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柱前衍生-反相高效液相色谱荧光测定及质谱鉴定土壤和苔藓中的脂肪酸
Pre-column Derivatization - HPLC Determination of Free Fatty Acids in Soil and Bryophyte with Fluorescence Detection and Mass Spectrometric Identification
查看参考文献8篇
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文摘
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合成新型荧光衍生试剂1-[2-(对甲苯磺酸酯)乙基]-2-苯基咪唑[4，5．f]9，10-菲(TSEPIP)，将其作为柱前衍生化试剂，在Eclipse XDB-Cs色谱柱上，采用梯度洗脱实现了30种游离脂肪酸(FFA)衍生物的基线分离。利用柱后在线的串联质潜以APCI大气压化学电离源正离子模式实现了各组分的质谱定性。对土壤与两种苔藓(狭叶绢藓、曲尾藓)中FFA组分的定量结果表明，苔藓植物从土壤中富集了大量的游离脂肪酸。荧光检测的激发和发射波长分别为λ_(ex)=260 mn，λ_(em)=380 nm。绝大多数脂肪酸的线性回归系数大于0．9993，检出限为3．2～37 fmol。建立的方法具有良好的重复性，对实际样品测定结果满意。 |
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其他语种文摘
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A simple and sensitive method for the determination of free fatty acids using pre-column derivatization - reversed phase HPLC with fluorescence detection and mass spectrometric identification was developed. 1-[2-(p-toluenesulfonate) ethyl]-2-phenylimrdazole [4,5-f] 9,10-phenanthrene (TSEPIP) was synthesized and used as the pre-column derivatization reagent. Experimental results showed that free fatty acids could react rapidly with TSEPIP in the presence of K_2CO_3 catalyst at 90 t in DMF solvent. Free fatty acid derivatives were separated on Eclipse XDB-C_8 column with a good baseline resolution. The identifications of 30 fatty acid derivatives were carried out by post-column in tandem mass spectrometer with atmospheric pressure chemical ionization (APCI) source. The contents of 30 free fatty acids in soil and two kinds of bryophytes (Entodon macropodus, Dicranum caesium) were determined. The results indicated that the biyophyte plants enriched an abundance of free fatty acids from soil. The fluorescence excitation arid emission wavelengths of derivatives were set at Ara = 260 nm and λ_(em) = 380 nm, respectively. The correlation coefficients for most fatty acid derivatives were > 0.9993, and the detection limit range (at signal-to-noise of 3:1) was 3.2-37 fmol. The method has been applied to the determination of free fatty acids in real samples with satisfactory results. |
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来源
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分析测试学报
,2006,25(5):1-6 【核心库】
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关键词
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高效液相色谱-质谱
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荧光检测
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柱前衍生
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脂肪酸
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地址
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1.
中国科学院西北高原生物研究所, 青海, 西宁, 810001
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曲阜师范大学化学科学学院, 山东, 曲阜, 273165
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语种
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中文 |
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文献类型
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研究性论文 |
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ISSN
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1004-4957 |
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学科
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化学 |
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基金
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国家自然科学基金资助项目
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文献收藏号
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CSCD:2431163
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参考文献 共
8
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