5-Br-PADAP衍生反相高效液相色谱法测定有机物中的氟含量  

Determination of fluoride in organics by RP-HPLC with 5-Br-PADAP pre-column derivation

作　　者：陈红梅[1,2] 朱春华[2] 杨文杰[2] 

机构地区：[1]全国染料标准化技术委员会印染助剂分委会,杭州311215 [2]浙江传化股份有限公司,杭州311215

出　　处：《天津工业大学学报》2011年第5期50-53,共4页Journal of Tiangong University

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.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.

关 键 词：5-BR-PADAP 反相高效液相色谱 氟离子 三元络合物 

分 类 号：TS190.112[轻工技术与工程—纺织化学与染整工程] TQ615.9[轻工技术与工程—纺织科学与工程]