分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2009年
11期
1627-1632
,共6页
海洋沉积物%多溴联苯醚%超声萃取%气相色谱-质谱联用
海洋沉積物%多溴聯苯醚%超聲萃取%氣相色譜-質譜聯用
해양침적물%다추련분미%초성췌취%기상색보-질보련용
Coastal sediments%polybrominated diphenyl ethers%ultrasonic extraction%gas chromatography/ mass spectrometry
建立了超声萃取-气相色谱-质谱法测定海洋沉积物中39种多溴联苯醚残留的分析方法.样品用V(正己烷):V(二氯甲烷) =1:1混合溶液提取,超声(控制水浴温度为25 ℃)提取60 min,采用硅胶和氧化铝净化,负化学离子源-气相色谱-质谱法进行检测,39种组分图谱在49 min 内能得到很好的分离. 39种混合样品的检出限为0.003～0.10 μg/kg; 加标回收率为66.2%～118.6%;相对标准偏差为0.8%～18.2%.用于实际样品分析,结果令人满意.
建立瞭超聲萃取-氣相色譜-質譜法測定海洋沉積物中39種多溴聯苯醚殘留的分析方法.樣品用V(正己烷):V(二氯甲烷) =1:1混閤溶液提取,超聲(控製水浴溫度為25 ℃)提取60 min,採用硅膠和氧化鋁淨化,負化學離子源-氣相色譜-質譜法進行檢測,39種組分圖譜在49 min 內能得到很好的分離. 39種混閤樣品的檢齣限為0.003～0.10 μg/kg; 加標迴收率為66.2%～118.6%;相對標準偏差為0.8%～18.2%.用于實際樣品分析,結果令人滿意.
건립료초성췌취-기상색보-질보법측정해양침적물중39충다추련분미잔류적분석방법.양품용V(정기완):V(이록갑완) =1:1혼합용액제취,초성(공제수욕온도위25 ℃)제취60 min,채용규효화양화려정화,부화학리자원-기상색보-질보법진행검측,39충조분도보재49 min 내능득도흔호적분리. 39충혼합양품적검출한위0.003～0.10 μg/kg; 가표회수솔위66.2%～118.6%;상대표준편차위0.8%～18.2%.용우실제양품분석,결과령인만의.
A method was developed for the determination of 39 polybrominated diphenyl ethers(PBDEs) from mono- to hepta-brominated in coastal sediment by gas chromatography/mass spectrometry. The sample was extracted with a solution of dichloromethane: n-hexane( 1:1,V/V) ,followed by ultrasonic extraction for 60 min at 25℃. The clean-up step was optimized using silica gel and alumina. The detection limit of the method was in the range of 0.003 - 0.10μg/kg. The results indicate that the average recovery of the internal standard was from 66.2% to 118. 6%. The relative standard deviation RSD( % ) was from 0. 8 % to 18. 2%. The method for the detection of 39 PBDE congeners in coastal sediment was sensitive,high reproducible with satisfactory recoveries.
