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 |
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引用本文: | 李金昶,周济舟,辛暨华,褚莹,于艳春,盛有山.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[J].分析化学,2003,31(2):167-170. |
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作者姓名: | 李金昶 周济舟 辛暨华 褚莹 于艳春 盛有山 |
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作者单位: | 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 |
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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。
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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 |
Determination of o-Toluidine and o-Nitrotoluene Using Solid-phase Extraction and High Performance Liquid Chromatography |
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Abstract: | 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 nm 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. |
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Keywords: | High performance liquid chromatography solid-phase extraction o-toluidine o-nitrotoluene |
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