索氏提取-高效液相色谱法测定大气颗粒物中的十溴联苯醚

Determination of Decabrominated Diphenyl Ether in Gas Particle Samples Using Soxhlet Extract Method Followed by High Performance Liquid Chromatography

建立了一种测定大气颗粒物中十溴联苯醚（deca BDE）的分析方法.首先采用索氏提取法对大气颗粒物中的十溴联苯醚进行萃取,然后采用高效液相色谱-紫外法（HPLC-UV）进行十溴联苯醚含量测定.方法的最佳条件为：萃取体系体积比为1∶2的丙酮-正己烷混合溶液,萃取时间48 h.含量测定条件为：采用ODS-BP的C18柱固定相,流动相体积比为97∶3的甲醇-水溶液,流速1.0 m L/min,紫外检测波长226 nm.该方法在10~200μg/g的范围内,具有较好的线性关系,线性方程为y=1.783 1x＋13.24 8,R2=0.997 6,加标回收率为90.0%~103.3%,RSD最大为5.0%,检出限为0.53μg/g,定量限为1.77μg/g.

A new method was developed to determinate decabrominated diphenyl ether（ deca BDE） in gas particle samples. The samples were extracted by Soxhlet method to accumulate deca BDE,and analyzed using high performance liquid chromatography（ HPLC） with ultra-variable wavelength（ UV） detector. The optimum conditions were attained as follows： the extracted reagent was a mixture of acetone and hexane（ the ratio of 1∶ 2）,and extracted time was 48 h.A ODS-BP C18 column was used,methanol-water（ 97∶ 3） was used as mobile phase,the flow rate was 1. 0 m L / min,the wavelength of detector was 226 nm. Linearity was observed well as y = 1. 783 1x ＋ 13. 248 in the range of 10 ~ 200μg /g,and the coefficient of correlation（ R2） was 0. 997 6. The average recoveries ranged from 90. 0% to 103. 3%,and the relative standard deviations（ RSD） were less than 5. 0%. The limit of detection（ LOD）,was 0. 53 μg / g,and the limit of quality（ LOQ） was 1. 77 μg / g.