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Development of a partitioned liquid-liquid extraction- dispersive solid phase extraction procedure followed by liquid chromatography-tandem mass spectrometry for analysis of 3-monochloropropane-1,2-diol diesters in edible oils
Journal of Chromatography A ( IF 4.1 ) Pub Date : 2018-03-13 , DOI: 10.1016/j.chroma.2018.03.017
J.A. Custodio-Mendoza , R.A. Lorenzo , I.M. Valente , P.J. Almeida , M.A. Lage , J.A. Rodrigues , A.M. Carro

A fast and effective method using a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) approach which includes partitioned liquid-liquid extraction (PLLE) and dispersive solid phase extraction (dSPE) clean-up step for the determination of seven 3-monochloropropane-1,2-diol (3-MCPD) fatty acid diesters in vegetable oils is developed and validated according to the Food and Drug Administration (FDA) guidelines. Due to the complexity of the matrices, combination of silica based sorbents (Silica Strong Anion Exchange (Si-SAX), Supel™ QuE Z-Sep+ (Z-Sep+) and Primary Secondary Amine (PSA) were tested for lipid removal. The effect of several experimental factors on the efficiency of the extraction procedure was studied by a screening design 3422//16 and a response surface Doehlert design. The separation and determination was carried out by liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS). The method provided suitable linearity (r2 > 0.9960), precision (relative standard deviation (RSD) lower than 10%) and accuracy, in terms of recovery. The limits of detection (LOD) and limits of quantification (LOQ) ranged from 10 to 20 μg kg −1 and from 25 to 50 μg kg−1, respectively. The recoveries at three spiking levels of 100, 250, and 500 μg kg−1 were over the range of 71.4–122.9% with RSD lower than 13%. The method was successfully applied in edible oils and fatty food samples. The results provide valuable information to assess the risk of exposure to these foodborne contaminants.



中文翻译:

开发了分液-液萃取-分散固相萃取程序,然后进行液相色谱-串联质谱分析食用油中的3-一氯丙烷-1,2-二醇二酯

一种快速有效的方法,使用改良的QuEChERS(快速,简便,廉价,有效,坚固和安全)方法,其中包括分液液萃取(PLLE)和分散固相萃取(dSPE)净化步骤,可测定7种植物油中的3-一氯丙烷-1,2-二醇(3-MCPD)脂肪酸二酯是根据食品和药物管理局(FDA)指南开发和验证的。由于基质的复杂性,测试了基于二氧化硅的吸附剂(二氧化硅强阴离子交换(Si-SAX),Supel™QuE Z-Sep +(Z-Sep +)和伯仲胺(PSA))的组合去除脂质的效果。筛选设计研究了几种实验因素对萃取过程效率的影响3 4 2 2// 16和响应面Doehlert设计。分离和测定通过液相色谱与串联质谱联用(LC-MS / MS)进行。 就回收率而言,该方法提供了合适的线性度(r 2 > 0.9960),精度(相对标准偏差(RSD)低于10%)和精度。检测极限(LOD)和定量极限(LOQ)分别为10至20μgkg -1和25至50μgkg -1。100、250和500μgkg -1的三个峰值水平下的回收率范围在71.4–122.9%之间,RSD低于13%。该方法已成功应用于食用油和高脂食品样品中。结果为评估这些食源性污染物的暴露风险提供了有价值的信息。

更新日期:2018-03-13
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