Xie Peijin, Xu Jingang, Hu Zhenzhen, El-Sepai Fawzi, Peimin Zhang, Zhu Yan
Department of Chemistry, Zhejiang University, Hangzhou 310028, P.R. China.
J Chromatogr Sci. 2011 Sep;49(8):622-7. doi: 10.1093/chrsci/49.8.622.
A new column-switching method has been proposed for the determination of 14 organic explosives (1,3,5,7-tetranitro-N-methylaniline, 1,3,5-trinitro-1,3,5-triazacyclohexane, 1,3,5-trinitrobenzene, 1,3-dinitrobenzene, nitrobenzene, 2,4,6-N-tetranitro-N-methylaniline, Trinitrotoluene, 4-amino-2,6-dinitrotoluene, 2-amino-4,6-dinitrotoluene, 2,6-dinitrotoluene, 2,4-dinitrotoluene, 2-nitrotoluene, 4-nitrotoluene, and 3-nitrotoluene) and/or five inorganic cations (Na(+), NH(4)(+), K(+), Mg(2+), and Ca(2+)) using liquid chromatography linked to ion chromatography by a switching valve. The mobile phase was methanol-water (40/60, v/v) for a C18 reversed-phase column and 3 mM of methanesulfonic acid (pH 2.5) for a cation-exchange column, respectively. Under the optimal conditions, the 14 organic explosives and the five inorganic cations were separated and detected simultaneously within 45 min. The limits of detection (S/N = 3) of the 14 organic explosives and the five inorganic cations were in the range of 0.0048-0.0333 mg/L and 0.0116-0.1851 mg/L, respectively. The linear correlation coefficients were 0.9971-0.9999, and the relative standard deviation of the retention time and the peak area were 0.02-0.31% and 0.51-3.64%, respectively. The method was successfully applied to the determination of organic explosives and inorganic cations in dust samples.
提出了一种新的柱切换方法,用于测定14种有机炸药(1,3,5,7-四硝基-N-甲基苯胺、1,3,5-三硝基-1,3,5-三氮杂环己烷、1,3,5-三硝基苯、1,3-二硝基苯、硝基苯、2,4,6-N-四硝基-N-甲基苯胺、三硝基甲苯、4-氨基-2,6-二硝基甲苯、2-氨基-4,6-二硝基甲苯、2,6-二硝基甲苯、2,4-二硝基甲苯、2-硝基甲苯、4-硝基甲苯和3-硝基甲苯)和/或5种无机阳离子(Na⁺、NH₄⁺、K⁺、Mg²⁺和Ca²⁺),该方法通过切换阀将液相色谱与离子色谱联用。C18反相柱的流动相为甲醇-水(40/60,v/v),阳离子交换柱的流动相为3 mM甲磺酸(pH 2.5)。在最佳条件下,14种有机炸药和5种无机阳离子在45分钟内可同时分离并检测。14种有机炸药和5种无机阳离子的检测限(S/N = 3)分别在0.0048 - 0.0333 mg/L和0.0116 - 0.1851 mg/L范围内。线性相关系数为0.9971 - 0.9999,保留时间和峰面积的相对标准偏差分别为0.02 - 0.31%和0.51 - 3.64%。该方法成功应用于粉尘样品中有机炸药和无机阳离子的测定。