毛细管电泳-场强放大样品堆积法检测染发剂中的7种苯胺类物质

建立了毛细管电泳-场强放大样品堆积测定染发剂中4,4′-二氨基二苯甲烷、苯胺、邻甲氧基苯胺、对氨基苯甲醚、3,4-二甲基苯胺、间氨基苯酚、1-萘胺7种苯胺类物质的分析方法。在优化的缓冲溶液体系(0.15 mol/L NaH2PO4,0.015 mol/L 三乙醇胺, pH 2.3)下7种分析物在6.5 min内实现基线分离。考察了样品中添加的磷酸浓度和乙腈浓度、水柱长度、电动进样时间与电压对场强放大富集效率及重现性的影响。最佳的富集条件为: 水柱注入3.45 kPa(0.5 psi)×6 s,样品中添加40%(v/v)乙腈和0.6×10~3mol/L磷酸,进样电压与进样时间为10 kV×10 s。线性范围为3～1000 μg/L(R2＞0.996),检出限为0.26～2.75 μg/L,将已有方法的检测灵敏度提高了1～3个数量级。在2种市售黑色染发剂中均检测到间氨基苯酚,含量分别为7.32 mg/g和1.34 mg/g。平均加标回收率为74%～108%。该方法灵敏度高、快速、重现性好、成本低,可供多种样品基质中痕量苯胺类污染物及其他阳离子物质的测定借鉴使用。

Determination of seven aromatic amines in hair dyes by capillary electrophoresis coupled with field-amplified sample stacking

A method for the determination of 4,4'-methylenedianiline, aniline, o-anisidine, 3, 4-dimethylaniline, p-anisidine, 3-aminophenol, 1-naphthylamine in hair dyes was established by capillary electrophoresis coupled with field-amplified sample stacking. The optimum running buffer was an aqueous solution containing 0.15 mol/L NaH2PO4 and 0.015 mol/L trolamine (pH 2.3), and the baseline separation was achieved within 6.5 min. The effects of phosphoric acid and acetonitrile concentration in the sample matrix, the length of the preinjection water plug, and the sample injection voltage and time on the stacking efficiency were investigated. The optimum stacking conditions for the real samples included a water plug of 3.45 kPa (0.5 psi) x 6 s, the addition of 40% (v/v) acetonitrile and 0.6 x 10(-3) mol/L phosphoric acid to the sample solution and a sample injection of 10 kV x 10 s. The seven analytes all showed good linearities (R2 > 0.996) within 3 - 1 000 microg/L, with the detection limits in the range of 0.26 - 2.75 microg/L. The method was shown to provide over 1 - 3 magnitudes of sensitivity enhancement. 3-Aminophenol was found in two black hair dyes, and the amounts were 7.32 mg/g and 1.34 mg/g, individually. The recoveries ranged from 74% - 108%. The proposed approach may find widespread applications for the determination of trace aromatic amines and other cationic analytes in various sample matrixes.