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采用整体式聚乙二醇固定相的胶囊相微萃取法从人乳中萃取六种双酚,然后用高效液相色谱-光电二极管阵列检测法进行测定。

Capsule phase microextraction of six bisphenols from human breast milk using a monolithic polyethylene glycol sorbent-based platform prior to high performance liquid chromatography-photo-diode array detection determination.

机构信息

Department of Chemistry, Laboratory of Analytical Chemistry, Aristotle University of Thessaloniki, Thessaloniki GR-54124, Greece.

Department of Chemistry and Biochemistry, Florida International University, Miami, FL, USA.

出版信息

J Chromatogr A. 2022 Dec 6;1685:463615. doi: 10.1016/j.chroma.2022.463615. Epub 2022 Oct 29.

Abstract

The determination of bisphenols in human breast milk is a matter of ongoing interest since it reveals the exposure levels in both lactating mothers, fetuses, and infants. Herein, capsule phase microextraction (CPME) is applied for the first time for the extraction of a mixture of bisphenols from human breast milk followed by their subsequent determination by high-performance liquid chromatography-photodiode array detection (HPLC-DAD). CPME is a recently introduced as an advanced micro preparative technique that meets the principles of Green Analytical Chemistry. Moreover, it integrates filtration, extraction and stirring mechanism into one single device, a composite attribute that allows selective extraction of analytes without any sample cleanup and facilitates faster extraction kinetics, resulting in enhancing the performance of the equilibrium-based extraction techniques that ensure better reproducibility and operational simplicity. Among four tested CPME devices, the sol-gel poly(ethylene glycol) capsules showed the best extraction efficiency. Critical factors of the extraction performance were investigated and optimized. The developed CPME-HPLC-PDA method was validated. Limits of detection and quantification were 7.58 ng/mL and 25 ng/mL, respectively. Relative recoveries were estimated between 89.7 and 110.5%, while the RSD values were <11% in all cases. CPME is poised to be a useful tool both for routine bioanalysis and research purposes.

摘要

测定人乳中的双酚类物质是一个备受关注的问题,因为它揭示了哺乳期妇女、胎儿和婴儿的暴露水平。本文首次应用胶囊相微萃取(CPME)从人乳中萃取双酚混合物,然后采用高效液相色谱-光电二极管阵列检测(HPLC-DAD)进行后续测定。CPME 是一种最近引入的先进的微制备技术,符合绿色分析化学的原则。此外,它将过滤、萃取和搅拌机制集成到一个单一的装置中,这种复合属性允许在无需任何样品净化的情况下选择性地萃取分析物,并促进更快的萃取动力学,从而增强基于平衡的萃取技术的性能,确保更好的重现性和操作简单性。在四种测试的 CPME 装置中,溶胶-凝胶聚乙二醇胶囊显示出最佳的萃取效率。对萃取性能的关键因素进行了考察和优化。建立的 CPME-HPLC-PDA 方法进行了验证。检测限和定量限分别为 7.58ng/mL 和 25ng/mL。相对回收率在 89.7%至 110.5%之间,而在所有情况下,RSD 值均<11%。CPME 有望成为常规生物分析和研究目的的有用工具。

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