高通量测定油脂及其制品中5种抗氧化剂的超高效合相色谱方法  

High-throughput determination of 5 kinds antioxidants from oils and their products by ultra-performance convergence chromatography

作　　者：王波 高黎红 陆秀云[3] 冯静 金凤 周围[1,3,2] WANG Bo GAO Li-hong LU Xiu-yun FENG Jing JIN Feng ZHOU Wei(Central Laboratory of Technical Center of Causu Entry-Exit Inspection and Quarantine Bureau, Lauzhou 730000 College of geography and Environmental Science, Northwest Normal University, Lanzhou 730070 Industry research and Analysis Laboratory of Olive oil , Longnan 746000)

机构地区：[1]甘肃出入境检验检疫局综合技术中心,兰州730000 [2]祥宇油橄榄产业研发及分析实验室,陇南746000 [3]西北师范大学地理与环境科学学院,兰州730070

出　　处：《分析试验室》2017年第7期831-836,共6页Chinese Journal of Analysis Laboratory

摘　　要：建立了超高效合相色谱(UPC^2)分离和测定油脂及其制品中5种脂溶性抗氧化剂的方法。样品经乙腈提取,浓缩过滤后直接进样分析;流动相以CO_2为主体,0.1%甲酸甲醇溶液为助溶剂;色谱柱Acquity UPC^2HSS C_(18) SB 3.0 mm×100 mm,1.8μm,流速1.5 mL/min,检测波长为280 nm,动态背压(ABPR)为12.4 MPa,柱温50℃,进样量为1.0μL。5种脂溶性抗氧化剂在5 min内实现完全分离,并在1~100 mg/L的范围内具有良好的线性(r>0.9989);回收率为95.3%~102.2%;相对标准偏差为1.5%~5.0%(n=8);方法检出限(S/N≥3)为0.5~1.0 mg/kg。通过对实际样品的分析表明,本方法具高效快速、操作简单、实验成本低等优点,可以满足油脂及其制品中5种脂溶性抗氧化剂的快速、高通量的检测。A method for the separation and determination of five fat-soluble antioxidants in oils and fats and their products by ultra-performance convergence chromatography was established. After extracted by acetonitrile, antioxidants were separated on a Waters Acquity UPC2 HSS C18 SB （3. 0 mm x 100 mm i. d. , 1.8 μm） column at 50 ℃ by using supercritical CO2-methanol （contain 0. 1% formic acid） as the mobile phase at a flow rate of 1.5 mL/min, and then analyzed by a UV detector at wavelength of 280 nm. The result showed that the whole analysis progress was only 5 min and there was a good linearity （r〉0. 9989） in the range of 1 - 100 mg/L; the recoveries were between 95.3 % and 102. 2 % ; the relative standard deviations （RSD） were between 1.5 % and 5.0 % ; and the limits of detection （LOD） of five fat-soluble antioxidants were 2.0 mg/L. The analysis of the samples indicated that the method had the advantages of high efficiency, fast operation, simple operation and low cost and could meet the rapid and high-throughput detection of five fat-soluble antioxidants in oils and fats and their products.

关 键 词：超高效合相色谱法 脂溶性抗氧化剂 油脂 

分 类 号：TQ075[化学工程]