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。
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.
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