高效液相色谱串联光谱及质谱测定纺织品中35种有害染料

High Performance Liquid Chromatography Tandem Spectrum and 35 Kinds of Harmful Dyes in the Textile of Mass Spectrometry Determination

采用高效液相色谱-二极管阵列检测器-质谱(HPLC-DAD-MS)快速测定纺织品中的35种有害染料。研究设计丙酮快速溶剂提取法的提取效率是超声波提取法的2.4~12.3倍,色谱柱为Agilent ZORBAX SB-C18 narrow-bore column 2.1 x 50mm,比150mm(5μm)色谱柱分析时间缩短了四分之三,比100mm(1.8μm)色谱柱分析时间缩短了三分之一,极大的提高了分析效率。以乙腈-0.01mol/L乙酸铵(含0.1%甲酸)溶液作为该35种染料化合物的流动相,获得了最优的色谱峰及质谱峰。该方法中,35种有害染料的检出限为2.7mg/kg^18.15mg/L,线性相关系数都大于0.995,平均回收率为70%~110%,相对标准偏差(RSD)均小于10%,可以满足纺织品中多种致癌染料同时检测的需要。

Adopting the HPLC-DAD-MS to take rapid determination of the 35 kinds of harmful dyes in textiles. The study result shows that the extraction efficiency of acetone rapid solvent extraction method is 2.4 to 12.3 times of that of ultrasonic extraction method and the chromatographic column is Agilent ZORBAX SB-C18 narrow-bore column 2.1 × 50mm and it has shortened the analysis time of 150mm （ 5μm ） chromatographic column by three-quarter and has shortened the analysis time of lOOmm （1.8μm） chromatographic column by one third, which has improved the analysis efficiency greatly. Take the acetonitrile -0.01mol/L ammonium acetate （containing 0.1 % formic acid） as the mobile phase of these 35 kinds of dye compounds, which has got the most excellent peaks and mass spectral peak. In this method, the detection limit of the 35 kinds of harmful dyes is between 2. 7mg / kg ~18.15mg / L and the linear correlation coefficient is all bigger than 0.995, besides, the average recovery rate is between 70%-110% and the relative standard deviation （RSD） is all less than 10%, which can meet the need of testing variety of carcinogenic dyes in textiles simultaneously.