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土壤和苔藓植物中游离脂肪酸的高效液相色谱荧光测定及质谱鉴定

Determination of Free Fatty Acids from Soil and Bryophyte by High-performance Liquid Chromatography Mass Spectrum (HPLC/MS) with Fluorescence Detection

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【作者】 石运伟明永飞赵先恩白敏程燕尤进茂

【Author】 SHI Yun-wei~①, MING Yong-fei~②, ZHAO Xian-en~①, BAI Min~①, CHENG Yan~①, YOU Jin-mao~① (①Department of Chemistry, Qufu Normal University, 273165,Qufu,Shandong; ②Lanzhou Institute of Chemical Physics ,Chinese Academy of Science,730000,Lanzhou,Ganshu,PRC)

【机构】 曲阜师范大学化学科学学院兰州化学物理研究所曲阜师范大学化学科学学院 273165山东省曲阜市730000甘肃省兰州市273165山东省曲阜市

【摘要】 合成了新型荧光试剂 1,23,4氢咔唑9基对甲苯磺酸酯 ,以此作为柱前衍生化试剂对19种游离脂肪酸 (FFA)进行了优化衍生 .在EclipseXDB -C8色谱柱上 ,采用梯度洗脱对 19种游离脂肪酸(FFA)衍生物进行了完全基线分离及定量分析 .荧光检测激发和发射波长分别为λex=333nm ,λem=390nm .多数脂肪酸的线性回归系数大于 0 .9989,检测限在 2 4 .8~ 80 .37fmol.采用APCI大气压化学电离源的正离子模式 ,实现了土壤和苔藓中FFA组分的定性 .方法具有稳定良好的重现性 ,对实际样品测定结果满意 .

【Abstract】 A novel fluorescence reagent 1,2-benzo-3,4-dihydrocarbazole-9-ethyl-toluene-4-sulfonate (BDBETS) was synthesized, and using which as pre-column derivatization reagent ,19 fatty acids were derivatized optimally. On a reversed-phased Eclipse XDB-C8 column, 19 fatty acid derivatives were separated at baseline and analysized quantificationally. Fluorescent detection excitation and emission wavelengths were set at λex 333 nm, λem390 nm, respectively. Correlation coefficients for fatty acid derivatives are >0.9989, and detection limits (at signal-to-noise of 3∶1) are 24.8~(80.37) fmol. Qualificative analysis of free fatty acids from soil and bryophyte samples was obtained on the basis of APCI source at positive model detection. The established method is sensitive and reproducible for the determination of free fatty acids from real samples with satisfactory results.

【基金】 国家自然科学基金资助项目 (2 0 0 75 0 16)
  • 【文献出处】 曲阜师范大学学报(自然科学版) ,Journal of Qufu Normal University(Natural Science) , 编辑部邮箱 ,2005年01期
  • 【分类号】O657.7;O657.3;O657
  • 【被引频次】9
  • 【下载频次】265
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