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基于FeO@NH-MIL-88(Fe)@TpPa磁性固相萃取结合高效液相色谱法测定牛奶中的痕量双酚类物质

Determination of trace bisphenols in milk based on FeO@NH-MIL-88(Fe)@TpPa magnetic solid-phase extraction coupled with HPLC.

作者信息

Wang Qingying, Chen Lianfang, Cui Xiaoyan, Zhang Jie, Wang Yaohui, Yang Xiupei

机构信息

College of Chemistry and Chemical Engineering, Chemical Synthesis and Pollution Control Key Laboratory of Sichuan Province, China West Normal University, Nanchong, 637000, China.

College of Chemistry and Chemical Engineering, Chemical Synthesis and Pollution Control Key Laboratory of Sichuan Province, China West Normal University, Nanchong, 637000, China.

出版信息

Talanta. 2023 May 1;256:124268. doi: 10.1016/j.talanta.2023.124268. Epub 2023 Jan 13.

DOI:10.1016/j.talanta.2023.124268
PMID:36657241
Abstract

Herein, a covalent organic framework (COF) was grown on a magnetic metal-organic framework (MOF) by a solvothermal method for the efficient extraction of bisphenols (BPs). The magnetic solid-phase extraction (MSPE) of four bisphenols (bisphenol A, bisphenol B, bisphenol AF and bisphenol C) was carried out without adjusting the pH and salt concentration. When 30 mg FeO@NH-MIL-88(Fe)@TpPa was used to adsorb for 25 min, 6 mL methanol was used to elute for 20 min, and the extract was detected by high-performance liquid chromatography (HPLC). The proposed method has a low detection limit of 0.011-0.036 ng mL, a wide linear range of 0.05-100 ng mL, and a correlation coefficient (R) of 0.9980-0.9998. The intra-day and inter-day precisions are 0.74-2.54% and 1.68-3.72%, respectively. Bisphenol A was determined by applying the proposed method to the determination of actual milk samples. The standard addition experiment showed that the relative recovery of the four bisphenols was 85.70-119.7%. Pseudosecond-order, first-order, Langmuir and Freundlich models were applied to explore the adsorption characteristics of FeO@NH-MIL-88(Fe)@TpPa. In general, the established FeO@NH-MIL-88(Fe)@TpPa-MSPE-HPLC-UV method exhibits attractive sensitivity, simple manipulation, and excellent reusability, and it has excellent prospects for the detection of trace BPs in complex milk matrices.

摘要

在此,通过溶剂热法在磁性金属有机框架(MOF)上生长了一种共价有机框架(COF),用于高效萃取双酚(BPs)。在不调节pH值和盐浓度的情况下,对四种双酚(双酚A、双酚B、双酚AF和双酚C)进行了磁性固相萃取(MSPE)。当使用30mg FeO@NH-MIL-88(Fe)@TpPa吸附25分钟,用6mL甲醇洗脱20分钟,并用高效液相色谱(HPLC)检测提取物。所提出的方法具有0.011 - 0.036 ng mL的低检测限、0.05 - 100 ng mL的宽线性范围以及0.9980 - 0.9998的相关系数(R)。日内和日间精密度分别为0.74 - 2.54%和1.68 - 3.72%。通过将所提出的方法应用于实际牛奶样品的测定来测定双酚A。标准加入实验表明,四种双酚的相对回收率为85.70 - 119.7%。应用伪二级、一级、朗缪尔和弗伦德里希模型来探索FeO@NH-MIL-88(Fe)@TpPa的吸附特性。总体而言,所建立的FeO@NH-MIL-88(Fe)@TpPa-MSPE-HPLC-UV方法具有吸引人的灵敏度、简单的操作和出色的可重复使用性,并且在检测复杂牛奶基质中的痕量双酚方面具有极好的前景。

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