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Development of an extraction method for the determination of inorganic anions (chloride sulfate and phosphate) in edible oils from different origins by ion chromatography

机译:离子色谱法测定不同来源食用油中无机阴离子(氯离子硫酸根和磷酸根)的提取方法的建立

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摘要

The present work reports the development of ion chromatography conductivity based detection analytical method for the determination of some inorganic anions (chloride, sulfate and phosphate) in vegetable oils. The analytes were extracted from samples prior to injection into the chromatographic system, employing a simple two-step procedure. In the first step, 4.5 g of the sample was vigorously mixed with 15 mL of deionized water and then mixed for 15 min on a horizontal roller. Afterwards, the mixture was sonicated for 15 min in an ultrasonic bath. Then, the mixture was centrifuged for 15 min at 5000 rpm and, after filtration through a 0.22 μm membrane, the aqueous phase was used for the determination of the analytes. A clean-up step was introduced in the analysis of olive oils in order to correct an increase of the baseline of the chromatograms. The limits of detection and quantification of the proposed method were, respectively, 0.005 and 0.02 μg g−1 for chloride, 0.02 and 0.06 μg g−1 for phosphate and 0.008 and 0.03 μg g−1 for sulfate. Vegetable oils from corn, canola, soybean, sunflower and olive were analyzed and recovery tests (94.8 ± 10.1% mean recovery) were performed to attest the accuracy of the proposed method.
机译:本工作报告了基于离子色谱电导率的检测分析方法的发展,该方法用于确定植物油中的某些无机阴离子(氯离子,硫酸根和磷酸根)。使用简单的两步程序从样品中提取分析物,然后将其注入色谱系统。第一步,将4.5 g样品与15 mL去离子水剧烈混合,然后在水平辊上混合15分钟。之后,将混合物在超声浴中超声处理15分钟。然后,将混合物以5000 rpm的速度离心15分钟,然后通过0.22μm膜过滤后,将水相用于测定分析物。为了校正色谱图基线的增加,在橄榄油的分析中引入了净化步骤。该方法的检出限和定量限分别为氯化物0.005和0.02μgg -1 ,磷酸盐分别为0.02和0.06μgg -1 和0.008硫酸盐0.03μgg -1 分析了来自玉米,低芥酸菜籽,大豆,向日葵和橄榄的植物油,并进行了回收率测试(平均回收率94.8±10.1%),以证明该方法的准确性。

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