Magnetic layered double hydroxide/zeolitic imidazolate framework-8 nanocomposite as a novel adsorbent for enrichment of four endocrine disrupting compounds in milk samples

For the first time, a novel nanocomposite, zeolitic imidazolate framework/magnetic layered double hydroxide (Fe3O4@LDH/ZIF), was successfully fabricated through in situ synthetic method with Fe3O4 as magnetic core and composite as shell. The resulting materials were characterized by XRD, TEM, FT-IR, VSM, TGA and nitrogen adsorption-desorption analysis. The Fe3O4@LDH/ZIF was employed as a sorbent in dispersive micro-solid phase extraction (D-mu-SPE) for enrichment of four endocrine disrupting compounds (EDCs) from milk samples prior to ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS) analysis. The synthesized nanocomposite showed bigger specific surface area and better absorption capacity than Fe3O4@LDH. The equilibrium adsorption capacities (Qe, mg/g) of EDCs on the Fe3O4@LDH/ZIF reached up to 47.4-138.8 mg/g, mainly resulting from hydrogen bonding, pi-pi interaction and electrostatic interaction between EDCs and nanocomposite. Several variables affecting the extraction efficiency were investigated and optimized. The method displays low limits of detection (3-15 ng L-1), good linearity (10-5000 ng L-1), acceptable precision (RSD < 7.8%) and accuracy (RE < 5.2%). Satisfactory repeatability was obtained with RSD in the range of 1.2-7.8%. This work provides a promising approach for the development of new sorbent media in sample preparation for the improvement of analytical performance.

Automated summary

A novel nanocomposite, Fe3O4@LDH/ZIF, was successfully fabricated and employed as a sorbent in dispersive micro-solid phase extraction for the enrichment of endocrine disrupting compounds in milk samples. The synthesized nanocomposite showed high adsorption capacities and promising potential for improving analytical performance in sample preparation.