Optimized DLLME Method Coupled to HPLC for Simultaneous Analyses of Benzoates, Sorbates and Methyl p-hydroxyl Benzoates in Fruits Products

Tighrine Abderrahmane, M. Marzouk, Amir Youcef
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Abstract

We used an accurate and green technique “Dispersive Liquid Liquid Micro Extraction” (DLLME) followed by HPLC-UV analysis for the analysis of benzoates (BA), sorbates (SA), and p-hydroxyl methyl benzoates (MB) in fruits products. We optimized the   extraction parameters by the box Behnken design. We validated the method by using the β accuracy profile including the systematic (trueness) and random (intermediate precision) errors. The extraction efficiency varied from 82.98 to 100.8 %. This method was linear with R2s values higher than 0.9752 for all the compounds. The repeatability and intermediate precision were less than 3.18 and 12.02 respectively; whereas, the detection limits were respectively 0.304, 0.306 and 0.153 mg/ ml for BA, SA and MB. This method is therefore reliable to the simultaneous quantification of these preservatives in fruit juices, nectars and jams. The levels of these additives in the samples exceeded 833.97 and 290.67 ppm for BA and SA, respectively; while, MB was not detected.  
优化DLLME - HPLC同时分析水果产品中苯甲酸酯、山梨酸酯和对羟基苯甲酸甲酯的方法
采用高效液相色谱-紫外分光光度法(HPLC-UV)对水果产品中苯甲酸酯(BA)、山梨酸酯(SA)和对羟基苯甲酸甲酯(MB)进行分析。采用box Behnken设计对提取参数进行优化。我们使用包含系统(真实度)和随机(中间精度)误差的β精度曲线验证了该方法。提取效率为82.98% ~ 100.8%。所有化合物的R2s值均大于0.9752,线性关系良好。重复性和中间精密度分别小于3.18和12.02;BA、SA和MB的检出限分别为0.304、0.306和0.153 mg/ ml。该方法可用于果汁、花蜜和果酱中这些防腐剂的同时定量。样品中BA和SA的含量分别超过833.97和290.67 ppm;而未检测到MB。
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