Campos Adriana Fernández, Cassella Ricardo J
1Departamento de Química Analítica, Universidade Federal Fluminense, Outeiro de São João Batista s/n, Centro, Niterói, RJ 24020-141 Brazil.
2Escuela de Química, Universidad de Costa Rica, Sede "Rodrigo Facio Brenes", Montes de Oca, C.P. 2060, San José, Costa Rica.
J Food Sci Technol. 2018 Oct;55(10):3922-3929. doi: 10.1007/s13197-018-3317-5. Epub 2018 Jul 19.
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 for chloride, 0.02 and 0.06 μg g for phosphate and 0.008 and 0.03 μg g 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.
本研究报告了一种基于离子色谱电导检测的分析方法的开发,用于测定植物油中的某些无机阴离子(氯离子、硫酸根离子和磷酸根离子)。在注入色谱系统之前,采用简单的两步程序从样品中提取分析物。第一步,将4.5 g样品与15 mL去离子水剧烈混合,然后在水平滚轴上混合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离心15分钟,通过0.22μm膜过滤后,将水相用于分析物的测定。在橄榄油分析中引入了净化步骤,以校正色谱图基线的升高。所提出方法的检测限和定量限分别为:氯离子0.005和0.02 μg/g,磷酸根离子0.02和0.06 μg/g,硫酸根离子0.008和0.03 μg/g。对来自玉米、油菜、大豆、向日葵和橄榄的植物油进行了分析,并进行了回收率测试(平均回收率为94.8±10.1%),以证明所提出方法的准确性。