食品科学 ›› 2010, Vol. 31 ›› Issue (8): 219-222.doi: 10.7506/spkx1002-6300-201008049

• 分析检测 • 上一篇    下一篇

高效液相色谱法测定食品中非食用色素酸性橙Ⅱ

徐 琴1,2,刘 琳2,傅余强2,牟志春2,蔡 发2,林 洪1   

  1. 1.中国海洋大学食品科学与工程学院 2.山东出入境检验检疫局技术中心
  • 收稿日期:2009-05-04 修回日期:2009-11-25 出版日期:2010-04-15 发布日期:2010-12-29
  • 通讯作者: 徐琴 E-mail:aqh.xuq@gmail.com

HPLC Determination of Acid Orange 7 in Foods

XU Qin1,2,LIU Lin2,FU Yu-qiang2,MU Zhi-chun2,CAI Fa2,LIN Hong1   

  1. 1. College of Food Science and Engineering, Ocean University of China, Qingdao 266003, China;
    2. Technology Center for Shandong Entry-Exit Inspection and Quarantine Bureau, Qingdao 266002, China
  • Received:2009-05-04 Revised:2009-11-25 Online:2010-04-15 Published:2010-12-29
  • Contact: XU Qin1 E-mail:aqh.xuq@gmail.com

摘要:

建立食品中非食用色素酸性橙Ⅱ的高效液相色谱快速检测方法。样品用饱和乙腈提取,经饱和正己烷萃取除去油溶性色素及杂质,采用高效液相色谱柱分离,二极管阵列检测器(DAD)检测,结合标准物质保留时间和DAD 光谱图进行定性分析,外标法定量。色谱柱为Agilent ZORBAX SB-C18(150mm × 4.6mm,5μm),流动相为乙腈- 体积分数0.3% 醋酸溶液进行梯度洗脱,检测波长为484nm,线性范围为0.01~1.0 μ g/mL,相关系数R2=0.9997。采用本方法对乳制品、辣椒粉、辣椒酱、卤肉制品、卤蛋、卤豆腐干6 种常见基质进行验证,结果表明,HPLC-DAD 测定食品中的酸性橙Ⅱ,对于1.0g 样品定容至5mL、进样量为20μL 时,检出限为0.05mg/kg;添加标准回收实验表明,本方法在添加水平分别为0.05、0.1、0.2mg/kg 时的样品平均回收率在74.9%~100.0% 之间,相对标准偏差(RSD)在1.41%~8.64% 之间(n=6)。本方法准确、可靠。

关键词: 食品, 酸性橙Ⅱ, 高效液相色谱法, 二极管阵列检测器, 测定

Abstract:

A high-performance liquid chromatographic (HPLC) method was developed for the determination of acid orange 7 in foods. Samples were extracted with n-hexane saturated acetonitrile, and the extract was then extracted twice with acetonitrile saturated n-hexane for the removal of oily pigments and other impurities. The resulting lower phase was subjected to HPLC analysis using Agilent ZORBAX SB-C18 column set at 40 ℃ followed by detection with a diode array detector (DAD) detector at 484 nm. Binary linear gradients were achieved using mobile phase A: acetonitrile and mobile phase B: 0.3% acetic acid aqueous solution at a flow rate of 1.0 mL/min. The calibration curve for determination of acid orange 7 by the method exhibited good linearity over the concentration from 0.01 to 1.0 mg/L with a correlation coefficient of 0.9997 and the limit of detection (LOD) of the method was 0.05 mg/kg. Mean recoveries of 6 replicates for acid orange 7 in 6 different matrix samples spiked at the levels of 0.05, 0.1 mg/kg and 0.2 mg/kg ranged between 74.9% and 100%, with a relative standard deviation (RSD) range of 1.41% to 8.64%. The method proved good in intra-laboratory accuracy and precision.

Key words: food, acid orange 7, high-performance liquid chromatography, diode array detector, determination

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