正相吸附高效液相色谱法定量分析过氧化氢工作液中蒽醌及降解物  

Quantitative Analysis of Anthraquinone and Degradation Products of Hydrogen Peroxide Working Solution by Normal-phase Adsorption High Performance Liquid Chromatography

作　　者：段正康[1] 曾航日[1] 彭叶[1] 李海涛[1] 王贵城[1] 李勇[1] 王世青[1] 

机构地区：[1]湘潭大学化工学院,湖南湘潭411105

出　　处：《分析科学学报》2014年第4期485-488,共4页Journal of Analytical Science

基　　金：中国石油化工股份有限公司巴陵分公司资助项目

摘　　要：建立了定量分析过氧化氢工作液中蒽醌及降解物的正相吸附高效液相色谱法。采用Agilent ZORBAX SIL色谱柱（250×4.6mm,5μm）,柱温30℃,以正己烷-二氯甲烷-乙酸乙酯（体积比80∶19.5∶0.5）为流动相,流速1.0mL/min,紫外检测波长254nm。对2-乙基蒽醌（EAQ）和四氢-2-乙基蒽醌（H4EAQ）采用色谱峰保留时间定性和外标法定量,EAQ和H4EAQ定量分析线性相关系数都在0.999以上,加标平均回收率为98.9%-101.0%,相对标准偏差（RSD,n=5）在0.5%-1.2%之间。降解物总含量或单个降解物含量采用与EAQ和H4EAQ相对校正因子为1的面积之和比进行计算。该方法简单快速、准确性高,色谱柱使用寿命长,可满足过氧化氢工作液中EAQ、H4EAQ及降解物的定量分析要求。A normal-phase adsorption high-performance chromatography method has been established for the separation and quantitative determination of 2-ethylanthraquinone （EAQ）, tetrahydro-2-ethylanthraquinone （H4EAQ） and the degradation products of hydrogen peroxide working solution. An Agilent ZORBAX SIL（250× 4.6 mm, 5 μm） column was adopted at the column temperature of 30 ℃. The mobile phase consisted of N-hexane-dichloromethane-ethyl acetate（80： 19.5：0.5,V/V） at a flow rate of 1 mL/min. The detection was performed by an ultraviolet absorbance detector at 254 nm. The qualitative analysis of EAQ and H4 EAQ was achieved by peak retention time and the quantitative analysis was achieved by external standard method. The results showed that the linear correlation coefficients of EAQ and H4EAQ were both above 0. 999,the average recoveries of the two compounds were 98. 9%-101.0% and the relative standard deviations were 0.5 %-1.2 %（n= 5）. This method is simple, rapid, accurate, and suitable for the quantitative analysis of EAQ, H4 EAQ and hydrogen peroxide degradation products with long column life.

关 键 词：正相吸附高效液相色谱法 过氧化氢工作液 降解物 定量分析 

分 类 号：O657.72[理学—分析化学]