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作 者:姜文宇[1] 方京冲[1] 史虹莉[1] 朱禧星[1]
机构地区:[1]复旦大学附属华山医院糖尿病研究室,上海200040
出 处:《复旦学报(医学版)》2003年第4期376-378,共3页Fudan University Journal of Medical Sciences
摘 要:目的 建立测定血清中23种脂肪酸组分的气相色谱法(GC)。方法 使用岛津公司GC17A毛细管气相色谱系统,经固相萃取后的脂质用14%BF3甲醇在80℃反应40 min,甲酯化后进样。色谱柱为DB-23石英毛细管柱(30 m×0.25 mm×0.25μm),检测器为氢火焰离子化检测器(FID),采用程序升温同时程序升压技术,初始柱温为140℃,程序升温速度3℃/min,终止温度为234℃;初始柱压为130 kPa,程序升压速度为1 kPa/min,最终压力为163 kPa。结果 16:0的最低检测限为3.6×10-11g;18:0、18:1n9c的最低检测限为2.4×10-11g。脂肪酸组分的线性范围为3.2~600 ng/μL(r>0.99)。方法回收率良好(84.40%~104.12%)。各种脂肪酸的天内精密度为0.25%~9.82%(n=5),天间精密度为0.47%~9.88%(n=5)。结论 本方法专一、灵敏、准确,可用于临床脂肪酸血清浓度的监测。Purpose: To establish a gas chromatography (GC) method for the determination of 23 fatty acids in serum. Methods: The extracted lipids were methylesterized by 14% BF3 at 80 °C for 40 min, then separated and measured by GC17A Shimadzu system equipped with a DB - 23 (30 m × 0. 25 mm × 0.25 μm) glass capillary column and a flame ionization detector, with nitrogen as the carrier gas. A temperature program accompanied by pressure program was designed, that is, column temperature raised from 140 °C to 234 °C (rate: 3 °C/min), meanwhile, column pressure raised from 130 kPa to 163 kPa (rate:1 kPa/min). Results: The limit of detection of 16:0, 18:0 and 18:1n9c were 3.6 × 10-11g, 2.4 × 10 -11g, 2.4 × 10-11g, respectively. In the range from 3.2 to 600 ng/μL, there was a linear relationship between the areas and concentrations (r>0.990). The method recovery was good (84.40%-104.12%), and the within-day RSD and between-day RSD were less than 10%. Conclusions: This method proved to be specific, sensitive and reproducible, and applicable for the determination of fatty acid composition in serum.
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