法定量。结果表明,2,4–二氨基甲苯和4,4′–二氨基二苯甲烷在50~500 μg/L质量浓度范围内具有良好的线性关系,相关系数R2均>0.999。2,4–二氨基甲苯和4,4′–二氨基二苯甲烷检出限分别为2.13 μg/kg和0.18 μg/kg,定量限分别7.03 μg/kg和0.53 μg/kg,相对标准偏差(n=6)分别为4.75%~7.14%和2.93%~6.84%,在3个加标水平下的平均回收率分别为88.69%~93.74%和91.47%~96.84%,该方法简单快速、灵敏度高、准确可靠,适用于家具用皮革中2,4–二氨基甲苯和4,4′–二氨基二苯甲烷的检验检测。

     

    Abstract: This article established an analytical method for determining the contents of 2, 4-diaminotoluene (TDA) and 4, 4'-diaminodiphenylmethane (MDA) in furniture leather using high performance liquid chromatography-tandem mass spectrometry. The experiments used a Shim-pack GIST-HP C18 chromatographic column for separation, and 0.005 mol/L ammonium acetate aqueous solution-methanol was adopted as the mobile phase for elution at a flow rate of 0.3 mL min−1. The electrospray ion source and multi-reaction monitoring mode were used in the mass spectrometry analysis, and the external standard curve method was used for quantification. The results showed that there was a good linear relationship for TDA and MDA in the mass concentration range of 50–500 μg/L with the correlation coefficients R2>0.999. The detection limits of TDA and MDA were 2.13 μg/kg and 0.18 μg/kg, respectively, and their quantification limits were 7.03 μg/kg and 0.53 μg/kg, respectively, while the relative standard deviations (RSD, n=6) were 4.75%–7.14% and 2.93%–6.84%, respectively, and the average recovery rates at three spiked levels were 88.69%–93.74% and 91.47%–96.84%, respectively. This method is simple, fast, sensitive, accurate and reliable, and is suitable for the detection of TDA and MDA in furniture leather.

     

/

返回文章
返回