色谱

色谱 ›› 2016, Vol. 34 ›› Issue (7): 697-702.DOI: 10.3724/SP.J.1123.2016.03027

• 特别策划:出入境检验检疫系统专栏(2016) • 上一篇    下一篇

柱前衍生-高效液相色谱法测定调制乳粉中左旋肉碱的含量

王巧玲1, 于玥1, 徐敦明2, 张志刚2, 方恩华2, 冯峰3, 张峰3, 储晓刚3   

  1. 1. 二连浩特出入境检验检疫局, 内蒙古 二连浩特 011100;
    2. 厦门出入境检验检疫局, 福建 厦门 361026;
    3. 中国检验检疫科学研究院食品安全研究所, 北京 100123
  • 收稿日期:2016-03-18 出版日期:2016-07-08 发布日期:2013-02-05
  • 通讯作者: 徐敦明
  • 基金资助:

    质检总局公益性行业科研专项项目(2012104002);福建省自然科学基金项目(2014J01057);检验检疫行业标准项目(2014B087).

Determination of L-carnitine in dairy products by high performance liquid chromatography coupled with pre-column derivatization

WANG Qiaoling1, YU Yue1, XU Dunming2, ZHANG Zhigang2, FANG Enhua2, FENG Feng3, ZHANG Feng3, CHU Xiaogang3   

  1. 1. Erlianhot Entry-Exit Inspection and Quarantine Bureau, Erlianhot 011100, China;
    2. Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361026, China;
    3. Institute of Food Safety, Chinese Academy of Inspection and Quarantine, Beijing 100123, China
  • Received:2016-03-18 Online:2016-07-08 Published:2013-02-05
  • Supported by:

    Public Science and Technology Research Funds Project of AQSIQ (No. 2012104002);Natural Science Foundation of Fujian Province (No. 2014J01057);Inspection and Quarantine Standards Project (No. 2014B087).

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114

被引次数

3

摘要：

建立了柱前衍生-高效液相色谱(HPLC)测定乳制品中左旋肉碱含量的方法。试样经0.1 mol/L盐酸超声提取后,采用阳离子交换固相萃取柱净化,在三乙胺和氯甲酸丁酯的催化下与L-丙酰胺-β-萘胺发生取代反应,使用配有二极管阵列检测器(DAD)的高效液相色谱仪测定,外标法定量。该方法在0.250~50.0 mg/L范围内线性关系良好,线性方程为y=164.4x-11.3,相关系数为0.9998,加标回收率为84.3%~86.0%,相对标准偏差为1.93%~3.18%。该方法的检出限为10 mg/kg,定量限为25 mg/kg。运用该方法对国内20个实际乳粉样品中的左旋肉碱含量进行测定,20个样品中均检出了左旋肉碱,含量为53~163 mg/kg。该方法快速、简便、准确,适用于乳品中左旋肉碱含量的检测。

关键词: 调制乳粉, 高效液相色谱, 衍生化, 左旋肉碱

Abstract:

A method has been established for the determination of L-carnitine in dairy products by high performance liquid chromatography (HPLC) coupled with pre-column derivatization. The samples were extracted by ultrasonator with 0.1 mol/L HCl as extraction solvent, and purified by a cation exchange solid phase extraction column, undergone a substitution reaction with L-propionamide-β-naphthylamine catalyzed by triethylamine and butyl chlorocarbonate. Then, the compound was detected by HPLC, with a diode array detection (DAD) as quantitative method. A linear calibration curve was obtained in the mass concentration range of 0.250-50.0 mg/L. The linear equation was y=164.4x-11.3 with the correlation coefficient of 0.9998, and the recoveries were 84.3%~86.0% with the relative standard deviations (RSDs) of 1.93%~3.18%. The limit of detection (LOD) was 10 mg/kg, and the limit of quantification (LOQ) was 25 mg/kg. The proposed procedure was then applied to the analysis of 20 real samples collected from China, and the contents of L-carnitine were 53-163 mg/kg. This method is rapid, simple, accurate and suitable for the determination of L-carnitine in dairy products.

Key words: dairy products, derivatization, high performance liquid chromatography (HPLC), L-carnitine

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