气相色谱法测定鱼油软胶囊中二十碳五烯酸和 二十二碳六烯酸的柱前衍生化方法改进
目的 建立柱前衍生-气相色谱法测定保健食品中二十碳五烯酸(eicosapentaenoic acid, EPA)和二十二碳六烯酸(docosahexaenoic acid, DHA)含量的分析方法。方法 鱼油软胶囊经皂化后用1%的硫酸-甲醇甲酯化, 用气相色谱法测定, FID检测器检测, 色谱柱为DB-FFAP(30 m×0.25 mm, 0.25 ?m), 进样口温度250 ℃, 检测器温度260 ℃, 柱温215 ℃, 直接进样, 外标法定量。结果 EPA和DHA在0.05~5 mg/mL范围内线性良好(rEPA=0.9999, rDHA=0.9999), EPA和DHA的回收率分别为93.1%~102.3%和92.2%~103.9%, EPA和DHA的相对标准偏差均小于3%。结论 该方法操作简便、快捷, 避免了有毒试剂的使用, 定量准确, 重现性好, 适合大批量样品的快速检测。
Objective To establish a rapid method for the determination of the content of eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) in health food by gas chromatography with pre-column derivatization. Methods Fish oil soft capsules were esterified with 1% sulfuric acid-methanol after saponification and then analyzed by gas chromatography coupled with flame ionization detector (FID). This method was performed by direct injection of sample via analytical column, DB-FFAP (30 m×0.25 mm, 0.25 ?m) under injector temperature of 250 ℃, detector temperature of 260 ℃, and column temperature of 215 ℃. The sample was quantified by external standard method. Results Both EPA and DHA had a good linearity in range of 0.05~5 mg/mL (rEPA=0.9999, rDHA=0.9999). The recoveries of EPA and DHA were 93.1%~102.3% and 92.2%~103.9%, respectively, while the relative standard deviations of EPA and DHA were 1.85% and 1.09%, respectively. Conclusions This method is accurate, simple, and high-efficiency in determination of EPA and DHA simultaneously without using toxic reagents. The procedure can be easily transferred to determine EPA and DHA in large number of samples.
标题：气相色谱法测定鱼油软胶囊中二十碳五烯酸和 二十二碳六烯酸的柱前衍生化方法改进
英文标题：Improvement of pre-column derivatization for the determination of eicosapentaenoic acid and docosahexaenoic acid in fish oil soft capsules by gas chromatography
作者：
李硕 中国食品药品检定研究院
李莉 中国食品药品检定研究院
曹进 中国食品药品检定研究院
张庆生 中国食品药品检定研究院
中文关键词:二十碳五烯酸,二十二碳六烯酸,柱前衍生化,气相色谱法,保健食品,
英文关键词:eicosapentaenoic acid,docosahexaenoic acid,pre-column derivatization,gas chromatography,health food,
发表日期：2015-11-12
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