色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
12期
1385-1389
,共5页
牟瑶%韦思平%徐敏%陈平%王钦%杜曦
牟瑤%韋思平%徐敏%陳平%王欽%杜晞
모요%위사평%서민%진평%왕흠%두희
气相色谱-质谱/选择离子监测%苯乙烯%环氧苯乙烷对映异构体%正交试验
氣相色譜-質譜/選擇離子鑑測%苯乙烯%環氧苯乙烷對映異構體%正交試驗
기상색보-질보/선택리자감측%분을희%배양분을완대영이구체%정교시험
gas chromatography-mass spectrometry/selected ion monitoring(GC-MS/SIM)%styrene%styrene oxide enantiomers%orthogonal experiment
建立了苯乙烯不对称环氧化反应的气相色谱-质谱/选择离子监测(GC-MS/SIM)筛选方法。以乙苯为内标,利用 GC-MS/SIM对苯乙烯环氧化反应样品进行分析,在选定的分析条件下完全分离并准确测定了苯乙烯和环氧苯乙烷对映异构体的含量,同时利用该方法对苯乙烯环氧化反应的正交试验进行了评估。该方法具有以下优点:高精密度(以 RSD表示的精密度为1.2%~5.2%,n=5)、良好的线性关系(苯乙烯、( R)-环氧苯乙烷和( S)-环氧苯乙烷标准曲线的相关系数分别为0.9997、0.9932和0.9963)、低定量限(苯乙烯、( R)-环氧苯乙烷和( S)-环氧苯乙烷的定量限分别为1.3、1.1和0.7 mg/L)以及合理的回收率(98.2%~108.2%)。该方法为苯乙烯及其同系物的不对称环氧化反应提供了一种新的分析测定途径。
建立瞭苯乙烯不對稱環氧化反應的氣相色譜-質譜/選擇離子鑑測(GC-MS/SIM)篩選方法。以乙苯為內標,利用 GC-MS/SIM對苯乙烯環氧化反應樣品進行分析,在選定的分析條件下完全分離併準確測定瞭苯乙烯和環氧苯乙烷對映異構體的含量,同時利用該方法對苯乙烯環氧化反應的正交試驗進行瞭評估。該方法具有以下優點:高精密度(以 RSD錶示的精密度為1.2%~5.2%,n=5)、良好的線性關繫(苯乙烯、( R)-環氧苯乙烷和( S)-環氧苯乙烷標準麯線的相關繫數分彆為0.9997、0.9932和0.9963)、低定量限(苯乙烯、( R)-環氧苯乙烷和( S)-環氧苯乙烷的定量限分彆為1.3、1.1和0.7 mg/L)以及閤理的迴收率(98.2%~108.2%)。該方法為苯乙烯及其同繫物的不對稱環氧化反應提供瞭一種新的分析測定途徑。
건립료분을희불대칭배양화반응적기상색보-질보/선택리자감측(GC-MS/SIM)사선방법。이을분위내표,이용 GC-MS/SIM대분을희배양화반응양품진행분석,재선정적분석조건하완전분리병준학측정료분을희화배양분을완대영이구체적함량,동시이용해방법대분을희배양화반응적정교시험진행료평고。해방법구유이하우점:고정밀도(이 RSD표시적정밀도위1.2%~5.2%,n=5)、량호적선성관계(분을희、( R)-배양분을완화( S)-배양분을완표준곡선적상관계수분별위0.9997、0.9932화0.9963)、저정량한(분을희、( R)-배양분을완화( S)-배양분을완적정량한분별위1.3、1.1화0.7 mg/L)이급합리적회수솔(98.2%~108.2%)。해방법위분을희급기동계물적불대칭배양화반응제공료일충신적분석측정도경。
A screening method by gas chromatography-mass spectrometry( GC-MS)with selected ion monito-ring( SIM)has been developed for asymmetric epoxidation of styrene. All samples were analyzed by GC-MS with the mode of SIM by using ethylbenzene as the internal standard,by which styrene and styrene epoxide enantiomers were completely separated and their concentrations were accurately determined. Furthermore,this method was used to evaluate the epoxidation reaction of styrene,which was optimized by orthogonal experi-ment. The advantages of the method are as follows:excellent precision( RSD in the range of 1. 2%-5. 2%,n=5),good linearity( the correlation coefficients for styrene,( R)/( S)-styrene oxide were 0. 999 7,0. 993 2 and 0. 996 3,respectively),low limits of quantitation( LOQs of styrene,( R)/( S)-styrene oxide were 1. 3,1. 1 and 0. 7 mg/L,respectively)and reasonable recoveries( 98. 2%-108. 2%). All in all,the method provided a new way to determine the asymmetric epoxidation mixture of styrene and its homologs.