建立了超高效合相色谱?质谱（ UPC2?MS）快速分析6种食用植物油（玉米油、葵花籽油、大豆油、茶油、菜籽油、花生油）中棕榈酸、硬脂酸、油酸、亚油酸、亚麻酸等5种常见脂肪酸的方法，并比较了这6种食用油中上述5种脂肪酸的含量差异。采用皂化反应对植物油进行前处理，以 ACQUITY UPC2 BEH 2?EP 色谱柱（100 mm ×2?1 mm，1?7μm）为分析柱，以超临界CO2?甲醇／乙腈（1∶1， v／v）为流动相进行梯度洗脱，流速为0?8 mL／min。在电喷雾负离子模式下进行检测，外标法定量。结果表明：5种脂肪酸标准物质在0?5～100 mg／L范围内呈现良好的线性关系，相关系数为0?9985～0?9998，定量限（ S／N≥10）为0?15～0?50 mg／L；在3个添加水平下，样品的加标回收率为89?61％～108?50％；方法重复性的相对标准偏差（ RSD）为0?69％～3?01％。该方法简单、快速、分离效果好，无需对脂肪酸样品进行衍生化，已成功地用于玉米油、葵花籽油、橄榄油、茶油、大豆油和花生油等6种食用油中常见脂肪酸含量的测定。
A fast analytical method for five common fatty acids in six edible vegetable oils was developed by ultra?performance convergence chromatography?mass spectrometry (UPC2?MS). The five fatty acids are palmitic acid, stearic acid, oleic acid, linoleic acid and linolenic acid. Their contents in the corn oil, sunflower oil, soybean oil, tea oil, rapeseed oil and peanut oil were compared. The chromatographic separation was performed on an ACQUITY UPC2 BEH 2?EP column (100 mm×2?1 mm, 1?7μm) using the mobile phases of carbon dioxide and metha?nol/acetonitrile (1∶1, v/v) with gradient elution. The separated compounds were detected by negative electrospray ionization ESI-?MS. The results showed that the reasonable linearities were achieved for all the analytes over the range of 0?5-100 mg/L with the correlation coeffi?cients (R2) of 0?998 5-0?999 8. The limits of quantification(S/N≥10)of the five fatty acids were 0?15-0?50 mg/L. The recoveries of the five fatty acids at three spiked levels were in the range of 89?61%-108?50% with relative standard deviations of 0?69%-3?01%. The developed method showed high performance, good resolution and fast analysis for the underivatized fatty acids. It has been successfully used to detect the five fatty acids from corn oil, sunflower oil, soybean oil, tea oil, rapeseed oil and peanut oil.
参考文献
| [1] | 蒋秀琴;刘立成;赵福忠;刘光前;王旭.常见植物油脂肪酸含量的分析[J].饲料博览,2010(3):27-30. |
| [2] | 周文化;郑仕宏;蒋爱民.植物油脂脂肪酸组成及位置分布研究进展[J].粮食与油脂,2011(3):4-6. |
| [3] | 傅宇飞;张佩佩;潘再法;王丽丽.非正常食用油的在线甲基化-气相色谱测定及模式识别分析研究[J].分析试验室,2013(8):103-108. |
| [4] | Lall R K;Proctor A;Jain V P.[J].Journal of the American Oil Chemists'Society,200986:309. |
| [5] | Gomes Reisa M;dos Reis M M;Leath S.[J].J Chroma-togr A,20111218:316. |
| [6] | Ghiaci M;Aghabarari B;Gil A.[J].FUEL,201190(11):3382. |
| [7] | 曾建立;杜泽学;陈艳凤.气相色谱分析未衍生化脂肪酸及其甲酯[J].石油炼制与化工,2012(7):104-110. |
| [8] | 李斌;裘立群;宋少芳;高艾英;张昊.气相色谱法分析植物油中的脂肪酸[J].分析试验室,2014(5):528-532. |
| [9] | 刘冰.GC-MS分析测定5种植物油中脂肪酸成分研究[J].食品工业,2014(4):222-224. |
| [10] | Vaz-Freire L T;da Silva M D R G;Freitas A M C.[J].Analytica Chimica Acta,2009633(02):263. |
| [11] | 孟哲;文大为;廖一平;刘虎威.快速气相色谱法测定食用油中的未衍生化长链脂肪酸[J].色谱,2007(2):254-257. |
| [12] | 李凯欣;陈砺;严宗诚;王红林.麻疯油转酯化产物的高效液相色谱分析[J].分析测试学报,2010(1):39-42. |
| [13] | Se?oráns F J;Iba?ez E.[J].Analytica Chimica Acta,2002465:131. |
| [14] | Francois I;Sandra P.[J].Journal of Chromatography A,20091216:4005. |
| [15] | 梅树莲;黄为民;周统武;庞重军;邹纲明.几种油酸亚油酸的定性定量分析[J].四川理工学院学报（自然科学版）,2005(4):75-78. |
| [16] | 李振宇;傅青;李奎永;梁图;金郁.超临界流体色谱对吴茱萸中吲哚类生物碱的快速分析[J].色谱,2014(5):506-512. |
| [17] | 汤娟;丁友超;曹锡忠;齐琰;钱凯.超高效合相色谱法快速检测纺织品中的8种荧光增白剂[J].色谱,2014(11):1230-1235. |
| [18] | 徐永威;孙庆龙;黄静;谭晓杰.Waters ACQUITY UPC2仪器结构和性能特点[J].现代仪器,2012(5):45-48. |
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