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ORIGINAL PAPER

In-situ fabrication of zeolite imidazole framework@hydroxyapatite composite for dispersive solid-phase extraction of benzodiazepines and their determination with high-performance liquid chromatography-VWD detection Zi-Ling Li 1 & Zi-Yang Zhang 1 & Teng-Wen Zhao 1 & Chun-Yan Meng 1 & Qian-Ying Zhang 2 & Man-Man Wang 1 Received: 26 April 2020 / Accepted: 18 August 2020 # Springer-Verlag GmbH Austria, part of Springer Nature 2020

Abstract A novel zeolite imidazole framework@hydroxyapatite composite (ZIF-8@HAP) was constructed via in-situ growth and developed for efficient dispersive solid-phase extraction (DSPE) of three benzodiazepines from urine samples. The prepared composite was characterized by scanning electron microscopy, energy-dispersive spectrometer, Fourier-transform infrared spectrometry, X-ray diffractometry, zeta potential analyzer, and nitrogen adsorption-desorption experiment. Characterization results showed typical dodecahedron ZIF-8 crystals that were uniformly located on the surface of rod-like HAP. The combination of ZIF-8 and HAP made the surface area significantly enhanced from 4.68 to 205.44 m2 g−1. Compared with a commercial C18 adsorbent, ZIF8@HAP exhibited superior removal performance for interfering components from urine and offered better extraction properties for the analytes. The prepared ZIF-8@HAP was applied as an adsorbent in DSPE, and the main experimental parameters, including pH and ionic strength of solution, adsorbent amount, adsorption time, elution solvent, and volume, were investigated. Under optimal conditions, the adsorption for 250 ng mL−1 of each analyte in 4 mL of urine was accomplished within 2 min using 60 mg of adsorbent. The method of ZIF-8@HAP–based DSPE followed by high-performance liquid chromatography gave enhancement factors of 13.3–15.3, linear ranges of 2.5–500 ng mL−1, and limits of detection (S/N = 3) of 0.7–1.4 ng mL−1. The relative recoveries at three spiked levels ranged from 88.7 - 102% with intra-day and inter-day precisions from 3.0 - 10.3% and 2.3 - 12.3%, respectively. These results indicated that the proposed strategy had promising applicability for convenient, rapid, and efficient determination of benzodiazepines in urine samples. Keywords Metal-organic frameworks . Sample pretreatment . Pharmaceutical analysis . Biological fluid

Introduction Benzodiazepines (BZPs) are a class of psychiatric pharmaceuticals extensively used to treat anxiety, insomnia, and other Electronic supplementary material The online version of this article (https://doi.org/10.1007/s00604-020-04517-y) contains supplementary material, which is available to authorized users. * Man-Man Wang [email protected] 1

School of Public Health, North China University of Science and Technology, No. 21 Bohai Road, Caofeidian, Tangshan 063210, Hebei, People’s Republic of China

2

North China University of Science and Technology Affiliated Hospital, No. 73 Jianshe Road, Tangshan 063000, Hebei, People’s Republic of China

mental illnesses due to their therapeutic properties,