高效液相色谱法检测高糖食品中芳氧羧酸类化合物的研究

Investigation on the determination method of aryloxycarboxylic acids in high sugar food

应用高效液相色谱对高糖食品中的芳氧羧酸类化合物进行测定,对测定影响因素进行系统实验分析。通过优化实验条件,并进行大量实验室内加标回收率、精密度、应用范围、检出限和定量限等一系列的实验研究,建立测定波长为224 nm、甲醇-乙腈-水（50：10：40,v/v/v,pH=3）、色谱柱C18（250 mm×4.6 mm I.D.）,粒度5μm、流速0.8 mL/min、进样20μL、柱温25℃的高效液相-二极管阵列检测法。结果表明,浓度范围在0.25～300μg/mL内与响应值成良好的线性关系,经前处理优化,糖果和糕点加标平均回收率分别为96.2%～99.0%和89.0%～96.5%,重复性试验相对标准偏差（RSD）分别为2.5%～4.7%和3.6%～4.9%（n=10）,精密度好;方法检出限为0.003g/kg,定量限为0.01 g/kg。

Aryloxycarboxylic acids in high sugar food were determined by using high performance liquid chromatography. In this paper, the influence factors in determination were investigated and gave the systematic experimental analysis. By optimizing the experimental conditions, plenty of laboratory spiked experiment on recovery rate, precision, range of application, the limit of detection and the limit of quantification were researched, a method by using IC-DAD determined of aryloxycarboxylic acids in high sugar food was established which determination wavelength was 224 nm, methanol acetonitrile water （50：10：40, v/v/v, pH=3）, C18 column （250 mm×4.6 mm LD.）, size 5 μm, the flow rate was 0.8 mL/min, injection of 20 μL, column temperature was 25℃. The results indicated the concentration of 2-（4-methoxy phenoxy） propionate in the 0.25-300μg/mL range with a good linear relationship between response. After pretreatment optimization, recovery of candy and cakes were 96.2%-99.0% and 89.0%-96.5%, RSD of repeatability were 2.5%-4.7% and 3.6%-4.9% （n=10） respectively, good precision; The detection limit was 0.003 g/kg and the limit of quantification was 0.01 g/kg.