分析试验室
分析試驗室
분석시험실
ANALYTICAL LABORATORY
2010年
1期
99-102
,共4页
周黎明%周建梅%卢彩虹%鲁胜利%李青松%刘波
週黎明%週建梅%盧綵虹%魯勝利%李青鬆%劉波
주려명%주건매%로채홍%로성리%리청송%류파
固相微萃取%气相色谱-质谱法%三苯胂%二苯胂酸%衍生化
固相微萃取%氣相色譜-質譜法%三苯胂%二苯胂痠%衍生化
고상미췌취%기상색보-질보법%삼분신%이분신산%연생화
Solid-phase microextraction%Gas chromatography-mass spectrometry with selective ion monitoring%Triphenylarsine%Diphenylarsinic acid%Derivatization
建立了一种同时测定水中痕量三苯胂和二苯胂酸的方法, 使用巯基乙酸甲酯作为二苯胂酸测定的衍生化试剂, 固相微萃取耦合气相色谱-质谱法(选择离子监测)同时测定三苯胂和二苯胂酸. 优化了萃取纤维丝、萃取时间、衍生化等操作条件. 同时对混合物测定的回收率、相对标准偏差和最低检测限进行了研究. 方法的回收率大于95%, 最低检测质量浓度分别为0.0005和0.0003 mg/L, 6次测定的相对标准偏差分别为5.3%、 7.6%.
建立瞭一種同時測定水中痕量三苯胂和二苯胂痠的方法, 使用巰基乙痠甲酯作為二苯胂痠測定的衍生化試劑, 固相微萃取耦閤氣相色譜-質譜法(選擇離子鑑測)同時測定三苯胂和二苯胂痠. 優化瞭萃取纖維絲、萃取時間、衍生化等操作條件. 同時對混閤物測定的迴收率、相對標準偏差和最低檢測限進行瞭研究. 方法的迴收率大于95%, 最低檢測質量濃度分彆為0.0005和0.0003 mg/L, 6次測定的相對標準偏差分彆為5.3%、 7.6%.
건립료일충동시측정수중흔량삼분신화이분신산적방법, 사용구기을산갑지작위이분신산측정적연생화시제, 고상미췌취우합기상색보-질보법(선택리자감측)동시측정삼분신화이분신산. 우화료췌취섬유사、췌취시간、연생화등조작조건. 동시대혼합물측정적회수솔、상대표준편차화최저검측한진행료연구. 방법적회수솔대우95%, 최저검측질량농도분별위0.0005화0.0003 mg/L, 6차측정적상대표준편차분별위5.3%、 7.6%.
A new method of derivatization solid-phase microextraction (SPME) coupled with gas chromatography-mass spectrometry (GC-MS) for the determination of triphenylarsine (TPA) and diphenylarsinic acid (DPAA) in water has been developed. Using 100 μm polydimethylsiloxane (PDMS) fibers, the influence of several parameters on the SPME and derivatization procedure such as the extraction time of the fiber in the aqueous sample, derivatization time and temperature, the desorption time and temperature, pH value have been studied. The lowes detection concentration is 0.0005 mg/L and 0.0003 mg/L respectively. The spiked recoveries are larger than 95%. The relative standard deviations for 6 runs are 5.3% and 7.6% respectively.