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深海鱼油中脂肪酸的柱前衍生-高效液相色谱串联质谱分析
Pre-column Derivatization High-Performance Liquid Chromatography Tandem Mass Spectrometry Determination of Fatty Acids from Deep-sea Fish Oil

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文摘 用1-[2-(对甲苯磺酸酯)乙基]-2-苯基咪唑[4,5-f]9,10-菲(TSEPIP)作为柱前荧光衍生试剂,在Eclipse XDBC8(4.6×150 mm,5μm,Agilent)反相色谱柱上,采用梯度洗脱在检测波长为380nm(激发波长为260nm)的条件下,实现了阿拉斯加深海鱼油中饱和脂肪酸含量的外标法定量测定.26种饱和脂肪酸的线性范围是200.0pmol~48.83fmol,线性相关系数均大于0.9996,检测限为3.824~47.13 fmol(信噪比为3:1测得,S/N 3:1).经柱后串联质谱大气压化学电离源(APCI)正离子模式实现了各种饱和与不饱和脂肪酸衍生物的质谱鉴定,进而通过峰面积归一化法得出了所有饱和与不饱和脂肪酸的相对含量.结果表明,深海鱼油主要含有C_(12)~C_(22)的脂肪酸,共鉴定出25种脂肪酸,其中不饱和脂肪酸含量占69.71%(峰面积百分比,下同),特别是具有重要生理作用的多不饱和脂肪酸,如C_(20:5)5,8,11,14,17-二十碳五烯酸(5,8,11,14,17-eicosapentaenoic acid,EPA,16.62%),C_(22:6):2,5,8,11,14,17-二十二碳六烯酸(2,5,8,11,14,17-docosahexenoic acid,DHA,12.31%).
其他语种文摘 A simple and sensitive method for the determination of fatty acids in Alaska deep-sea fish oil using 1-[2-(p-toluenesulfonate)-ethyl]-2-phenylimidazole-[4,5-f]-9,10-phenanthrene (TSEPIP) as derivatization reagent on a reversed phase Eclipse XDB-C_8 (4.6 150mm,5 m,Agilent) column in conjunction with a gradient elution followed by reversed phase high-performance liquid chromatography with fluorescence detection at 380 nm(excitation wavelength 260 nm) and tandem mass spectrometric identification has been developed. The contents of 26 free fatty acids in deep-sea fish oil were determined by external standard method, and the linear range of them was 200.0 pmol~48.83 fmol, all the correlation coefficients >0.9996, detection limits were 3.824~47.13 fmol (at signal to noise 3:1, S/N 3:1). The identification of all saturated and unsaturated fatty acid derivatives was carried out by post-column tandem mass spectrometry with atmospheric pressure chemical ionization (APCI) source in positive-ion mode, and the relative content of all saturated and unsaturated fatty acids was contrasted by peak area. According to the analysis of HPLC/MS/APCI, 25 fatty acids were identified, the main fatty acids in deep-sea fish oil are C_(12)~C_(22) and 69.71% (peak area percent) of them are unsaturated fatty acids, especially polyunsaturated fatty acids which have important physiological function, such as 5, 8, 11, 14, 17-eicosapentaenoic acid(EPA,16.62 %), 2, 5, 8, 11, 14, 17-docosahexenoic acid (DHA, 12.31 %).
来源 食品科学 ,2007,28(8):358-362 【核心库】
关键词 阿拉斯加深海鱼油 ; 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 1002-6630
学科 化学
基金 国家自然科学基金 ;  青海省科技攻关重点项目
文献收藏号 CSCD:2908889

参考文献 共 9 共1页

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7.  赵先恩. 荧光衍生试剂1-[2-(对甲苯磺酸醋)乙基]2-苯基咪唑[4,5-f]9,10-菲的合成及其在长链脂肪酸分析中的应用. 色谱,2006,24(5):456-461 被引 6    
8.  SIMONETTAA F. A method to assessg enomic DNA methylation using high-performance liquid chromatography/electrospray ionization mass spectrometry. Anal Chem,2002,74:4526-4531 被引 1    
9.  邹耀洪. 2-氨基-2-甲基丙醇衍生气相色谱/质谱分析深海鱼油脂肪酸. 分析化学,2004,32(1):71-75 被引 7    
引证文献 5

1 谢瑶 高效液相色谱及液相色谱-质谱联用技术在保健食品检测中的应用 化学通报,2010,73(8):684-688
被引 2

2 董宏祯 微生物油脂中花生四烯酸的气相色谱定量检测 中国油脂,2011,36(9):78-81
被引 0 次

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