气质联用法同时测定氧化型染发剂中13种染料中间体方法建立

Simultaneous determination of 13 dye intermediates in oxidized hair coloring agent by gas chromatography-mass spectrometry

目的本文采用气相色谱-质谱法建立同时测定氧化型染发剂中13种染料中间体的方法。方法样品采用乙酸乙酯进行超声波提取,以质谱全扫描方式进行数据定性,标准曲线进行定量。结果优化了样品前处理和色谱分离条件,建立了氧化型染发剂中13种染料中间体的同时测定方法,13种染料中间体线性范围在1.0μg/ml^10.0μg/ml内,线性良好,相关系数在0.9920~0.9995之间,平均加标回收率(n=6)为89.2%~106.5%之间,相对标准偏差(n=10)为1.18%~6.66%,最低检出限为0.01 ng^0.22 ng。结论所建立的气相色谱-质谱联用方法灵敏度高,操作简单,快速,实验结果准确,适用于染发剂中多类别染料中间体检测。

Objective A method for the simultaneous determination of 13 dye intermediates in oxidized hair coloring agent was established by gas chromatography -mass spectrometry. Methods The samples were extracted by ultrasonic wave with ethyl acetate. Then MS full scan mode was used for qualitative analysis, and the standard curve was used for quantitative analysis. Results Sample pretreatment and chromatographic separation conditions were optimized to establish a method for simultaneous determination of 13 dye intermediates in oxidized hair coloring agent. The 13 dye intermediates showed good linear relationship between peak area and the concentration in the range of 1.0 μg/ml - 10.0 μg/ml, and the correlation coefficients were between 0. 9920 -0. 9995, the average recovery （n = 6 ） was between 89.2% and 106.5% , the relative standard deviation （n = 10） was between 1.18% and 6.66% , the minimum detection limit was from 0.01 ng to 0.22 ng. Conclusion The gas chromatography - mass spectrometry method exhibits high sensitivity, easy operation, high speed and accurate results. It is suitable for detec- tion of a variety of dye intermediates in hair coloring agent.