| 5-Br-PADAP衍生反相高效液相色谱法测定有机物中的氟含量 |
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| 引用本文： | 陈红梅,朱春华,杨文杰.5-Br-PADAP衍生反相高效液相色谱法测定有机物中的氟含量[J].天津工业大学学报,2011,30(5):50-53. |
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| 作者姓名： | 陈红梅 朱春华 杨文杰 |
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| 作者单位： | 1. 全国染料标准化技术委员会印染助剂分委会,杭州311215;浙江传化股份有限公司,杭州311215
2. 浙江传化股份有限公司,杭州,311215 |
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| 摘 要： | 通过氧瓶燃烧对样品进行预处理,以2-(5-溴-2-吡啶偶氮)-5-二乙氨基酚(5-Br-PADAP)作为衍生试剂,在锆离子(Zr4+-)存在下对氟离子进行柱前衍生,反相高效液相色谱法测定有机物中氟离子的含量,其衍生物5-Br-PADAP-Zr4+-F-的三元络合物的最大吸收为576 nm,流动相选择乙腈/乙醇(85/15)时衍生物可与非目标物有效分离,分离度大于3,氟离子质量浓度在0.5～2.5μg/mL范围内具有良好的线性,相关系数r2=0.999 61,方法的相对标准偏差(RSD)在1.04%～3.49%,平均回收率为88.80%～108.54%,检出限可达0.8μg/mL.
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| 关 键 词： | 5-Br-PADAP 反相高效液相色谱 氟离子 三元络合物 |
Determination of fluoride in organics by RP-HPLC with 5-Br-PADAP pre-column derivation |
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| CHEN Hong-mei,ZHU Chun-hua,YANG Wen-jie.Determination of fluoride in organics by RP-HPLC with 5-Br-PADAP pre-column derivation[J].Journal of Tianjin Polytechnic University,2011,30(5):50-53. |
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| Authors: | CHEN Hong-mei ZHU Chun-hua YANG Wen-jie |
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| Affiliation: | CHEN Hong-mei1,2,ZHU Chun-hua2,YANG Wen-jie2(1.Subcommittee on Textile Auxiliaries of Technical Committee on Dyestuff of Standardization Administration of China,Hangzhou 311215,China,2.Zhejiang Transfar Co Ltd,China) |
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| Abstract: | A reversed-phase high performance liquid chromatographic(RP-HPLC) method for determination of the trace fluoride in the compounds was developed with pre-column derivation by 5-Br-PADAP.The maximum absorption of the 5-Br-PADAP-Zr4+-F-complex,which could be separated effectively at a certain condition of the Acetonitrile / ethanol(85/15) mobile phase,was found at 576 nm.The detection limit was 0.8 μg/mL,and recovery was 88.80%-108.54%.The method shows good linear relationship in the concentration of 0.5-2.5 μg/mL with the correlation coefficient of 0.999 61,giving the range of the RSD(n=6) 1.04%-3.49%,as well as the strong speciality and good repetition.This method is available to determine the trace fluride with satisfactory results. |
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| Keywords: | 5-Br-PADAP RP-HPLC fluoride ternary complexes |
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