固相萃取富集-高效液相色谱分离和测定邻甲苯胺和邻硝基甲苯  被引量:7

Determination of o-Toluidine and o-Nitrotoluene Using Solid-phase Extraction and High Performance Liquid Chromatography

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作  者:李金昶[1] 周济舟[1] 辛暨华[2] 褚莹[1] 于艳春[1] 盛有山[1] 

机构地区:[1]东北师范大学分析测试中心,长春130024 [2]长春生物制品研究所

出  处:《分析化学》2003年第2期167-170,共4页Chinese Journal of Analytical Chemistry

摘  要:建立了以固相萃取技术进行富集 ,高效液相色谱进行分离和检测邻甲苯胺和邻硝基甲苯的方法。污染水中的邻甲苯胺和邻硝基甲苯采用Sep pakC1 8萃取柱进行固相萃取。色谱分离条件是 :Shim PackCLCODS(1 5 0mm× 4 .6mmid ,5 μm)柱为分析柱 ,甲醇 水 =60∶4 0 (V V)为流动相 ,流速为 1 .0mL min,邻甲苯胺和邻硝基甲苯的紫外检测波长分别为 2 3 0nm和 2 5 4nm ,本法具有良好的灵敏度和重现性。A simple, rapid and sensitive method for the determination o-toluidine and o-nitrotoluene in sample using solid-phase extraction (SPE) and high performance liquid chromatography with ultraviolet detection was developed. A SPE procedure was described for extracting and preconcentrating o-toluidine and o-nitrotoluene on sep-pak C-18 cartridges, with methanol as solvent. The mobile phase of methanol-water was used for the separation and determination. The chromatographic separation of o-toluidine and o-nitrotoluene was performed on a Shim-pak CLC ODS column and detection by ultraviolet detection at 230 mn and 254 nm respectively. The detection limit of the o-toluidine and o-nitrotoluene was 0.063 mg/L and 0.048 mg/L respectively. Recovery was 96.4% for o-toluidine and 95.93% for o-nitrotoluene with relative standard deviation, of 2.3% for o-toluidine and 1.58% for o-nitrotoluene.

关 键 词:邻甲苯胺 邻硝基甲苯 固相萃取 富集 高效液相色谱 分离 测定 分析 

分 类 号:O658[理学—分析化学]

 

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