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通过环糊精修饰的毛细管电泳优化19种多环芳烃的分离条件及其在食用油中的应用

Optimizing separation conditions of 19 polycyclic aromatic hydrocarbons by cyclodextrin-modified capillary electrophoresis and applications to edible oils.

作者信息

Ferey Ludivine, Delaunay Nathalie, Rutledge Douglas N, Cordella Christophe B Y, This Hervé, Huertas Alain, Raoul Yann, Gareil Pierre

机构信息

Chimie-ParisTech, Laboratory of Physicochemistry of Electrolytes, Colloids and Analytical Sciences (PECSA), 75005 Paris, France; AgroParisTech, UMR 1145 Ingénierie Procédés Aliments, 75005 Paris, France; INRA, UMR 1145 Ingénierie Procédés Aliments, 75005 Paris, France; Sofiprotéol, 75008 Paris, France.

Chimie-ParisTech, Laboratory of Physicochemistry of Electrolytes, Colloids and Analytical Sciences (PECSA), 75005 Paris, France; CNRS, UMR 7195, Paris, France; UPMC Université Paris 06, Paris, France.

出版信息

Talanta. 2014 Feb;119:572-81. doi: 10.1016/j.talanta.2013.11.062. Epub 2013 Dec 1.

DOI:10.1016/j.talanta.2013.11.062
PMID:24401457
Abstract

For the first time, the separation of 19 polycyclic aromatic hydrocarbons (PAHs) listed as priority pollutants in environmental and food samples by the United States Environmental Protection Agency (US-EPA) and the European Food Safety Authority was developed in cyclodextrin (CD)-modified capillary zone electrophoresis with laser-induced fluorescence detection (excitation wavelength: 325 nm). The use of a dual CD system, involving a mixture of one neutral CD and one anionic CD, enabled to reach unique selectivity. As solutes were separated based on their differential partitioning between the two CDs, the CD relative concentrations were investigated to optimize selectivity. Separation of 19 PAHs with enhanced resolutions as compared with previous studies on the 16 US-EPA PAHs and efficiencies superior to 1.5 × 10(5) were achieved in 15 min using 10mM sulfobutyl ether-β-CD and 20mM methyl-β-CD. The use of an internal standard (umbelliferone) with appropriate electrolyte and sample compositions, rinse sequences and sample vial material resulted in a significant improvement in method repeatability. Typical RSD variations for 6 successive experiments were between 0.8% and 1.7% for peak migration times and between 1.2% and 4.9% for normalized corrected peak areas. LOQs in the low µg/L range were obtained. For the first time in capillary electrophoresis, applications to real vegetable oil extracts were successfully carried out using the separation method developed here.

摘要

首次在美国环境保护局(US-EPA)和欧洲食品安全局列为环境和食品样品中优先污染物的19种多环芳烃(PAHs)的分离中,采用激光诱导荧光检测(激发波长:325 nm)的环糊精(CD)修饰毛细管区带电泳实现。使用包含一种中性CD和一种阴离子CD混合物的双CD系统,能够实现独特的选择性。由于溶质是基于它们在两种CD之间的差异分配进行分离的,因此研究了CD的相对浓度以优化选择性。使用10 mM磺丁基醚-β-CD和20 mM甲基-β-CD,在15分钟内实现了19种PAHs的分离,与之前对16种美国环境保护局PAHs的研究相比,分辨率有所提高,效率优于1.5×10⁵。使用内标(伞形酮),并结合适当的电解质和样品组成、冲洗序列以及样品瓶材料,显著提高了方法的重复性。6次连续实验的典型相对标准偏差(RSD),峰迁移时间在0.8%至1.7%之间,归一化校正峰面积在1.2%至4.9%之间。获得了低μg/L范围内的定量限(LOQ)。在毛细管电泳中首次成功地将此处开发的分离方法应用于实际植物油提取物。

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