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核壳磁性沸石咪唑酯骨架-8作为从人尿中磁性固相萃取马钱子碱和士的宁的吸附剂。

Core-shell magnetic zeolite imidazolate framework-8 as adsorbent for magnetic solid phase extraction of brucine and strychnine from human urine.

作者信息

Ding Ya-Wen, Jin Ling, Feng Shi-Lan, Chen Juan

机构信息

School of Pharmacy, Lanzhou University, Lanzhou 730000, China.

College of Pharmacy, Gansu University of Chinese Medicine, Lanzhou 730000, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2021 Apr 20;1173:122702. doi: 10.1016/j.jchromb.2021.122702.

Abstract

Core-shell magnetic zeolite imidazolate framework-8 (FeO@PAA@ZIF-8) was successfully synthesized and first employed as adsorbent of magnetic solid-phase extraction (MSPE) for the determination of brucine and strychnine in human urine sample coupled with high performance liquid chromatography. The as-prepared FeO@PAA@ZIF-8 was characterized by transmission electron microscopy, Fourier-transform infrared spectrometry, X-ray diffraction, vibrating sample magnetometer and zeta potential analysis. Main parameters affecting the MSPE efficiency, including amount of adsorbent, sample solution pH, extraction time, ionic strength, desorption solvent, desorption time and desorption volume were further optimized. Under the optimized conditions, the proposed method provided good linearity (5.0-1000.0 μg L) with determination coefficients between 1.0000 and 0.9998, low limits of detection in the range of 1.1-1.2 μg L, and excellent reproducibility with relative standard deviations of less than 7.7%. The intra-day and inter-day precision were 1.5-3.2% and 2.1-7.2%, respectively. Satisfactory spiked recoveries were between97.2% and 115.4% with the relative standard deviations less than 6.3%. The results demonstrated that FeO@PAA@ZIF-8 composite was a promising magnetic adsorbent for the preconcentration of brucine and strychnine in human urine sample.

摘要

成功合成了核壳磁性沸石咪唑酯骨架-8(FeO@PAA@ZIF-8),并首次将其用作磁性固相萃取(MSPE)吸附剂,结合高效液相色谱法测定人尿液样本中的马钱子碱和士的宁。通过透射电子显微镜、傅里叶变换红外光谱、X射线衍射、振动样品磁强计和zeta电位分析对所制备的FeO@PAA@ZIF-8进行了表征。进一步优化了影响MSPE效率的主要参数,包括吸附剂用量、样品溶液pH值、萃取时间、离子强度、解吸溶剂、解吸时间和解吸体积。在优化条件下,该方法具有良好的线性(5.0 - 1000.0 μg/L),测定系数在1.0000至0.9998之间,检测限低至1.1 - 1.2 μg/L,具有出色的重现性,相对标准偏差小于7.7%。日内和日间精密度分别为1.5 - 3.2%和2.1 - 7.2%。加标回收率令人满意,在97.2%至115.4%之间,相对标准偏差小于6.3%。结果表明,FeO@PAA@ZIF-8复合材料是一种用于人尿液样本中马钱子碱和士的宁预富集的有前景的磁性吸附剂。

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