高效液相色谱法用于氧化型染发产品中42种限用染发剂的筛查和定量分析

Qualitative screening and quantitative analysis of 42 restricted hair dyes in oxidative hair color products by high performance liquid chromatography

建立了一种利用高效液相色谱筛查和定量分析氧化型染发产品中42种限用染发剂的方法。染发产品经亚硫酸氢钠水溶液-乙醇超声提取后,以0.02 mol/L乙酸铵水溶液-乙腈为流动相,在TechMate AQUA-STIII色谱柱上进行梯度洗脱和分离,选择235和280 nm作为检测波长,对42种染发剂进行一次性定性筛查,同时实现其中35种染发剂的定量分析,当筛查结果表明产品中含有2,6-二甲氧基-3,5-吡啶二胺盐酸盐、2-甲基-5-羟乙氨基苯酚等7种染发剂时,以0.02 mol/L乙酸铵水溶液-乙腈为流动相,在Waters Symmetry C_(18)色谱柱上进行等度洗脱,选择235 nm作为检测波长进行定量分析。结果表明:42种染发剂的方法检出限为10~101μg/g,定量限为33~337μg/g。在相应的线性范围内,42种染发剂色谱峰面积与质量浓度线性关系良好,相关系数(r)均大于0.9998。在4个不同含量水平下,各目标化合物的平均回收率在81.3%~119.6%之间,RSD不大于5%。

A method for qualitative screening and quantitative analysis of 42 restricted hair dyes in oxidative hair color products by high performance liquid chromatography(HPLC)was established.The sample was ultrasonically extracted in mixed solvent of aqueous sodium bisulfite solution and ethanol.Firstly,the liquid chromatography condition for qualitative screening of 42 dyes and for quantitative analysis of 35 of them was established,which was as follows:The mobile phase was the mixed solvent of aqueous solution of 0.02 mol/L ammonium acetate and acetonitrile;gradient elution was carried out on a TechMate AQUA-STIII column;the detection wavelengths were 235 nm and 280 nm.If the other seven dyes including 2,6-dimethoxy-3,5-pyridinediamine·HCl,2-methyl-5-hydroxyethylaminophenol,3-nitro-p-hydroxyethylaminophenol,pyrazolone methyl pyrazolone,hydroxypropyl bis(N-hydroxyethyl-pphenylenediamine)·HCl,4-chlororesorcinol and 6-hydroxyindole were detected in the products,another liquid chromatography condition was required for their quantitative analysis,which was as follows:The mobile phase was the mixed solvent of aqueous solution of 0.02 mol/L ammonium acetate and acetonitrile;isocratic elution was carried out on a Waters Symmetry C_(18) column;the detection wavelength was 235 nm.The results showed that the limits of detection(LODs)of the 42 dyes were from 10μg/g to 101μg/g,while the limits of quantification(LOQs)were from 33μg/g to 337μg/g.The 42 dyes all had good linearities in their respective range,with correlation coefficients(r)higher than 0.9998.The average spiked recoveries of 42 dyes at four levels were from 81.3%to 119.6%,with RSDs no more than 5%.