摘要
采用新型荧光标记试剂10-乙基吖啶酮-2-磺酰氯(EASC)作为柱前衍生试剂,在Hypersil BDS C18反相色谱柱上(4.6mm×200mm,10μmi.d.),采用梯度洗脱在20min内实现了12种EASC-脂肪胺衍生物的快速基线分离.最佳检测波长为λex/λem=270nm/430nm.EASC与常用的Dansyl-Cl相比具有更强的光致发光特性(紫外和荧光):紫外吸收强度之比为3.2:1,相对荧光强度之比为30.0:1—105.4:1,荧光量子效率之比为43.0:1.通过荧光检测及离子阱大气压化学电离源的正离子模式获得了胺类组分的准确定量和相应的柱后质谱鉴定.质谱灵敏度之比为1.6:1~6.2:1.建立的方法对环境水样中脂肪胺类化合物的测定具有快速、准确和重现性良好等优点,回归系数大于0.9995,检出限为4.0-12.7fmol.
On a reversed-phase Hypersil BDS C18 (4.6 mm × 200 mm, 10 μm i. d. ) column, 12 aliphatic amines were derivatized using 10-ethyl-9-oxo-9,10-dihydroacridine-2-sulfonyl chloride (EASC) as a new precolumn derivatization reagent. The complete baseline resolution was obtained in conjunction with a gradient elution with acetonitrile/H2O as mobile phase within 20 min. The optimum excitation and emission wavelengths were at λex/λem = 270 nm/430 nm. Comparing with the widely used Dansyl-Cl, EASC has stronger photoluminescence characteristics( ultraviolet and fluorescence) : UVEASC/UVDansyl-Cl = 3.2 (UV: ultraviolet absorption intensity) ; I ( EASC )/I (Dansyl-Cl) = 30. 0 : 1-105.4 : 1 ( I: relative fluorescence intensity) ; fluorescence quantum yield : Фf ( EASC)/Фf (Dansyl-Cl) = 43.0 : 1. Fast and accurate quantitative analysis of aliphatic amines with fluorescence and corresponding post-column ion trap mass spectrometry(LC-APCI-MS) were obtained. EASC-amines exhibited stronger mass spectrometric sensitivity relative to that of dansyl-amine derivatives: MSEASC/MSDansyl-Cl = 1.6: 1-6. 2:1 times( MS: relative intensity of ion current). The established method for the determination of aliphatic amines in environmental water samples exhibited good reproducibility and recovery. Excellent linear responses were observed with the correlation coefficients 〉 0. 9995. The detection limits(at signal-to-noise of 3:1 ) were at levels of 4.0-12.7 fmol.
出处
《高等学校化学学报》
SCIE
EI
CAS
CSCD
北大核心
2009年第4期675-681,共7页
Chemical Journal of Chinese Universities
基金
国家自然科学基金(批准号:20075016)
中国科学院百人计划项目(批准号:328)资助
关键词
高效液相色谱-离子阱质谱
荧光检测
柱前衍生
10-乙基吖啶酮-2-磺酰氯
脂肪胺
High performance liquid chromatography/ion-trap mass spectrometry
Fluorescence detection
Pre-column derivatization
10-ethyl-9-oxo-9,10-dihydroacridine-2-sulfonyl chloride
Aliphatic amine