信阳师范学院学报(自然科学版)
信暘師範學院學報(自然科學版)
신양사범학원학보(자연과학판)
JOURNAL OF XINYANG NORMAL UNIVERSITY(NATURAL SCIENCE EDITION)
2015年
2期
222-225
,共4页
索氏提取法%高效液相色谱%十溴联苯醚%大气颗粒物
索氏提取法%高效液相色譜%十溴聯苯醚%大氣顆粒物
색씨제취법%고효액상색보%십추련분미%대기과립물
Soxhlet extract method%high performance liquid chromatography(HPLC)%decabrominated diphenyl ether(decaBDE)%gas particle
建立了一种测定大气颗粒物中十溴联苯醚( decaBDE)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 mL/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 =1.7831x+13.248, R2=0.9976,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.
建立瞭一種測定大氣顆粒物中十溴聯苯醚( decaBDE)的分析方法.首先採用索氏提取法對大氣顆粒物中的十溴聯苯醚進行萃取,然後採用高效液相色譜-紫外法( HPLC-UV)進行十溴聯苯醚含量測定.方法的最佳條件為:萃取體繫體積比為1∶2的丙酮-正己烷混閤溶液,萃取時間48 h.含量測定條件為:採用ODS-BP的C18柱固定相,流動相體積比為97∶3的甲醇-水溶液,流速1.0 mL/min,紫外檢測波長226 nm.該方法在10~200μg/g的範圍內,具有較好的線性關繫,線性方程為y =1.7831x+13.248, R2=0.9976,加標迴收率為90.0%~103.3%,RSD最大為5.0%,檢齣限為0.53μg/g,定量限為1.77μg/g.
건립료일충측정대기과립물중십추련분미( decaBDE)적분석방법.수선채용색씨제취법대대기과립물중적십추련분미진행췌취,연후채용고효액상색보-자외법( HPLC-UV)진행십추련분미함량측정.방법적최가조건위:췌취체계체적비위1∶2적병동-정기완혼합용액,췌취시간48 h.함량측정조건위:채용ODS-BP적C18주고정상,류동상체적비위97∶3적갑순-수용액,류속1.0 mL/min,자외검측파장226 nm.해방법재10~200μg/g적범위내,구유교호적선성관계,선성방정위y =1.7831x+13.248, R2=0.9976,가표회수솔위90.0%~103.3%,RSD최대위5.0%,검출한위0.53μg/g,정량한위1.77μg/g.
A new method was developed to determinate decabrominated diphenyl ether ( decaBDE) in gas particle samples.The samples were extracted by Soxhlet method to accumulate decaBDE, 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 mL/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 0.53μg/g, and the limit of quality (LOQ) was 1.77 μg/g.