流动注射在线预富集-高效液相色谱法测定四种硝基类化合物

Determination of Four Kinds of Nitro Compounds by On-line Coupled Flow Injection Preconcentration with High Performance Liquid Chromatography

建立了以香烟过滤嘴纤维作吸附剂，在线固相萃取-高效液相色谱（SPE—HPLC）测定水中邻硝基苯甲酸、对硝基苯胺、邻硝基苯酚、3-氯硝基苯四种硝基类化合物的方法。邻硝基苯甲酸、对硝基苯胺、邻硝基苯酚、3-氯硝基苯分别在0．006～4．80、0．003～2．40、0．002～1．60、0．002～1．60mg／L范围内峰面积与浓度呈线性关系，相关系数分别为0．9994、0．9996、0．9997和0．9996；检出限（S／N=3）分别为1．0、0．8、0．6，0．6μg／L；富集倍数分别为28．2、176．6、172．1、153．3。该法用于河水中四种硝基类化合物的测定，回收率为85．41％～116．44％，相对标准偏差在1．1％～5．4％范围内。

A new method was established for the determaination of nitro compounds in water by on-line coupled solid-phase extraction （SPE） with high-performance liquid chromatography （HPLC）. A preconcentration column packed with the cigarette filter was used to replace a conventional sample loop on the injector valve of the HPLC for on-line solid-phase extraction. The collected analytes were subsequently eluted with a mobile phase of methanol-water （65：35,V/V） for HPLC separation. The separation was performed on a chromatographic column Eclipse XDB-C18 with the flow rate of the mobile phase at 0.8 mL/min and the detection wavelength was set at 213 nm. There were excellent linearity between peak area and concentration of analytes in the concentration range of 0. 00644.80 mg/ L for o-nitrobenzoic acid, 0. 003-2.40 mg/L for p-nitroaniline, 0. 002-1.60 mg/L for o-nitrophenol and 0. 002-1.60 mg/L for 3-chloro-nitrobenzene with the correlation coefficients of 0. 9994,0. 9996, 0. 9997 and 0. 9996, respectively. The detection limits （S/N=3） were 1.0 μg/L, 0.8 gg/L, 0.6 μg/L and 0.6 μg/L respectively. The enhancement factors were 28.2,176.6,172.1 and 153.3, respectively. The developed method was applied to the analysis of four kinds of nitro compounds in river water samples with recovery for the spiked samples in the range of 85.41% to 116.44%, and the RSD was from 1.1% to 5.4 %.