固相微萃取-气相色谱-质谱联用测定人血清中游离脂肪酸

Determination of Free Fatty Acids in Human Serum Using Gas Chromatography-Mass Spectrometry Preceded by Solid-Phase Microextraction

采用甲基丙烯酸丁酯-羟基硅油（BMA／OH—TSO）固相微萃取探头（SPME）与气相色谱-质谱（GC—MS）联用测定人血清中游离脂肪酸的含量．用H2SO4-甲醇对血清中游离脂肪酸进行甲酯化反应，考察了影响探头萃取效率的因素如时间，温度和盐浓度等，优化了衍生化条件．结果表明：该方法检测限低，重现性好，线性范围宽（2～3个数量级），回收率在78．38％～105．1％之间，可用于血清中游离脂肪酸的测定．

A novel solid-phase microextraction （ silicone oil （BMA/OH-TSO） was applied to the SPME） fiber coated with analysis of free fatty aci butyl methacrylate/hydroxy-terminated ds （FFAs） in samples by coupling to gas chromatography-mass spectrometry （GC-MS）. The free fatty acids in human serum were esterified using H2SO4-methanol. Influences of related experimental parameters such as extraction time, temperature, and salt addition were systematically investigated. The derivatization parameters were optimized. Results indicated that this method had satisfactory precision, accuracy, linearity and limits of detection （LODs）. The recovery rates varied from 76.35%-107.0%. This method is suitable for the determination of FFA in human serum.