毛细管气相色谱内标法测定沙棘油中的脂肪酸  

Determination of Fatty Acids in Sea-buckthorn Oil with Capillary Gas Chromatography by Using Internal Standard Method

作　　者：张凤枰[1] 索有瑞[2] 王洪伦[2] 赵先恩[2] 涂杰[1] 张蓉健[1] 

机构地区：[1]国家粮食储备局成都粮食储藏科学研究所,成都610031 [2]中国科学院西北高原生物研究所,西宁810001

出　　处：《中国粮油学报》2008年第1期198-202,共5页Journal of the Chinese Cereals and Oils Association

摘　　要：建立了以十七烷酸甲酯为内标物，用毛细管气相色谱同时测定沙棘油中六种脂肪酸（棕榈酸、棕榈油酸、硬脂酸、油酸、亚油酸、亚麻酸）的方法。样品经氢氧化钾-甲醇皂化、三氟化硼-甲醇酯化后使生成相应的脂肪酸甲酯，以DM—FFAP毛细管柱分离，火焰离子化检测器测定。用保留时间定性，内标法定量。结果表明，在所选择的色谱条件下，上述脂肪酸在10min内获得较好的分离；六种脂肪酸的峰面积与其质量浓度有良好的线性关系，相关系数均大于0．9998；样品加标回收率（n=6）为92．1％～101．4％；相对标准偏差为2．37％～4．19％；最低检出限为4．0mg／L。该方法操作简便、快速、准确，适合批量样品的测定。A capillary gas chromatographic method for the simultaneous determination of six fatty acids （palmitic acid, palmitoleic acid, stearic acid, oleic acid, linoleic acid and linolenic acid） in sea- buckthom oil was developed and heptadecanoic acid methyl ester was selected as the internal standard substance. The developed procedure is as follows： The sample is firstly saponified with KOH - CH3OH and then the fatty acids are methylated with BF3 - CH3OH, and the obtained fatty acid methyl esters are detected by gas chromatography using a DM - FFAP capillary column and a flame ionization detector. The retention time of the peak is applied for qualitative analysis, and the internal standard method is used for quantitative analysis. The six fatty acid esters are well separated through DM - FFAP capillary column （30m× 0.32mm i.d. x 0.25μm） within 10 min. The recoveries for the spiked standards and the relative standard deviations are 92.1% - 101.4% and 2.37% - 4.19%, respectively. The detection limit （s/n = 3） is 4.0 mg/L. The method is simple, fast and accurate for the fatty acid determination of batches of sample.

关 键 词：毛细管气相色谱 内标法 脂肪酸 沙棘油 

分 类 号：TS21[轻工技术与工程—粮食、油脂及植物蛋白工程]