气相色谱法同时检测南极磷虾中2种ω-3脂肪酸含量

Simultaneous determination of 2 kinds of ω-3 fatty acids in Euphausia superba by gas chromatography

中文关键词:  南极磷虾  二十碳五烯酸  二十二碳六烯酸  气相色谱法  酯化

英文关键词:Euphausia superba  eicosapentaenoic acid  docosahexaenoic acid  gas chromatography  esterification

中文摘要:

      目的 建立甲酯化-气相色谱法同时检测南极磷虾中二十碳五烯酸(eicosapentaenoic acid, EPA)和二十二碳六烯酸(docosahexaenoic acid, DHA)含量的分析方法。方法 样品经二氯甲烷提取后, 与0.5%硫酸-甲醇溶液在60 ℃条件下反应30 min, 反应液使用硅酸镁柱层析净化。将洗脱液转移至15 mL离心管中, 2000 r/min离心20 min, 上清液氮吹浓缩后, 用乙腈定容至1 mL, 使用DB-1701色谱柱(30 m×0.32 mm, 1.00 μm)分离, 火焰离子化检测器检测, 外标法定量。结果 方法在0.02~2.00 mg/mL的线性范围内, 相关系数为0.9999。平行样品的相对标准偏差不超过6% (n=3), 平均回收率大于82.6%。结论 该方法简便高效、检出限低、重现性好, 可用于新鲜和干燥南极磷虾样品中EPA和DHA的检测。

英文摘要:

      Objective To establish an analytical method for the simultaneous determination of eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) in Euphausia superba by methyl esterification-gas chromatography. Methods The samples were extracted with dichloromethane, and reacted with 0.5% sulfuric acid-methanol solution at 60 ℃ for 30 min, the reaction solution was purified by magnesium silicate column chromatography. Subsequently, the eluate was transferred to a 15 mL centrifuge tube, and centrifuged at 2000 r/min for 20 min, the upper solution was concentrated by blowing nitrogen, and the solution was diluted with acetonitrile to a final volume of 1 mL, then, the obtained sample was separated using a DB-1701 chromatographic column (30 m×0.32 mm, 1.00 μm), and then detected by a flame ionization detector, and quantified by an external standard method. Results The method had good linear correlations within the concentration range of 0.02-2.00 mg/mL with correlation coefficients were 0.9999. The relative standard deviations of parallel samples were no more than 6% (n=3), and the average recoveries were greater than 82.6%. Conclusion This method is simple and efficient, with low detection limit and good reproducibility, it can be suitable for the determination of EPA and DHA in fresh and freeze-dried Euphausia superb samples.