氧化型染发剂中12种风险组分的加速溶剂萃取-气相色谱质谱-内标测定法

Determination of 12 risk components in oxidation hair dyes by accelerated solvent extraction-gas chromatography-mass spectrometry with internal standard

目的开发氧化型染发剂中12种风险组分的加速溶剂萃取-气相色谱质谱(GC-MS)-内标测定法,研究样品加速溶剂萃取最佳操作条件。方法样品加入石英砂、亚硫酸钠、硅酸镁混合后,使用乙酸乙酯溶剂,在压力10.0 MPa,温度100℃下,静态萃取5 min,循环1次。萃取结束后氮吹浓缩,定容过滤后供GC-MS测定,内标法定量。结果样品在1.0~100.0μg/mL浓度范围内线性关系良好,相关系数r=0.9920~0.9996;最低检出浓度0.08~0.40 mg/kg;平均回收率为81.0%~101.5%;相对标准偏差(RSD)在1.95%~6.27%之间。结论该方法分析简单、快速、准确,可用于氧化型染发剂风险组分检测。

Objective To develop a method for the determination of 12 risk components in oxidation hair dyes by solvent extraction-gas chromatography-mass spectrometry(GC-MS)with internal standard,study the optimum operating conditions of accelerated solvent extraction.Methods The samples mixed with quartz sand,sodium sulfite and magnesium silicate were extracted using solvent of ethyl acetate for 5 min at 10.0 MPa and 100℃for one cycle.The extract was concentrated with nitrogen and diluted to volume and filtrated.The analytes were determined by GC-MS and quantified by internal standard method.Results Good linearity was observed in the range of 1.0-100.0μg/mL with correlation coefficients(r)from 0.9920 to 0.9996.Minimum detection concentration was in ranges of 0.08-0.40 mg/kg.The average recovery and the relative standard deviations(RSD)were in ranges of 81.0%-101.5%and 1.95%-6.27%,respectively.Conclusion The method is simple,rapid and accurate.It is suitable for the analysis of risk components in oxidation hair dyes.