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Improved gas chromatographic method for the determination of the individual free fatty acids in cheese using a capillary column and a PTV injector

机译:改进的气相色谱法,使用毛细管柱和PTV进样器测定奶酪中的各个游离脂肪酸

摘要

A gas chromatographic method with a capillary column and a programmed temperature vaporizer injector has been used to analyze the individual free fatty acids in cheese. The lipids were extracted from an acidified cheese slurry with diethyl ether and treated with tetramethylammonium hydroxide (TMAH) to convert the free fatty acids to tetramethylammonium soaps (TMA-soaps), which were subsequently pyrolyzed to methyl esters in the injector. Carrying out injection at the initial column temperature resulted in lower dispersion of the results, but the solvent front prevented quantitative determination of butyric and caproic acids, and an injector temperature of 300 °C was therefore employed. Under the conditions tested, trimethylamine (tma) flash-off did not affect the determinations. The accuracy of the method improved at higher free fatty acid contents (coefficient of variation of 0.53% for a total free fatty acid content of 9000 mg/kg as opposed to 7.0% for a total free fatty acid. content of 1400 mg/kg). The recovery rate for individual free fatty acids ranged between 91 and 103%.
机译:具有毛细管柱和程序升温蒸发器的气相色谱方法已用于分析奶酪中的各个游离脂肪酸。用二乙醚从酸化的干酪浆中提取脂质,并用四甲基氢氧化铵(TMAH)处理,将游离脂肪酸转化为四甲基铵皂(TMA-soaps),随后在注射器中将其热解为甲酯。在初始柱温下进样会导致结果分散度较低,但是溶剂前沿无法定量测定丁酸和己酸,因此采用了300°C的进样器温度。在测试条件下,三甲胺(tma)闪蒸不影响测定。在较高的游离脂肪酸含量下,该方法的准确性得以提高(总游离脂肪酸含量为9000 mg / kg时变异系数为0.53%,而总游离脂肪酸含量为7.0 mg%时变异系数为1400 mg / kg) 。单个游离脂肪酸的回收率在91%至103%之间。

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