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  

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

作　　者：王巧玲 于玥 徐敦明[2] 张志刚[2] 方恩华[2] 冯峰[3] 张峰[3] 储晓刚[3] 

机构地区：[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

出　　处：《色谱》2016年第7期697-702,共6页Chinese Journal of Chromatography

基　　金：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)~~

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0.999 8,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。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. 0mg / L. The linear equation was y = 164. 4x-11. 3 with the correlation coefficient of 0. 999 8,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）was25 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.

关 键 词：高效液相色谱 左旋肉碱 调制乳粉 衍生化 

分 类 号：O658[理学—分析化学]