College of Chemistry, Jilin University, Changchun, P. R. China.
J Sep Sci. 2011 Mar;34(6):675-80. doi: 10.1002/jssc.201000807. Epub 2011 Jan 31.
In this study, a novel method for the determination of nitroanilines in hair dye samples has been developed based on poly(methacrylic acid-co-ethylene glycol dimethacrylate) monolith microextraction (PMME) and high-performance liquid chromatography (HPLC) analysis. Four nitroanilines, p-nitroaniline (PNAL), m-nitroaniline (MNAL), o-nitroaniline (ONAL), and 2,4-dinitroaniline (DNAL), are studied as representatives. To obtain optimum extraction efficiency, several experimental parameters including sample flow rate, sample volume, sample pH, and eluent flow rate have been investigated. Under the optimal experimental conditions, the linear regression coefficients of the standard curves are greater than 0.9990. The limits of detection for p-nitroaniline, m-nitroaniline, o-nitroaniline, and 2,4-dinitroaniline are 0.012, 0.008, 0.018, and 0.005 μg/mL, respectively. The intraday and interday relative standard deviations are less than 3.1 and 5.4%, respectively. The proposed method is simple, rapid, sensitive, and competent when used for the determination of nitroanilines in hair dye samples and the accuracy is assessed through recovery experiments.
本研究基于聚(甲基丙烯酸-co-乙二醇二甲基丙烯酸酯)整体柱微萃取(PMME)和高效液相色谱(HPLC)分析,开发了一种测定染发剂中硝基苯胺的新方法。以对硝基苯胺(PNAL)、间硝基苯胺(MNAL)、邻硝基苯胺(ONAL)和 2,4-二硝基苯胺(DNAL)为代表,研究了四种硝基苯胺。为了获得最佳萃取效率,考察了样品流速、样品体积、样品 pH 值和洗脱液流速等实验参数。在最佳实验条件下,标准曲线的线性回归系数均大于 0.9990。对硝基苯胺、间硝基苯胺、邻硝基苯胺和 2,4-二硝基苯胺的检出限分别为 0.012、0.008、0.018 和 0.005μg/mL。日内和日间相对标准偏差分别小于 3.1%和 5.4%。该方法简单、快速、灵敏,适用于染发剂中硝基苯胺的测定,通过回收率实验评估了其准确性。