HPLC法测定酱腌菜中脱氢乙酸的含量

Determination of Dehydroacetic Acid in Preserved Vegetables by HPLC

建立HPLC法测定酱腌菜中脱氢乙酸含量的方法,并对测量结果进行了不确定度分析和评定。色谱柱为Thermo AcclaimTMC18(250mm×4.6 mm,5μm);流动相:甲醇-0.02 mol/L乙酸铵溶液(10﹕90);流速:1.0 mL/min;检测波长:293 nm;柱温:35℃。该方法具有良好的精密度与稳定性,脱氢乙酸在1.079～25.90μg/mL范围内线性良好,其平均回收率为95.2%,方法检出限为0.43 mg/kg,测量结果的不确定度主要由样品称量引入,标准曲线斜率引入的不确定度影响最小。该方法简便、易操作、结果准确、重现性好,适用于酱腌菜中脱氢乙酸含量的检测。

To establish method for determination of dehydroacetic acid in preserved vegetables by HPLC, and to evaluate the uncertainty for the result. The chromatographic separation was performed on Thermo AcclaimTM C18 column using methanol-0.02 mol/L ammonium acetate solution as mobile phase of 10∶90 at the flow rate of 1.0 mL/min. The column temperature was set at 35 ℃. The detection wavelength was 293 nm. Result showed the method had good precision and stability, The calibration curves established showed good linearity over the concentration ranges of 1.079～25.90, and average recovery was95.2%.The LOD is 0.43 mg/kg. The results indicate that weighting sample is the largest factor contributed to the combined uncertainty, Slope is lowest. The method was simple, accurate and reproducible, it was suitable for determination of dehydroacetic acid in preserved vegetables.