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辛酸TSEPIP荧光衍生物制备及荧光光谱研究与分析应用
Preparation of caprylic TSEPIP derivative and its fluorescence spectra study and application for HPLC analysis

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文摘 合成了荧光衍生试剂1-[2-(对甲苯磺酸酯)乙基]-2-苯基咪唑[4,5-f]9,10-菲(TSEPIP),经衍生化和固相萃取制得了TSEPIP的辛酸衍生物(TSEPIP-C_8).研究了TSEPIP-C_8在包括溶剂极性、温度、卤素离子、重金属离子等不同的溶液环境因素影响下的荧光光谱性质,为高效液相色谱荧光分析检测提供了依据.在Eclipse XDB-C_8反相色谱柱上,在380 nm检测波长下采用梯度洗脱,实现了26种脂肪酸(FFA)TSEPIP衍生物的基线分离,应用该法完成了丹参中脂肪酸的含量分析.借助柱后串联质谱APCI大气压化学电离源正离子模式,能够实现各组分的快速定性.26种脂肪酸的线性回归系数均 》0.999 6,检出限为3.824~47.13 fmol(进样量10 μL,信噪比为3:1).
其他语种文摘 TSEPIP-C_8 derivative was prepared based on the derivatization of caprylic(C_8) acid using 1-[2-(p-toluenesulfonate)ethyl]-2-phenylimidazole[4,5-f]9,10-phenanthrene(TSEPIP) as the derivatization reagent by pre-column derivatization and solid phase extraction(SPE).Fluorescence spectra properties of TSEPIP-C_8,at different solvent polarity,temperature and in the presence of different halide salts and heavy metal atoms,were studied on fluorescence spectrophotometer,which provided dependence for HPLC analysis with fluorescence detection.Separation of 26 types of derivatized fatty acids(C_1-C_(26)) was carried out at the detection wavelength 380 nm with a good baseline resolution in conjunction with a gradient elution on a reversed-phase Eclipse XDB-C_8 column.By this procedure,the contents of free fatty acids in Salvia miltiorrhiza B.were determined.The simple and convenient identification of fatty acid derivatives was carried out by post-column tandem mass spectrometry with atmospheric-pressure chemical ionization(APCI) source in a positive ion mode.Excellent linear responses were observed with correlation coefficients >0.999 6,and the detection limits were 3.824~47.13 fmol(injection volume 10 μL,at signal-to-noise of 3:1).
来源 化学试剂 ,2007,29(11):658-662,672 【核心库】
关键词 荧光衍生试剂 ; 荧光光谱 ; 高效液相色谱-质谱 ; 柱前衍生 ; 荧光检测 ; 脂肪酸
地址

中国科学院,西北高原生物研究所, 青海, 西宁, 810001

语种 中文
文献类型 研究性论文
ISSN 0258-3283
学科 化学
基金 中国科学院“百人计划”项目
文献收藏号 CSCD:3004734

参考文献 共 10 共1页

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引证文献 1

1 罗晓燕 多臂萘酰亚胺树枝分子的合成和荧光性质 有机化学,2013,33(11):2423-2429
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王小艳 0000-0003-2691-9851
索有瑞 0000-0002-1535-6531
刘永军 0000-0002-1686-8272
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