Zhao Guohua, Liu Jing-Fu, Nyman Margareta, Jönsson Jan Ake
Food College of Southwest University, Beibei 400715, Chongqing, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Feb 1;846(1-2):202-8. doi: 10.1016/j.jchromb.2006.09.027. Epub 2006 Oct 27.
A method based on hollow fiber supported liquid membrane extraction coupled with a gas chromatograph equipped with flame ionization detector (GC-FID) was developed for the determination of six short-chain fatty acids including acetic acid, propionic acid, i-butyric acid, n-butyric acid, i-valeric acid and n-valeric acid in serum. Hollow fiber supported liquid membrane extraction was employed for preconcentration and clean-up of the samples. The fatty acids were extracted from the acidic donor (diluted serum) into a liquid membrane formed in the wall of the hollow fiber with 10% tri-n-octylphoshphine oxide (TOPO) in di-n-hexyl ether, and then extracted back into a basic acceptor solution filled in the lumen of the hollow fiber. After being acidified with HCl, the acceptor was directly analyzed by GC-FID. The acceptor concentration, donor pH, membrane liquid and extracting time were optimized giving an enrichment factor up to 155 times. The good linearity (r(2)>0.980), reasonable recovery (87.2-121%), and satisfactory intra-assay (8.2-11.5%) and inter-assay (6.1-11.6%) precision illustrated the good performance of the present method. Limits of detection (LOD) ranged from 0.04 to 0.24 microM and limits of quantification (LOQ) varied from 0.13 to 0.80 microM.
建立了一种基于中空纤维支撑液膜萃取结合配有火焰离子化检测器的气相色谱仪(GC-FID)的方法,用于测定血清中的六种短链脂肪酸,包括乙酸、丙酸、异丁酸、正丁酸、异戊酸和正戊酸。采用中空纤维支撑液膜萃取对样品进行预浓缩和净化。脂肪酸从酸性供体(稀释血清)中萃取到由二正己醚中10%三正辛基氧化膦(TOPO)在中空纤维壁上形成的液膜中,然后再萃取回到填充在中空纤维内腔的碱性接受液中。用盐酸酸化后,接受液直接用GC-FID分析。对接受液浓度、供体pH值、膜液和萃取时间进行了优化,富集倍数高达155倍。良好的线性(r(2)>0.980)、合理的回收率(87.2-121%)以及令人满意的批内精密度(8.2-11.5%)和批间精密度(6.1-11.6%)表明了本方法的良好性能。检测限(LOD)范围为0.04至0.24 microM,定量限(LOQ)在0.13至0.80 microM之间变化。